Threaded filler or colorant, or inorganic material for paper, in particular, natural calcium carbonate-containing colorant, method for manufacturing, composition containing the same, and uses thereof

FIELD: chemical and pulp-and-paper industry.

SUBSTANCE: aqueous suspension of at least one filler or mineral contains natural carbonate, polymeric dispersing agent as stabilizer of suspension viscosity, product of natural carbonate treatment with gaseous CO2, and product of natural carbonate reaction with at least one medium or strong H3O+-donors, has pH more than 7.5 at 200C. As natural carbonate suspension contains calcium carbonate (e.g., marble, calcite, carbonate-containing dolomite, chalk, ore mixtures thereof with talcum, and/or TiO2, MgO, or other minerals inert to H3O+-donors). As H3O+-donors suspension contains H2SO3, HSO

-4
, H3PO4, oxalic acid or mixtures thereof in molar ratio to carbonate of 0.1-2. Used carbon dioxide under pressure of 0.05-5 bar may be added from outside, recycled or obtained by continuous H3O+-donors addition. Treatment with H3O+-donors and gaseous CO2 may be carriedout simultaneously or separately, wherein in the last case temperature and time of respective stages are 5-900C and 1-5 h. Claimed suspension is dried to obtain colorant. Colorant has BET specific surface of 5-200 m2/g according to ISO 9277 and mean grain size measured by sedimentation method of 0.1-50 mum. Colorants are used in compositions, as agent for paper lamination, for paper pulp filling, coloration, and board production. Obtained paper is useful in numeric and ink-jet printing.

EFFECT: paper with decreased mass at constant surface.

33 cl, 1 dwg, 2 tbl, 8 ex

 

The present invention relates to the field of mineral fillers, in particular for use in the paper industry, and their improvements by the appropriate treatments for the purpose of improvement of the method of manufacturing a sheet of paper or improve its properties.

Such fillers are well known to the specialist should be called, for example, natural calcium carbonate, synthetic, or "besieged" calcium carbonate ("COC") and various fillers as dolomite, mixed fillers on the basis of the carbonates of various metals, such as, in particular, carbonate of calcium associated with magnesium carbonate, and similar various fillers as talc or similar, and mixtures of these excipients with one another, as, for example, mixtures of talc with calcium carbonate, the calcium carbonate with kaolin or even mixtures of natural calcium carbonate with aluminium hydroxide, mica or even with synthetic or natural fibers.

It seems necessary to consider in detail the method of manufacturing a sheet of paper, cardboard or similar. The specialist knows that pasta ("pulp"), which consists essentially of fibers (cellulose fibers of natural origin, as from coniferous or deciduous wood, or synthetic origin or mixtures), filler, such as written the above, and an appropriate share of the water.

Usually prepare a thick paste or a thick mixture, which is diluted with water to obtain a diluted paste or liquid mixtures". This paste is administered various additives, such as various polymers, to improve flocculation and, therefore, the "shaping" of the sheet, the filler retention and drainage of water under the canvas. Containing a fraction of the original filler aquatic environment, which drain under vacuum, under canvas, called "lead water". The sheet is then subjected to various treatments, of which an important operation is the operation called layering. During this operation layup know that there are losses nalivaeva salt solution and coated paper. This coated paper is re-used as filler mass and is called "waste due to breaks when layering".

The invention mainly relates to the treatment with a combination of one or more donor ions H3About+from the average power to a strong and active gas medium, pigments, fillers or minerals in aqueous suspensions containing natural calcium carbonate such as natural calcium carbonate, or any pigment containing natural calcium carbonate in combination with other minerals. In fact, it is logical that the natural calcium carbonate may be smeans minerals, inert with respect to the donor ions H3About+from the average power to a strong, well-known in the paper industry.

The invention is particularly applicable in the paper industry while achieving, in particular, equal or better properties sheet, and, in particular, opacity, whiteness, decreasing its weight for a given thickness. This reduction of weight of the paper at a constant sheet thickness, while preserving or improving the properties sheet in the continuation of the description of this application will be called property "volume".

Of particular interest is the application of the invention is of course as non-exhaustive, for improving properties during digital printing as ink jet printing, uncoated, but filled with processed according to the invention the pigment paper, or even on paper treated on the surface, or coated through the use of the pigments according to the invention.

In this particular field of inkjet printing, but not limiting the scope of protection of the invention, the invention relates to compositions, the filler which has simultaneously increased, the coarser the grain size distribution and high surface area.

Another special application of the invention lies in the field of paints.

Thus, the main aim of the invention is to reduce the weight of the paper manageruser while preserving identical, even improving them, the properties of the above paper.

Another important aim of the invention is the processing and layering sheets of paper or paper sheets in a broad sense, including cardboard and similar materials, using compositions according to the invention, and, in particular, treatment of pigmented surfaces of a sheet of paper.

The weight of the paper of this thickness is of great interest for reasons of transport and, in particular, the cost of postal items, as well as for reasons of environmental protection, namely, in particular, the savings of natural materials and energy resources.

Thus, in patent WO 92/06038, the purpose of which is to improve the opacity and whiteness of the paper containing the agent "volume" on the sheet, or coated with a salt solution containing the agent, we offer a solution which does not allow to achieve savings of energy resources.

Properties of opacity and best of whiteness is achieved through a very complex process, which occurs during the formation of a sheet of paper. As is known, the sheet is formed on canvas by flocculation or agglomeration or weave the various components of the paste, and, in particular, at the level of fibers or fibrils. This "agglomeration" is favored by drainage water, which is sucked off under the canvas. Some is which of these physico-chemical phenomena can occur, in particular, at the head of the camera or "headbox", or there may occur some transformations or interactions that will be conducive to such or such property on the canvas and on.

Without regard to any theory, the applicant believes that the filler depending on the treatment, which it is subjected or not, will interact differently with the fibrils and fibers. The invention relates to a special treatment, which, according to the present context, leads to the property "volume", then there is a good interaction with the grid of fibers. As also indicated in the document WO 92/06038, "volume" is expressed in the best light scattering sheet.

The problem, however, is complicated by the fact that the solution for "volume", which contributes to the increase in the internal pores of the paper (WO 96/32449, p.2, lines 15 and following), retards the drainage of water and, consequently, slows down the process of making paper, while there is a tendency to more and more fast running machines.

According to the invention, greatly improves the final property, the abrasion of the pigment during the manufacture of paper, that is, the invention allows to reduce abrasive wear of the used metal or plastic sieve and abrasion of the pigment during the operation layering paper, t is is, according to the invention, it is possible to reduce abrasive wear of the used plates. In patent WO 96/32449 emphasizes the importance of this property, and indicated that the pigment TiO2a good agent "volume", but too abrasive (and also expensive) (p.1, line 35 and following).

Finally, the present invention relates also to the ability to maintain the strength of the paper with the reduced mass in special applications such as the manufacture of envelopes.

As indicated above, and as confirmed in detail in the patents WO 96/32448 and WO 96/32449, there are two main types of calcium carbonate: one natural and the other is synthetic.

Synthetic calcium carbonate or "COC" get in a known manner by the reaction of anhydrous or calcined (slaked) lime CO2then get synthetic calcium carbonate, which, depending on the reaction conditions, is in different forms, such as needles, or other crystalline forms.

There are many patents relating to the synthesis of the COC.

Only as a reference in U.S. patent 5364610 describes the method of preparation of calcium carbonate with getting the JCC in scalenohedron forms. It describes as prior art methods of obtaining through the formation of carbonate with CO2. The JCC is represented as giving the paper improved their is TBA, in particular whiteness. The authors of this application also cited U.S. patent 5075093.

It is also well known that the OCC can provide "capacity due to the interactions that weaken the grid of fibers. In the above-mentioned patent WO 93/06038, however, describes how the formation of carbonate of lime with obtaining COC, having the properties of "volume".

On the contrary, natural carbonate does not provide this property, whereas, obviously, will be of great interest to obtain, in order not to force the use in industry of synthetic carbonate.

Therefore, there is a significant need for achievement, on the basis of natural carbonates, property volume or conducive to the properties of the surface interactions. Moreover, it is unexpected is the fact that the COC has an adverse effect on the strength of the mesh of fibers that new pigment according to the invention, not only gives the same properties as the OCC, however, retains the favorable properties of natural calcium carbonate.

Unexpectedly obtained a pigment with a perfect synergistic properties.

In this industry have already been proposed various processes.

In patent WO 96/32448 describes a processing method of a dispersion of calcium carbonate (denoted by the term "sludge" to consider what those industries), with minor concentrations of carbonate (1-30% solids) using homopolymer of dimethyldiallylammonium, which is a cationic aggregating agent with a low molecular weight from 10,000 to 500,000, for "volume". According to this patent, a well-used as the OCC and crushed natural carbonate, known as RPC ("ground natural calcium carbonate"), or mixtures thereof. This method is mainly flocculation, aggregation of small particles into larger, and properties of interaction with the fibers reach, mostly due to the coarse particle size of the particles. Physical properties deteriorate when its mass is reduced.

In patent WO 96/32449 describes almost the same technical instruction. The goal is to achieve selective aggregation of small and ultramatic particles using an aggregating agent, which is the filler, opposite to the filler loading.

In U.S. patent 4367207 cited in the patent WO 92/06038, describes a method of processing caso3with the help of CO2in the presence of anionic electrolyte organophosphonates type, however, the aim is only to obtain slurry of finely ground carbonate.

In the European patent 0406662 describes a method of production of synthetic carbonate, whereby carry out the preliminary mixing of caso3aragonite-type calcium oxide is, then to this add sludge derived phosphoric acid, like phosphoric acid or its salts, or various phosphates (see page 4, lines 17 and following), and, finally, enter the CO2for the implementation of the classical reactions of formation of carbonate. The purpose of this patent is to obtain a special way the OCC with large particle size and a specific crystalline (needle-like) form, which in the industry is not known. In the patents cited as prior art other patents relating to the method of obtaining the JCC by treatment with carbon dioxide as the improvement consisting in the introduction of CO2successive stages or added before the reaction centers of crystallization, corresponding to the desired crystalline form.

According to this European patent 0406662 use phosphoric acid for education (page 4, lines 46 and following) in a special way aragonite forms due to unidentified compounds type calcium salt of phosphoric acid, which serves as new centers of crystallization to the desired crystalline form (line 52, line 55).

Applications received carbonate is listed on p.5, lines 2 and later. Incidentally insulating and similar properties suitable carbonate in the paper industry for the possibility of introducing higher the quantities of mineral substances in the paper, which leads to the safe inside the papers. In this patent does not specify any properties, as the opacity of the paper, its brilliance or "volume", which clearly is not the object of the present invention. The only example of the application furthermore relates to compositions of carbonate/resin.

Also known methods of imparting special properties to the carbonate.

By the way, you should specify the achievement resistance to acids which are suitable when the carbonate is used as filler in the paper manufacturing process acid by representing one of the classic ways of paper production. Thus, in U.S. patent 5043017 describes the stabilization of calcium carbonate and in particular COC (column 1, line 27) by exposure to chelating agent calcium, as hexametaphosphate calcium, and conjugate base, which may be a salt of an alkali metal weak acid (phosphoric, citric, boric, acetic,... ). In this document refer to the prior art, in which the sodium hexametaphosphate is used as a dispersant, or according to which the salt of a weak acid is used after primary education carbonate in the production of JCC or, on the contrary, in the first stage of production. This document also cited U.S. patent 4219590, which describes a method for improving the dry calcium carbonate is houtem processing completely dry sour, consisting of anhydride by gas". In fact, in this document we are talking about the improvement of already known surface treatment, which is carried out by using fatty acids or acidic resins and similar substances (column 1, line 17). According to this document, the carbonate is treated with vapors generated by the boiling phosphoric acid, hydrochloric acid, nitric acid, capric acid, acrylic acid or chlorides or fluorides of aluminum, or fumaric acid, etc. the Goal is crushing particles of carbonate to dispermic particles (column 2, lines 65 and beyond). According to this document, it is recommended to use HF, SO2or phosphoric anhydride, and the only example describes the use of HF or titanium tetrachloride (the latter improves the opacity of the paper; column 3, lines 12 and later).

Also known U.S. patent 5230734, according to which the use of CO2to obtain the mixed calcium carbonate-magnesium.

In patent WO 97/08247 describes the preparation of carbonate for paper received subacid way. Carbonate is treated with a mixture of weak bases and weak acids, which include phosphoric acid, and one of the two agents should occur from organic acids.

In patent WO 97/14847 also describes how resistant is the slot carbonate for paper, which is treated with a mixture of two weak acids with the aim of "inactivation" of the surface carbonate.

In patent WO 98/20079 also describes a method of obtaining resistant to acid carbonate and, in particular, the OCC by adding calcium silicate and a weak acid or alum. In this document as prior art cited U.S. patent 5164006, according to which use processing with CO2to achieve resistance in an acidic environment. But then you add products such as zinc chloride, although they do not meet the standards of environmental protection. In addition, the pigment according to the invention it is sensitive to acids, and its unexpectedly positive reactivity allows to achieve a good interaction with the fibers.

In this industry, therefore, for decades, seeking to improve the properties of natural carbonate and/or synthetic carbonates JCC, which has specific properties. Among these studies are some attempts on "volume", but it should be noted that none of these works do not refer to the use of CO2. This gas is suitable for treatments involving giving antacid properties, without any relation to the "volume", or for the production of JCC by about the processing carbon dioxide. Also combining phosphoric acid and CO2but only to improve the production of JCC.

In fact, the best properties attached with the OCC, in industry everywhere strive to produce synthetic carbonates, with more and more improved properties. The merit of the invention consists in the desire to work on the basis of natural carbonates.

The invention relates, therefore, to obtain new water suspensions of one or more pigments, fillers or minerals, containing if need be one polymeric dispersant as a stabilizer rheology of the suspension, and these pigments can reduce a lot of paper at a constant surface.

These new water suspension are different because:

a) they contain natural carbonate or one or more reaction products of the above carbonate with gaseous CO2and one or more reaction products of the above carbonate with one or more donor ions H3O+from the average force to the strong; and

b) they have a pH value, measured at a temperature of 20° C, above 7.5.

They also differ in that the pigment, filler or mineral has a BET specific surface defined according to the standard ISO 9277, component 5-200 m2/g, preferably 20-80 m /g and highly preferably 30-60 m2/year

Preferably the aqueous suspensions according to the invention are characterized in that the pigment, filler or mineral has the following characteristics:

- the average grain diameter defined by the method of sedimentation on the device Sedigraf 5100™ is 50-0,1 micrometer;

and BET specific surface, determined according to the standard ISO 9277 is 15-200 m2/year

Even more preferably, they differ in that the pigment, filler or mineral has the following properties:

- the average grain diameter defined by the method of sedimentation on the device Sedigraf 5100™ is 25-0,5 micrometer, and even more preferably 7-0,7 micrometer;

and BET specific surface, determined according to the standard ISO 9277 is 20-80 m2/g and even more preferably 30-60 m2/year

The invention relates, furthermore, to the pigments or fillers in the dry state, such as natural calcium carbonate or any pigment containing natural calcium carbonate obtained by drying aqueous suspensions according to the invention, and this drying is carried out by using a well-known specialist tools for drying.

The invention also relates to the handling of pigments or fillers in aqueous suspension, such as the nature of the hydrated calcium carbonate or any pigment, containing natural calcium carbonate, or mixtures thereof, including there other fillers and pigments which do not contain carbonate ions; to the containing compositions and their applications in the paper industry, in particular to achieve good properties "volume", and thus filled or coated papers.

More specifically the invention relates to aqueous suspensions of pigments, fillers or minerals that may contain a polymeric dispersant as a stabilizer rheology of the suspension and includes a natural carbonate such as natural calcium carbonate or dolomite processed in combination with one or more donor ions H3O+from the average power to the strong and gaseous CO2.

As examples of various natural carbonates derived from the chalk, especially Champagne chalk, calcite or marble, and their mixture with talc, kaolin and/or dolomite and/or hydroxides of aluminum and/or titanium dioxide, magnesium oxide and the oxides and hydroxides, known in the industry.

According to this application, these various fillers and mixtures of fillers or mixed fillers United by one common name "fillers", except when you need a more specific indication of the filler or the AC is of egorie fillers.

Used acid is any acid from the average force to strong or any mixture of such acids, generating ions H3About+in terms of processing.

According to a preferred variant implementation, a strong acid is chosen among the acids having a pKa less than or equal to zero at a temperature of 22° S, and more preferably chosen among sulfuric acid, hydrochloric acid or mixtures thereof.

According to a preferred variant implementation, the medium-strength acid is chosen among the acids having a pKa of from 0 to 2.5, inclusive, at a temperature of 22° S, and more preferably chosen among H2SO3, HSO

-
4
N3RHO4, oxalic acid, or mixtures thereof. In particular, we can mention, for example, pKa1H3RHO4equal 2,161 (Rompp Chemie, ed. Thieme).

According to a preferred variant implementation, the acid or acid medium strength can be mixed with the acid or acids of medium strength.

According to the invention, the amount in moles of donor ions H3About+from the average force to strong relative to the number of moles of caso3is generally 0.1 to 2, preferably 0.25 to 1.

According to the invention, a method of processing pigments, fill the lei or minerals in aqueous suspensions containing natural carbonate, characterized in that the above-mentioned pigment is treated by a combination of one or more donor ions H3About+from the average power to the strong and gaseous CO2.

Preferably this proposed according to the invention, the method of processing of pigments, fillers or minerals in aqueous suspensions containing natural carbonate, which allows to reduce the weight of the paper at a constant surface, characterized in that it includes the following 3 stages:

a) treatment with donor or donor ions H3O+from the average force to the strong;

b) treatment with gaseous CO2and this treatment or is an integral part of stage a), or by parallel stage a), or it is carried out after stage a);

c) raising the pH value, measured at a temperature of 20° C, above 7.5 in the time interval after the end of stages a) and b)of from 1 hour to 10 hours, preferably from 1 hour to 5 hours, without added base, or immediately at the end of stages a) and b) adding the base, and stage C) is the last stage of the method.

Even more preferably gaseous CO2comes from the feed externally CO2or from recycling CO2or by adding continuously the same donor ions is 3About+from the average force to strong, as such, used in stage a) processing, or another donor ions H3About+from the average power to the strong, or even due to the increased pressure of CO2and preferably high pressure 0.05-5 bar. On this occasion it should be noted that the work tank filled with fillers with a density of about 1-2, can reach a height of, for example, 20 meters, and thereby creates a high pressure of CO2that can reach several bar and, in particular, up to about 5 bar at the bottom of the tank or in a closed vessel.

According to a preferred variant implementation, stages a) and b) can be repeated several times.

Also, according to a preferred variant implementation of the pH value, measured at a temperature of 20° is 3-7,5 during stages a) and b) processing and treatment temperature is 5-90° and preferably 45-60° C.

According to another preferred variant implementation, between 1 hour and 10 hours, and more preferably between 1 hour and 5 hours after treatment, the pH value is the value above 7.5 at room temperature, and this is without adding any reason. If any base is added, then immediately increases the pH value. Moreover, noresult, after a few days no resistance to acids not see.

The method of processing of pigments, fillers or minerals in aqueous suspensions containing natural carbonate, which allows to reduce the weight of the paper at a constant surface according to the invention, characterized in that the concentration of gaseous CO2in suspension, by volume such that the ratio (volume of suspension:volume of gaseous CO2) is from 1:0.05 to 1:20, when the above ratio from 1:1 to 1:20 in stage a) and from 1:0.05 to 1:1 in stage b).

Highly preferably, the concentration of gaseous CO2in suspension, by volume such that the ratio (volume of suspension:volume of gaseous CO2) is from 1:0.05 to 1:10, when the above ratio from 1:0.5 to 1:10 in stage a) and from 1:0.05 to 1:1 in stage b).

Gaseous CO2can be dosed in liquid or anhydrous form.

Also preferably, the duration of stage (b) processing is 0-10 hours, and more preferably 2-6 hours.

The processing method according to the invention is carried out in aqueous phase (sludge) with minor, moderate or high concentrations of dry matter, however, it can also be done in case of sludge mixtures of these different concentrations. The dry matter content is preferably 1-80 wt.%.

Without tie is with any theory, the applicant believes, that gaseous CO2besides, plays the role of the pH regulator and regulator of absorption/desorption.

According to one variant of the invention, a method of obtaining a water suspension according to the invention is characterized by the fact that after three stages of processing method according to the invention treated product is suspended in water using a dispersant and, if necessary, again concentrating.

Obtained according to the invention the aqueous suspension of the filler can be introduced into the manufacturing process of a sheet of paper, cardboard or similar material on the level of preparation of thick paste or diluted paste or these two levels depending on the manufacturing process of paper. The filler is actually injected one or more times in accordance with the usual recommendations of the manufacturers of paper.

Processed according to the invention the filler is also of great interest after the formation of the sheet and, in particular, the filler according to the invention can be introduced in recycled lead water or also recycled waste due to breaks when layering".

An alternative process according to the invention can be applied to recycled lead water or waste due to breaks when layering"; then recycled environment process according to the stages predlagaemoj is in the invention method, as specified above.

The invention relates to the manufacture of paper from cellulose fibers of wood origin, such as based on wood of deciduous or coniferous trees.

The invention relates also to a paper produced from fibers not wood, but on the contrary, of synthetic fibers.

Therefore, the invention also relates to methods of making paper, cardboard or similar materials, modified so due to the inclusion of the method according to the invention.

The invention also relates to the new products obtained by the method which has just been described.

The following examples explain the invention, but without limiting its scope.

Conduct a series of experiments with sludge with low content of solids, i.e. a maximum of about 30%, and another series of experiments with slurries with high solids content, i.e. up to about 80%.

The high content of great interest in this industry, but create special problems with viscosity. Then, it is often necessary, but optional, to add a dispersant, which may cause interference in the process (the effect of dispersant on competitive reactions at the level of the phenomena of adsorption on the surface of the carbonate or other types of fill the lei).

EXAMPLE 1

This example illustrates the invention and relates to the handling slurries with low content of dry substances.

To implement this in all the experiments of example 1 relating to water suspensions with low content of dry matter, cooked, caso3or a mixture of minerals containing calcium carbonate, in the form of suspension ("sludge"), solids or dry matter, which varies from 5 to 30 wt.%, or in the form of sediment on the filter, or in the form of a dry powder, in an appropriate reactor and, if necessary, diluted until the desired solids content by using demineralized water or tap water.

In the case of experience related to water suspension medium dry matter, cooked, caso3in the form of suspension ("sludge"), solids or dry matter in which is about 45 wt.%

For all experiments use a glass reactor of 1 liter or 10 liter or plastic container with a capacity of 100 liters or cistern displacement of 40 m3that is provided (supplied) type agitator rotor/stator, and a high-speed stirrer rotating disk 50 mm in diameter for reactors with a capacity of 1 liter and 10 liters or 200 mm for plastic containers with a capacity of 100 liters or 1500 mm for tanks with a volume of 40 m3.

the La some experiments, which will be clarified in further examples, use the mixer fluidized bed capacity 6 liters or 600 liters of the Lodige type.

After a homogeneous mixture in suspension or slurry establish appropriate experience temperature.

Then add the donor ions H3O+from the average power to a strong, preferably selected among H2SO3, HSO

-
4
N3RHO4, oxalic acid or mixtures thereof, in the form of a solution with concentration, component 1-85 wt.%, within a particular period of time. Deviations described below.

Add or enter CO2through the bottom of the tank or by using submerged down into the reservoir tube, within the time period specified below.

The control sample is paper made in parallel in the same way, with the same number of untreated filler, weighing 75 g/cm2and with the same amount of pulp.

Experience No. 1

Natural calcium carbonate type of Norwegian marble with a grain size distribution such that 75 wt.% particles have a diameter less than 1 micron, a specific device Sedigraph 5100 firm Micrometrics, in the form of sediment on the filter in an amount of 5 kg, calculated on the dry pigment in the container capacity is 100 liters diluted with distilled water until obtaining a slurry with a dry matter concentration of 10 wt.% Then, the thus obtained slurry is treated with sulfuric acid in the form of 10 wt.%-aqueous solution, the corresponding 0.20 mol H3About+per mole of caso3at a temperature of 20° and under stirring for two minutes with a speed of 500 revolutions per minute. After 15 minutes the suspension of calcium carbonate for 5 hours bubbled CO2with the increased pressure of 50 mbar so that the ratio (volume of suspension:volume of gaseous CO2) is about 1:0.15 in.

After conditioning for 24 hours to form sheets of paper containing as a filler suspension of the tested calcium carbonate.

To accomplish this, receive sheets of paper from a slurry or paste of cellulose mark SR 23 containing paste from sulfate wood and fibers, consisting of 80% birch and 20% pine. Then 45 g per dry matter of the slurry or paste is diluted in 10 litres of water in the presence of about 15 grams per dry matter of the composition of the tested fillers to obtain experimentally the content of the filler is from 20% to nearly 0.5%. After stirring for 15 minutes and add to 0.06 wt.% in relation to the dry weight of the paper retention agent polyacrylamide type receiving sheet with a mass equal to 75 g/m2and filled at (20±0,5%). Used for forming the sheet, the device is a system of Rapid-are Kothen, model 20.12 MS company Naude.

Thus, the formed sheet is Assiut for 400 seconds at a temperature of 92° C and in vacuum 940 mbar. The content of the filler is controlled by analysis of the ash.

Measure the thickness of the thus formed sheet.

The thickness of the paper or cardboard sheet represents the perpendicular distance between two parallel surfaces.

Samples were kondicionirovanie within 48 hours (according to the German norm DIN EN 20187).

This provision determines that the paper is a hygroscopic substance, and as such has the property that consists in the ability to adapt their moisture content to come in the appropriate status relative to that of the surrounding air. The moisture is absorbed, when increasing the humidity of the surrounding atmosphere, and Vice versa, is deleted when decreasing the humidity of the surrounding atmosphere.

Even if the relative humidity remains constant, the moisture content in the paper do not necessarily remains the same if the temperature is maintained constant within certain limits. During increase or decrease of moisture content on physical properties of paper are modified.

On this basis, the samples should be conditioned for at least a time period of 48 hours until reaching equilibrium. Samples were also tested under identical climatic conditions. The atmosphere of the experience in the case of paper was installed so that h is ordinary it meets the following data:

relative humidity of 50% (±3)

the temperature of 23° With (±1)

The thickness was determined according to the German norm DIN EN 20534 when using a micrometer, test print ("test print") which comes to 10 n/cm2. The result of the experiment was determined by calculating the average of 10 measurements. The result is expressed in micrometers.

The control sample is paper made in parallel in the same way, with the same amount of filler, but raw, with a mass of 75 g/m2and with the same amount of pulp.

The results:

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry is 7.7, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, control: 112 microns, with a weight of 75 g/m2;

for the prototype: 120 mm weight 75 g/m2that casting to the magnitude of the thickness of 112 μm gives a weight of 70 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 112 μm, achieve win in 5 g/m2or 6.6% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience No. 2

In a glass reactor with a capacity of 10 liters and under stirring 3 kg per dry pigment residue on the oltre type of Norwegian marble with a grain size distribution, such that 75 wt.% particles have a diameter less than 1 micron, a specific device Sedigraph 5100 of the company Micromeritics, in the form of a slurry with a concentration of dry matter 10 wt.% and at a temperature of 20° C, is treated with phosphoric acid in the form of 10 wt.%-aqueous solution, corresponding to 0.15 mol H3O+per mole of caso3. Then through the sludge bubbled CO2under high pressure of about 100 mbar for 5 hours so that the ratio (volume of suspension:volume of gaseous CO2) was approximately 1:0,1. Immediately after receipt, and after 1 hour, 2 hours, 3 hours, 4 hours and 5 hours to measure the pH value. Form leaves from the slurry with a low content of dry matter. With the help of 0.53 wt.% in relation to the dry weight of pigment dispersant of the type of sodium polyacrylate with a specific viscosity of 0.75 is possible to increase the concentration of dry matter to the value of 47 wt.%

The specific viscosity of the anionic dispersant in the examples, which is denoted by the symbol of the Greek letter "this" (η ), was defined as follows: obtained polymer solution, neutralized to 100% with sodium hydroxide solution (pH 9) for measuring, by dissolving 50 g with respect to the dry polymer in 1 liter of distilled water containing 60 g of NaCl. Then, using a capillary viscometer with a constant Baume 0,000105 in thermolabile is new at a temperature of 25° With the heating bath was measured by the time required for pouring through capillary exactly certain amount of alkaline polymer solution, and compared with the time during which the same volume of a solution of 60 g of NaCl/liter passes through the capillary.

The specific viscosity "this" can be defined as follows:

Get the best results if the diameter of the capillary is chosen so that the time required for the polymer solution, minus the time required for a solution containing only NaCl was value in the interval from 90 to 100 seconds.

After conditioning for 24 hours to form sheets of paper according to the same method as in experiment No. 1, with a mass of 75 g/m2and measure their thickness also using the same method as in experiment No. 1.

The results:

(a) pigment:

3 hours later after the processing of natural calcium carbonate according to experience, the pH value of the slurry is 7.5, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 123 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot 68,9 g/m2.

It is seen that in this experience, if the thickness of the inu paper lead to a total of 113 μm, reach win at 6.1 g/m2or 8.8% in relation to the paper pulp, which means significant savings in relation to the environment.

Also conduct measurements of opacity and whiteness filestoremove sheets.

Opacity was measured as the rate of light transmission of paper sheets with the help of a spectrophotometer of the type of Color Data Eirepho 2000 according to the standard DIN 53146.

The white paper was measured according to the standard ISO called Brightness R 457, filter Tappi when using ultraviolet light using a spectrophotometer type Data Color Eirepho 2000. The measurement was carried out on a stack of 10 sheets, in order to avoid the influence of light transmission.

Obtained by the above method, the results are as follows:

- white test sample according to the invention: 89,6

- the opacity of the prototype according to the invention: 89,4

- white control (untreated) sample: 88,4

- the opacity of the control (untreated) sample: 86,4.

Experience No. 3

In a glass reactor 75 g per dry pigment filtercake type of Norwegian marble with a grain size distribution such that 75 wt.% particles have a diameter less than 1 micron, a specific device Sedigraph 5100 of the company Micromeritics, in the form of a slurry with a dry matter concentration of 10 wt.% and at a temperature of 20° C, is treated with phosphoric acid is you in the form of 10 wt.%-aqueous solution, corresponding to 0.25 mol H3About+per mole of caso3. Then through the sludge bubbled CO2at atmospheric pressure for 5 hours so that the ratio (volume of suspension:volume of gaseous CO2) was about 1:0.05 is taken.

After conditioning for 24 hours to form sheets of paper according to the same method as in experiment No. 1, with a mass of 75 g/m2and measure their thickness also using the same method as in experiment No. 1.

The results:

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate according to the experience of the pH value of the slurry is 7.7, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 119 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot 71,1 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win 3.9 g/m2or 5.2% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience No. 4

1 kg per dry pigment calcium carbonate type Finnish marble with a grain size distribution such that 63 wt.% particles have a diameter of less than 1 micro is a, a particular with the help of the device Sedigraph 5100 of the company Micromeritics, crushed wet through, with a concentration of 75% (based on dry substance, when used to 0.55 wt.% of sodium polyacrylate with a specific viscosity of 0.54 diluted to the concentration in the sludge dry matter 45 wt.% and at a temperature of 20° C, is treated with phosphoric acid in the form of 10 wt.%-aqueous solution, corresponding to 0.15 mol H3About+per mole of caso3. Then through the sludge bubbled CO2under high pressure of about 100 mbar for 5 hours so that the ratio (volume of suspension:volume of gaseous CO2) was 1:0.1 to

The product was screened and after keeping for 24 hours to form a sheet by the same method, as in experiment No. 1, with a mass of 75 g/m2. Measure their thickness also in the same way as in experiment No. 1, and the results are then compared against the use of raw calcium carbonate with a grain size distribution such that 63 wt.% particles have a diameter less than 1 micron, a specific device Sedigraph 5100 of the company Micromeritics.

The results:

(a) pigment:

2 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry is 7.6, which means the absence of any stability towards acids;

b) for paper:

thickness measurements:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 116 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot of 72.9 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win at 2.1 g/m2or 2.8% in paper pulp, which means significant savings in relation to the environment.

Experience No. 5

In a glass reactor 75 g per dry pigment calcium carbonate type of Norwegian marble with a grain size distribution such that 75 wt.% particles have a diameter less than 1 micron, a specific device Sedigraph 5100 of the company Micromeritics, in the form of a slurry with a dry matter concentration of 10 wt.% and at a temperature of 35° is treated with phosphoric acid in the form of 10 wt.%-aqueous solution, corresponding to 0.15 mol H3About+per mole of caso3. Then through the sludge bubbled CO2at atmospheric pressure for 5 hours so that the ratio (volume of suspension:volume of gaseous CO2) was about 1:0.05 is taken.

After conditioning for 24 hours to form sheets of paper according to the same method as in experiment No. 1, with a mass of 75 g/m2and measure their thickness also using the same method as in experiment No. 1.

The results:

(a) pigment:

JV is a degree 5 hours after completion of processing of natural calcium carbonate, according to experience, the pH value of the slurry is 7.8, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 118 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot 71,8 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win 3.2 g/m2or 4.2% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience No. 6

In a glass reactor 75 g per dry pigment calcium carbonate type of Norwegian marble with a grain size distribution such that 75 wt.% particles have a diameter less than 1 micron, a specific device Sdigraph 5100 company Micromeritics, in the form of a slurry with a dry matter concentration of 10 wt.% and at a temperature of 45° is treated with phosphoric acid in the form of 10 wt.%-aqueous solution, corresponding to 0.30 mol H3About+per mole of caso3. Then through the sludge bubbled CO2at atmospheric pressure for 5 hours so that the ratio (volume of suspension:volume of gaseous CO2) was 1:0.05 is taken.

After conditioning for 24 hours to form the sheets of paper by the same method as in experiment No. 1, with a mass of 75 g/m2and measure their thickness also using the same method as in experiment No. 1.

The results:

(a) pigment:

later, 4 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry is 7.9, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 118 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot 71,8 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win 3.2 g/m2or 4.2% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience No. 7

In a glass reactor 36 g per dry pigment calcium carbonate type Finnish marble with a grain size distribution such that 65 wt.% particles have a diameter less than 1 micron, a specific device Sedigraph 5100 of the company Micromeritics, from 21.6 wt.% (calcium carbonate) in the form of a slurry with a dry matter concentration of 4.8 wt.% (more diluted) and at a temperature of 35° is treated with phosphoric acid in the form of a 5 wt.%-aqueous solution, corresponding to 0.32 mol H3About+per mole of caso3. For the eat through the sludge bubbled CO 2at atmospheric pressure for 5 hours so that the ratio (volume of suspension:volume of gaseous CO2) was 1:0.05 is taken.

After conditioning for 24 hours to form sheets of paper according to the same method as in experiment No. 1, with a mass of 75 g/m2and measure their thickness also using the same method as in experiment No. 1.

The results:

(a) pigment:

after 6 hours after completion of processing of natural calcium carbonate, according to experience, the pH value of the slurry is 7.5, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 121 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot 70,0 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win in 5 g/m2or 6.6% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience No. 8

In a glass reactor 3750 grams per dry pigment calcium carbonate type Finnish marble with a grain size distribution such that 65 wt.% particles have a diameter less than 1 micron, a specific device Sedigraph 5100 of the company Micromeritics, 75.0 wt.% (calcium carbonate in the form of a slurry with a dry matter concentration of 20 wt.% and at a temperature of 60°C process using phosphoric acid in the form of a 5 wt.%-aqueous solution, corresponding to 0.5 mol H3O+per mole of caso3. Then through the sludge bubbled CO2at atmospheric pressure for 2 hours so that the ratio (volume of suspension: volume of gaseous CO2) was 1:0,1.

After conditioning for 24 hours to form sheets of paper according to the same method as in experiment No. 1, with a mass of 75 g/m2and measure their thickness also using the same method as in experiment No. 1.

The results:

(a) pigment:

after 6 hours after completion of processing of natural calcium carbonate, according to experience, the pH value of the slurry is 7.8, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 132 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot 64,2 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win 10.8 g/m2or 14.4% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience No. 9

In a glass reactor 36 g per dry pigment calcium carbonate type Finnish marble with a grain size distribution such that 65 wt.% particles have a diameter is anise 1 micron, a particular with the help of the device Sedigraph 5100 of the company Micromeritics, from 21.6 wt.% in the form of a slurry with a dry matter concentration of 4.8 wt.%, but when the temperature is 45° C, is treated with phosphoric acid in the form of a 5 wt.%-aqueous solution, corresponding to 0.32 mol H3About+per mole of caso3. Then through the sludge bubbled CO2at atmospheric pressure for 5 hours so that the ratio (volume of suspension:volume of gaseous CO2) was 1:0.05 is taken.

After conditioning for 24 hours to form sheets of paper according to the same method as in experiment No. 1, with a mass of 75 g/m2and measure their thickness also using the same method as in experiment No. 1.

The results:

(a) pigment:

later, 8 hours after completion of processing of natural calcium carbonate, according to experience, the pH value of the slurry was 8.1, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 126 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot of 67.1 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win 7.9 g/m2or 10.5% in relation to the paper pulp, which means significant the percent savings in relation to the environment.

Measurement of abrasion gives the value of 1.7 mg, which should be compared with the amount of abrasion of the control sample, component 4,5 mg

Experience No. 10

In a glass reactor 36 g per dry pigment calcium carbonate type Finnish marble with a grain size distribution such that 65 wt.% particles have a diameter less than 1 micron, a specific device Sedigraph 5100 of the company Micromeritics, from 21.6 wt.% in the form of a slurry with a dry matter concentration of 4.8 wt.% and the temperature at this time 90° is treated with phosphoric acid in the form of a 5 wt.%-aqueous solution, corresponding to 0.32 mol H3About+per mole of caso3. Then through the sludge bubbled CO2at atmospheric pressure for 5 hours so that the ratio (volume of suspension:volume of gaseous CO2) was 1:0.05 is taken.

After conditioning for 24 hours to form sheets of paper according to the same method as in experiment No. 1, with a mass of 75 g/m2and measure their thickness also using the same method as in experiment No. 1.

The results:

(a) pigment:

2 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry is 7.5, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 13 mm weight 75 g/m 2;

for the prototype: 125 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot of 67.7 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win at 7.3 g/m2or 9.7% in relation to the paper pulp, which means significant savings in relation to the environment.

Measuring abrasion using the device Einlehner type 2000 gives the value of 2.0 mg, which should be compared with the amount of abrasion of the control sample, component 4,5 mg

The above experiments show that the advantages of the invention consist in the reduction of weight for an identical thickness and to reduce abrasion, and better smoothness when the best white and also achieve better retention of filler.

Experience No. 11

In the reactor of 40 m3and a height of 12 m 3600 kg per dry pigment calcium carbonate type Carrara marble with a grain size distribution such that 65 wt.% particles have a diameter less than 1 micron, a specific device Sedigraph 5100 of the company Micromeritics, from 28.6 wt.% (calcium carbonate) in the form of a slurry with a concentration of dry matter of 24.8 wt.% and at a temperature of 55° is treated with phosphoric acid in the form of 10 wt.%-aqueous solution, corresponding to 0.30 mol H3About+per mole of caso3. In parallel reactions, and then through the sludge in t the value of 5 hours bubbled CO 2by internal recirculation of CO2and injection of CO2in the lower part of the reactor at high pressure 1.2 bar so that the ratio (volume of suspension:volume of gaseous CO2) was 1:5.

After conditioning for 24 hours to form sheets of paper according to the same method as in experiment No. 1, with a mass of 75 g/m2and measure their thickness also using the same method as in experiment No. 1.

The results:

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry is 7.7, which means the absence of any stability towards acids.

BET specific surface is 35.5 m2/, This measurement of the specific surface BET conducted by BET method in accordance with the norm ISO 9277, namely the measurement is carried out by cooling in liquid nitrogen in a stream of nitrogen on the sample dried to constant mass and temperature-controlled at a temperature of 250° C, for one hour in nitrogen atmosphere. These conditions correspond to those norms, in particular, called the norm ISO 9277 in the claims;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 126 μm with a weight of 75 g/m2that casting in which the mask thickness 113 μm gives a lot to 67.3 g/m 2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win 7.7 g/m2or 10.3% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience No. 12

This experience illustrates the invention and relates to an example of layering up different masses on the plastic media using, on the one hand, nalivaeva sludge with low concentrations of untreated fillers and, on the other hand, sludge with a low concentration of processed according to the invention fillers.

Follow the common methodology experience 11 for processing sludge from 17.2% (based on dry substance of powdered calcium carbonate and from 0.5 wt.% polyacrylate dispersant type up to obtain a particle size distribution such that 65% of the particles have a diameter less than 1 micrometer, a particular with the help of the device Sedigraph 5100 of the company Micromeritics.

Protocol experience of layering is to implement layering using machines for coating paper type Erichsen Bechcoater™ on a sheet of semi-plastic, manufactured by Muhlebach, Switzerland.

Two used nakaweesi salt solution have a composition comprising 100 parts of the slurry of the test pigment and 12 parts latex based on styrene/acrylate, manufactured by BASF under the name ACRONAL S 360 D™ .

In what erom case, the slurry of the pigment, experienced, corresponds to the raw sludge of calcium carbonate from 17.2% (based on dry substance of crushed calcium carbonate with 0.5 wt.% polyacrylate dispersant type and particle size distribution such that 65% of the particles have a diameter less than 1 micrometer, identified through the device Sedigraph 5100 of the company Micromeritics.

In the second case, the slurry of pigment that experience, meets the sludge from 17.2% (based on dry substance of calcium carbonate, the calcium carbonate treated by the above method.

The results of the thickness measurements in the case of three related experiments: first, when using a plastic base, and the other when using the basics covered in mud above the untreated calcium carbonate, and finally, the third when using the basics covered in mud above the treated calcium carbonate, are presented below in table. And figure 2

The above table shows that:

in the absence of layering paper thickness is 79,59;

in the case of the classical layering thickness of the paper only comes to 81,19 weight 4,78 g/m2;

in the case of layering by using the compositions according to the invention the thickness of the paper greatly increases up to 95,19 weight 4,28 g/m2.

The thickness of the applied layer is produced simply by the difference between the thickness of the coated paper and one uncoated paper.

The increase in the thickness of the applied layer, therefore, is 15.6 μm between layering by using the product according to the invention and untreated paper (95,19 towards 79,59), the thickness of the paper is 79,59 for mass 4,28 g/m2against only 1.6 between layering with classical compositions and raw paper (81,19 towards 79,59) for mass 4,78 g/m2.

The increase of thickness is expressed by the so-called property "volume"), hence, using the composition according to the invention is roughly 10 times faster for about the same weight.

The same type of calculation for different masses allows you to draw a plot of the thickness (in micrometers) from weight (g/m2(see figure 2)

Interpretation the above graph allows you to see that in the control experiment, i.e. the experience with the untreated control sample, the slope of the thickness of the applied layer is 0.5 μm· g-1·m-2while in the experience according to the invention the slope of the thickness of the applied layer is 3.5 μm· g-1·m-2.

It is seen that attain hence much better coverage (opaque layer) sheet, much better machinability("kalandrakas") and high porosity due to the use of the product according to the present invention.

Experience No. 13

This experience illustrates the invention and uses 150 g per dry matter of sludge on the filter calcium carbonate type of Norwegian marble with a grain size distribution such that 65% of the particles have a diameter less than 1 micrometer determined by measuring the device Sedigraph 5100 containing 0.5 wt.% calculated on dry substance of sodium polyacrylate with a specific viscosity equal to 0.75, which is diluted to a concentration of 20% with water. Then prepare 1 litre of product in a glass reactor and heated to a temperature of 70° C. for 1 hour and added dropwise amount of hydrochloric acid in the form of a 10%aqueous solution, corresponding 0,507 mol H3About+per mole of caso3. Then the resulting product is again within 30 minutes enter into interaction with CO2due to internal recirculation CO2and injection of CO2in the lower part of the reactor, after which it is kept in a horizontal position on two rotating cylinders when the pH value is equal to 7.6.

After conditioning for 24 hours to form the sheets of paper in the same way as in experiment No. 1, with a mass of 75 g/m2then measure their thickness also using the same methodology as in experiment No. 1.

The results:

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry composition is yet 7,6, that means no resistance against acids;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 114 μm with a weight of 75 g/m2;

for the prototype: 120 mm weight 75 g/m2that casting to the magnitude of the thickness of 114 μm gives a lot 71,2 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 114 μm, achieve win 3.8 g/m2or 5% in weight of the paper, which means significant savings in relation to the environment.

Experience No. 14

This experience illustrates the invention and uses 150 g per dry matter of sludge on the filter calcium carbonate type of Norwegian marble with a grain size distribution such that 65% of the particles have a diameter less than 1 micrometer determined by measuring the device Sedigraph 5100 containing 0.5 wt.% calculated on dry substance of sodium polyacrylate with a specific viscosity equal to 0.75, which is diluted to a concentration of 20% with water. Then prepare 1 litre of product in a glass reactor and heated to a temperature of 70° C. for 1 hour and added dropwise amount of oxalic acid with two moles of water of crystallization (2 H3About+in the form of a 10%aqueous solution, corresponding 0,335 mol H3About+per mole of caso3.

Then the product it is within 30 minutes of being in interaction with CO 2due to internal recirculation CO2and injection of CO2in the lower part of the reactor and maintain it in a horizontal position on two rotating cylinders when the pH value is equal to 7.7.

After conditioning for 24 hours to form the sheets of paper in the same way as in experiment No. 1, with a mass of 75 g/m2then measure their thickness also using the same methodology as in experiment No. 1.

The results:

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry is 8.0, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, control: 114 μm with a weight of 75 g/m2;

for the prototype: 121 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 114 μm gives a lot of 70.4 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 114 μm, achieve win at 4.6 g/m2or 6.1% in relation to the paper pulp, which means significant savings in relation to the environment.

EXAMPLE 2

This example relates to the handling slurries with high solids content.

To implement this in all the experiments of example 2 is prepared mineral in the form of an aqueous suspension (slurry), solids or dry matter in to the ora can reach up to 80 wt.%, or in the form of sediment on the filter, or in the form of a dry powder, in an appropriate reactor and, if necessary, diluted until the desired solids content by using demineralized water or tap water.

Experience No. 15

For this experience, illustrating the prior art, to prepare the aqueous composition is injected into the mixer and mixing:

- 750 g dry substance Norwegian marble with a grain size distribution such that 75% of the particles have a diameter less than 1 μm, determined by measuring the device Sedigraph 5100;

- 250 g per dry matter originating from the Finnish talc with a grain size distribution such that 45% of the particles have a diameter less than 2 μm, determined by measuring the device Sedigraph 5100;

5 g dry substance acrylic binder, consisting of 90 wt.% acrylic acid and 10 wt.% christianfundamentalist with 25 moles of ethylene oxide;

- the amount of water necessary for the formation water compositions with a 65%concentration of dry substance.

After stirring for 30 minutes and education joint structure between the grains of marble and talc with a binder added to 5.2 g of polyacrylate, partially neutralized with sodium hydroxide, and the specific viscosity component of 0.5, and an additional quantity of water and hydroxide is the atrium to obtain a water suspension from 59.4%concentration of dry substance.

Form sheets with a weight of 75 g/m2in the same way as in experiment No. 1, and measure their thickness also using the same methodology as in experiment No. 1. The measured thickness is 116 µm for weight 75 g/m2.

Experience 16

For this experience, illustrating the prior art, according to the same procedure as in experiment No. 1, form sheets of paper weighing 75 g/m2based on water suspension with 77,5%concentration of dry substance Norwegian marble with a grain size distribution such that 63% of the particles have a diameter less than 1 μm, determined by measuring the device Sedigraph 5100.

The measured thickness is 115 μm for weight 75 g/m2.

Determined by the same method as in experiment No. 2, and according to the standard DIN 53146, opacity is 86,4.

Determined by the same technique as in experiment No. 2, and according to the standard ISO Brightness R 457 filter Tappi, white is 88,4.

Experience No. 17

For this experience, illustrating the prior art, according to the same method as in experiment No. 1, form sheets of paper weighing 75 g/m2based on water suspension with 67,2%concentration of dry substance of the sediment on the filter type of the Norwegian marble with a grain size distribution such that 75% of the particles have a diameter less than 1 μm, determined by measuring the device Sedigraph 5100 and containing 0.5 wt.% calculated on the dry matter of the poly is relate sodium with a specific viscosity, part of 0.75.

The measured thickness is 114 µm for weight 75 g/m2.

Experience No. 18

For this experience, explaining the invention, is prepared to 4000 g of the composition of experience No. 15, which is a blend of 25 wt.% calculated on dry substance talc and 75 wt.% calculated on dry substance caso3originating from the Norwegian marble, in the form of a suspension with a concentration of dry matter equal to 59.4%in the mixer fluidized bed (device), and added dropwise within 45 minutes number of phosphoric acid in the form of a 20%aqueous solution, corresponding to 0.15 mol H3About+per mole of caso3.

After processing apparatuscontinue to rotate for one hour. This device fluidized bed, continuing to rotate, allows air exchange with the carbon dioxide released by the reaction, thus leading to the presence of carbon dioxide in the atmosphere equipment.

Then the obtained product is kept in a horizontal position on two rotating cylinders, when the pH value is equal to 7.6.

After conditioning for 24 hours to form the sheets of paper in the same way as in experiment No. 1, with a mass of 75 g/m2then measure their thickness also using the same methodology as in experiment No. 1.

The results:

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate according to the experience of the pH value of the slurry is 7.8, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (experiment No. 15): 116 μm with a weight of 75 g/m2;

for the prototype: 118 μm with a weight of 75 g/m2that casting to the magnitude of the thickness 116 μm gives a lot 73,9 g/m2.

It is seen that in this experience, if the thickness of the paper lead to a total of 116 μm, achieve win at 1.1 g/m2or 1.5% in weight of the paper, which means significant savings in relation to the environment.

Experience No. 19

For this experience, explaining the invention, prepared 3290 g songs of experience No. 16, which is a calcium carbonate originating from the Norwegian marble, in the form of a slurry with a concentration of dry matter equal to 75.8%in the mixer fluidized bed (apparatus Ldige), and added dropwise within 2 hours the amount of phosphoric acid in the form of a 20%aqueous solution corresponding to 0.5 mol H3About+per mole of caso3.

After processing apparatuscontinue to rotate for one hour. This device fluidized bed, continuing to rotate, allows air to exchange the carbon dioxide, released by the reaction, thus leading to the presence of carbon dioxide in the atmosphere equipment.

Then the obtained product is kept in a horizontal position on two rotating cylinders when the pH value is equal to 7.6.

After conditioning for 24 hours to form the sheets of paper in the same way as in experiment No. 1, with a mass of 75 g/m2then measure their thickness also using the same methodology as in experiment No. 1.

The results:

(a) pigment:

later, 7 hours after the end of the processing of natural calcium carbonate according to the experience of the pH value of the slurry is 7.6, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (experiment No. 16): 115 μm with a weight of 75 g/m2;

for the prototype: 130 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 115 μm gives a lot 66.5 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 115 μm, achieve win 8.5 g/m2or 11.3% in paper pulp, which means significant savings in relation to the environment.

Experience No. 20

For this experience, explaining the invention, a mixture of 1600 g of calcium carbonate type of Norwegian marble with a grain size distribution such that 75% of the particles have a diameter less than 1 μm, the definition of the Noi by the measurement device Sedigraph 5100, possessing certain properties, in redispersion state in the form of the precipitate on the filter is mechanically mixed with 400 g of another, different carbonate obtained according to the above experience No. 18, with a concentration of dry substance of 52.8% (see above) in the apparatus with fluidized bed (devicewithin 30 minutes, and then dispersed with 0.5 wt.% calculated on dry substance of the dispersant, which is a sodium polyacrylate with a specific viscosity equal to 0.75, then establish a concentration of 60%. Then the product is kept in a horizontal position on two rotating cylinders at pH 8.5.

After conditioning for 24 hours to form the sheets of paper in the same way as in experiment No. 1, with a mass of 75 g/m2then measure their thickness also using the same methodology as in experiment No. 1.

The results:

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry is 8.5, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, the control (experiment No. 17): 114 μm with a weight of 75 g/m2;

for the prototype: 118 μm with a weight of 75 g/m2that casting to the magnitude of the thickness 114 um dalmasso to 72.2 g/m 2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 114 μm, achieve win 2.8 g/m2or 3.7% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience no 21

For this experience, explaining the invention, 1200 g of calcium carbonate type of Norwegian marble with a grain size distribution such that 65% of the particles have a diameter less than 1 μm, determined by measuring the device Sedigraph 5100, redispersion state in the form of the precipitate on the filter is mechanically mixed with 300 g of another carbonate, processed according to the above experience No. 18, with a concentration of dry substance, part of 52.8%in the presence of water to achieve a concentration of 60%. After mechanical mixing is carried out in the mixer fluidized bed (devicewithin 30 minutes, add 500 g of talc Finnish origin and grain size distribution, such that 35% of the particles have a diameter less than 1 μm, determined by measuring the device Sedigraph 5100, and talc pre-treated with 1.2% of binder type, acrylic copolymer, and water to obtain a concentration of 60%. Again subjected to mechanical mixing for 30 minutes with injection of CO2with a flow rate of 100 ml/min and then dispersed with 0.5 wt.% calculated on dry substance policr the LVL of sodium with a specific viscosity, equal to 0.75. The product is then incubated in a horizontal position on two rotating cylinders; pH is 8.4.

After conditioning for 24 hours to form the sheets of paper in the same way as in experiment No. 1, with a mass of 75 g/m2then measure their thickness also using the same methodology as in experiment No. 1.

The results:

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry is 8.5, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, control: 114 μm with a weight of 75 g/m2;

for the prototype: 116 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 114 μm gives a lot of 73.5 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 114 μm, achieve win 1.5 g/m2or 2% in weight of the paper, which means significant savings in relation to the environment.

Experience No. 22

For this experience, explaining the invention, obtained according to the previous experience of the slurry injected CO2with a flow rate of 100 ml/min for 5 hours, then the resulting product is kept in a horizontal position on two rotating cylinders when the pH value is equal to 8.1.

After keeping for 4 hours to form the sheets of paper in the same way, as in experiment No. 1, with a mass of 75 g/m2then measure their thickness also using the same methodology as in experiment No. 1.

The results:

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry was 8.1, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, control: 114 μm with a weight of 75 g/m2;

for the prototype: 117 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 114 μm gives a lot to 73.1 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 114 μm, achieve win 1.9 g/m2or 2.5% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience no 23

For this experience, explaining the invention, cook 6000 g of calcium carbonate originating from the Norwegian marble with a grain size distribution such that 65% of the particles have a diameter less than 1 μm, determined by measuring the device Sedigraph 5100, in the form of a dispersion or slurry with a concentration of dry substance 77.8%, in the mixer fluidized bed (device) and diluted with water to a concentration of 75.7 percent. Add 0.15 mol H3About+per mole of caso3using phosphoric sour the s in the form of an aqueous 20%solution, and adding exercise dropwise within 45 minutes.

Then through the product bubbled CO2with a flow rate of 100 ml/min and for 5 hours after which the resulting product can withstand, on the one hand, within one week and, on the other hand, for 4 weeks in a horizontal position on two rotating cylinders.

The results:

(a) pigment:

3 hours later after the processing of natural calcium carbonate, according to experience, the pH value of the slurry is 7.6, after 1 week it is 7.8, as well as 4 weeks, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

after standing for 1 week form the sheets of paper in the same way as in experiment No. 1, with a mass of 75 g/m2then measure their thickness also using the same methodology as in experiment No. 1.

The results of thickness measurement:

for the original sample, control: 115 μm with a weight of 75 g/m2;

for the prototype: 119 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 115 μm gives a lot to 72.2 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 115 μm, achieve win 2.8 g/m2or 3.7% in relation to the paper pulp, which means significant savings in relation to the environment.

After in the derivare for 4 weeks form the sheets of paper in the same way, as in experiment No. 1, with a mass of 75 g/m2then measure their thickness also using the same methodology as in experiment No. 1.

The results of thickness measurement:

for the original sample, control: 115 μm with a weight of 75 g/m2;

for the prototype: 119 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 115 μm gives a lot to 72.2 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 115 μm, achieve win 2.8 g/m2or 3.7% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience no 24

This experience explains the invention and the recycling of carbon dioxide with the help of a mixer rotor/stator type of Silversea.

In a pilot unit volume of 1 m3and a height of 2 m in a reactor equipped with a mixer of Silversea, first enter 284 l of sludge with a concentration of 27% (based on dry substance of natural calcium carbonate originating from Carrara marble with a grain size distribution such that 65% of the particles have a diameter less than 1 μm, determined by measuring the device Sedigraph 5100, at a temperature of 62° that is diluted by the amount of water required to obtain a suspension with a concentration of 23.1% (based on dry substance, then mixed with a quantity of H3RHO4in the form of a 50%aqueous solution, corresponding to 0.26 mol H3About+on the ol, caso 3. The temperature at the beginning of the addition of an acid, which lasts 1 hour and 45 minutes, is 52° C. the addition is carried out manually from a glass. The amount of water added with the acid, leads to the sludge with a concentration of 15.8% in dry substance.

The slurry is then treated for 4 hours with 60 kg derived from recycling CO2in the tank of about 50 l with stirring using a stirrer of Silversea.

The results:

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry is 7.7, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, control: 117 μm with a weight of 75 g/m2;

for the prototype: 126 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 117 μm gives a lot to 69.6 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 117 μm, achieve win at 5.4 g/m2or 7.2% in paper pulp, which means significant savings in relation to the environment.

Experience no 25

This experience explains the invention and the processing of waste through breaks when layering".

With this purpose, to obtain the concentration of waste due to breaks when n is slavanie" 10 wt.% is dispersed in water with stirring and within 30 minutes 800 g of waste due to breaks when layering" quality 100 g/m 2with a filler content of about 15 wt.%, corresponding to 120 g per dry matter of natural calcium carbonate such as the Finnish marble with a grain size distribution such that 35% of the particles have a diameter less than 1 μm, determined by measuring the device Sedigraph 5100, and a layer of 25 g/m2on the surface and 400 g per dry weight of natural calcium carbonate such as the Finnish marble with a grain size distribution such that 80% of the particles have a diameter less than 1 μm, determined by measuring the device Sedigraph 5100, and the marble crushed with the use of 0.8% (based on dry weight of sodium polyacrylate as a dispersant and agent for grinding and styrene-butadiene latex as a binder for the layup.

After dispersion in a glass reactor with a capacity of 10 liters and under stirring the slurry with a concentration of dry substance 10 wt.% and at a temperature of 55°C is treated with phosphoric acid in the form of a 50 wt.%-aqueous solution, corresponding to 0.4 mol H3O+per mole of caso3. Then through the sludge and fiber bubbled CO2at atmospheric pressure for 5 hours so that the ratio (volume of suspension:volume of gaseous CO2) was 1:0,1.

Sheets of paper were produced in the same way as in the pre is idusa experiments, by mixing processed "waste due to breaks when layering" with fresh fibers so as to obtain a filler content of 20 wt.% in the final paper.

Results;

(a) pigment:

5 hours after the end of the processing of natural calcium carbonate, according to experience, the pH value of the slurry on the basis of "waste due to breaks when layering" is 7.6, which means the absence of any stability towards acids;

b) for paper:

thickness measurement:

for the original sample, control (obtained as the sample without treatment with acid and gaseous CO2): 115 μm with a weight of 75 g/m2;

for the prototype: 123 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 115 μm gives a lot to 70.1 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 115 μm, achieve win 4.9 g/m2or 6.5% in relation to the paper pulp, which means significant savings in relation to the environment.

Experience No. 26

For this experience, explaining the invention, prepared 447 kg compositions of experience No. 16, which is a calcium carbonate originating from the Norwegian marble, in the form of a suspension with a concentration of dry matter equal to 75.8%in the mixer fluidized bed (device) and added dropwise within 2 hours the amount of phosphoric acid in the form of a 20%aqueous solution, corresponding to 0.3 mol H3About+per mole of caso3.

After treatment with phosphoric acid product was incubated for 3 hours, the period during which process with the help of CO2due to internal recirculation of gaseous CO2.

Then the product is kept in a horizontal position on two rotating cylinders and after 5 hours, the pH value is 7.8.

After conditioning for 24 hours to form the sheets of paper in the same way as in experiment No. 1, with a mass of 75 g/m2but with the filler in the form of a 25% pigment, and then measure their thickness also using the same methodology as in experiment No. 1.

BET specific surface determined by the same method as in experiment No. 11, is 11.5 m2/year

The results of thickness measurements the following:

for the original sample, the control (experiment No. 13 with a filler in the form of a 25% pigment ): 114 μm with a weight of 75 g/m2;

for the prototype: 119 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 114 μm gives a lot 71,8 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 114 μm, achieve win 3.2 g/m2or 4.3% in relation to the paper pulp, which means significant savings in relation to the environment.

The results of the measurement of the breaking length defined according to the standard DIN EN ISO 194-2, includes DIN 53112-1:

for the original sample, the control (experiment No. 13 with a filler in the form of a 25% pigment): 2,22 km;

for a test sample with a filler in the form of a 25% pigment: 2,54 km, which means an increase in breaking length of 14.4% compared to the raw product with a weight of 75 g/m2.

In addition, the tensile strength determined according to DIN EN ISO 1924-2, size 15 mm 28 N in the case of the test sample against only 24,5 N for the control sample.

The opacity is determined by the same technique as in experiment No. 2 and according to the standard DIN 53146, is 86.6.

White, determined by the same technique as in experiment No. 2 and according to the standard ISO Brightness R 457 filter Tappi is 89,0.

Experience no 27

For this experience, explaining the invention, prepared 447 kg compositions of experience No. 16, but with the granules, in which case only 40% of the particles have a diameter less than 1 μm, determined by measuring the device Sedigraph 5100, in the form of a slurry of calcium carbonate originating from the Norwegian marble with a concentration of dry matter equal to 75.8%in the mixer fluidized bed (device) and added dropwise within 2 hours the amount of phosphoric acid in the form of a 20%aqueous solution, corresponding to 0.3 mol H3About+per mole of caso3.

Then the obtained product you who eribaum in a horizontal position on two rotating cylinders when the pH value, equal to 7.6.

After conditioning for 24 hours to form sheets of paper according to the same method as in experiment No. 1, with a mass of 75 g/m2but with the filler in the form of a 25% pigment, and measure their thickness also using the same method as in experiment No. 1.

BET specific surface, determined according to the method, as in experiment No. 11, is 9.8 m2/year

The results of thickness measurement:

for the original sample, the control (experiment No. 11 with a filler in the form of a 25% pigment ): 114 μm with a weight of 75 g/m2;

for the prototype: 121 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 114 μm gives a lot of 70.7 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 114 μm, achieve win at 4.3 g/m2or 5.7% in relation to the paper pulp, which means significant savings in relation to the environment.

The results of the measurement of the breaking length defined according to the standard DIN EN ISO 1924-2, including DIN 53112-1, the following:

for the original sample, the control (experiment No. 11 with a filler in the form of a 25% pigment): 2.30 km;

for a test sample with a filler in the form of a 25% pigment: 2,48 km, which means an increase in breaking length by 8.7% compared with the untreated product, with a weight of 75 g/m2.

In addition, the tensile strength determined according to DIN EN ISO 1924-2, size 15 mm, the leaves 27,3 N in the case of the test sample against only 24,5 N to control.

The opacity is determined by the same method, and that such experience # 2 and according to the standard DIN 53146, is 87,7.

White, determined by the same method, and that such experience # 2 and according to the standard ISO Brightness R 457 filter Tappi is 89,0.

This same pattern according to the experience then put on a paper derived from wood, of a thickness of 53 μm and a mass equal to 32.9 g/m2±0,39%, from laboratory machines for coating paper (Helicoater company Dixson).

Short head "dwell" is used at an angle to the plate 45°. Speed layering is 800 m/S.

Used Nastavenie salt solutions have a composition that includes 100 hours/one hundred of the test pigment, 12 h/hundred latex (DL 966 styrene/butadiene type) and 0.5 h/hundred CMC (Finnfix FF5) and with a dry matter content of 56.6 per cent.

The results:

- the thickness of the uncoated paper: 53 microns;

- the thickness of the coated paper with a weight of 7 g/m2in the case of the control sample experience no 13: 56 microns;

- the thickness of the coated paper with a weight of 7 g/m2in the case of this experience, according to the invention: 59 microns;

the thickness of the applied layer with a mass of 7 g/m2in the case of the control sample experience No. 13: 3 μm;

the thickness of the applied layer with a mass of 7 g/m2in the case of this experience: 6 microns.

These results allow to conclude that the thickness nanesena what about the layer can be increased two times compared to control.

EXAMPLE 3

This example relates to the use of inkjet printing ("ink jet") treated and untreated calcium carbonate used as a filler ("filler") paper pulp.

Natural calcium carbonate type of Norwegian marble with a grain size distribution such that 75 wt.% particles have a diameter less than 1 micrometer, defined with the help of the device Sedigraph 5100™ company Micromeritics™ in the form of a filtercake in the amount of 0.5 kg per dry pigment is diluted in a container with a capacity of 10 liters with distilled water until obtaining a slurry with a dry matter concentration of 15 wt.%. Then, the thus obtained slurry is treated with 10% phosphoric acid 10 wt.%-aqueous solution at a temperature of 65° under stirring for 20 minutes at speed (mixer), 500 revolutions per minute. After 15 minutes the suspension of calcium carbonate for 1 hour bubbled CO2.

After ozonation form the sheets of paper containing as a filler suspension, also called the sludge, the test of calcium carbonate.

To accomplish this, produce the sheets of paper from a slurry or paste of cellulose mark SR 23 containing paste from sulfate wood and fibers, consisting of 80% birch and 20% pine. Then 45 g per dry matter of the slurry or paste is diluted in 10 litres of water is the presence of about 15 g of the test composition fillers to obtain experimentally the content of the filler is from 20% to nearly 0.5%. After stirring for 15 minutes and add to 0.06 wt.% in relation to the dry weight of the paper retention agent polyacrylamide type form a sheet with a mass equal to 75 g/m2and filled at (20±0,5%). Used for forming the sheet, the device is a system of Rapid-are Kothen, model 20.12 MS company Naude.

Thus, the formed sheet is dried for 400 seconds at a temperature of 92° and in vacuum 940 mbar.

The content of the filler is controlled by analysis of the ash.

Measure the thickness of the thus obtained sheet. The thickness of the paper or cardboard sheet represents the perpendicular distance between two parallel surfaces.

Samples were kondicionirovanie within 48 hours (according to the German norm DIN EN 20187).

This provision determines that the paper is a hygroscopic substance, and as such has the property that consists in the ability to change its moisture content in accordance with the humidity of the ambient air. The moisture is absorbed, when increasing the humidity of the surrounding atmosphere, and, on the contrary, is deleted when decreasing the humidity of the surrounding atmosphere.

Even if the relative humidity remains constant, the moisture content in the paper do not necessarily remains the same if the temperature is maintained constant in the definition of the data within. During increase or decrease of moisture content on physical properties of paper are modified.

On this basis, the samples should be conditioned for at least a time period of 48 hours until reaching equilibrium. Samples were also tested under identical climatic conditions.

The atmosphere of the experience in the case of paper was installed so that it meets the following data:

relative humidity of 50% (±3)

the temperature of 23° With (±1)

The thickness was determined according to the German norm DIN EN 20534 when using a micrometer, test print ("test print") which comes to 10 n/cm2. The result of the experiment was determined by calculating the average of 10 measurements. The result is expressed in micrometers. The control sample is paper made in parallel in the same way, with the same amount of filler, but raw, with a mass of 75 g/m2and with the same number (same brand) pulp.

The results:

a) pigment:

after 12 hours after treatment, natural calcium carbonate, as in this example, the pH value of the slurry (paste) is 7.2, which means the absence of any stability towards acid;

b) paper:

the results of thickness measurement:

for the original sample, control: 112 microns, with a weight of 75 g/m2;

for the prototype: 120 mm weight 75 g/is 2that casting to the magnitude of the thickness of 112 μm gives a weight of 70 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 112 μm, achieve win in 5 g/m2or 6.6% in relation to the paper pulp, which means significant savings in relation to the environment.

Specifications printing:

If you perform inkjet printing, comparing the product of the prior art (figure) and according to this experience, in accordance with the invention (figure A), in the device for inkjet printers EPSON brand™ Stylus COLOR 500™ we can see that the fingerprint according to the invention is much clearer (see drawing).

EXAMPLE 4

This example relates to the use of inkjet printing ("ink jet") treated and untreated calcium carbonate used for the operation layering paper and as a filler for paper pulp.

Natural calcium carbonate type of Norwegian marble with a grain size distribution such that 75 wt.% particles have a diameter less than 1 micron, a specific device Sedigraph 5100™ company Micromeritics™ in the form of a filtercake in the amount of 0.5 kg per dry pigment is diluted in a container with a capacity of 10 liters with distilled water until obtaining a slurry with a dry matter concentration of 15 wt.% Then, the thus obtained slurry is treated with 10% phosphoric acid 10 wt.%-nagrastar at a temperature of 65° With under stirring for 20 minutes at speed (mixer), 500 revolutions per minute. After 15 minutes the suspension of calcium carbonate for 1 hour bubbled CO2.

Protocol layering:

use the same Protocol as in the above experience 27, namely the prototype then put on a paper derived from wood, of a thickness of 53 μm and a mass equal to 32.9 g/m2±0,39%, from laboratory machines for coating paper (Helicoater™ firm Dixson™ ).

Short head "dwell" is used at an angle to the plate 45°. Speed layering is 800 m/S.

Used Nastavenie salt solutions have a composition that includes 100 hours/one hundred of the test pigment, 12 h/hundred latex (DL 966 styrene/butadiene type) and 0.5 h/hundred CMC (Finnfix FF5™ ) and with a dry matter content of 56.6 per cent.

Samples were kondicionirovanie within 48 hours (according to the German norm DIN EN 20187). This provision determines that the paper is a hygroscopic substance, and as such has the property that consists in the ability to change its moisture content in accordance with the humidity of the ambient air. The moisture is absorbed, when increasing the humidity of the surrounding atmosphere, and, on the contrary, is deleted when decreasing the humidity of the surrounding atmosphere.

Even if the relative humidity remains constant is nnom level, the moisture content in the paper do not necessarily remains the same if the temperature is maintained constant within certain limits. During increase or decrease of moisture content on physical properties of paper are modified.

On this basis, the samples should be conditioned for at least a time period of 48 hours until reaching equilibrium. Samples were also tested under identical climatic conditions.

The atmosphere of the experience in the case of paper was installed so that it meets the following data:

relative humidity of 50% (±3)

the temperature of 23° With (±1)

The thickness was determined according to the German norm DIN EN 20534 when using a micrometer, test print ("test print") which comes to 10 n/cm2. The result of the experiment was determined by calculating the average of 10 measurements. The result is expressed in micrometers. The control sample is paper made in parallel in the same way, with the same amount of filler, but raw, with a mass of 75 g/m2and with the same number (same brand) pulp.

The results:

a) pigment:

after 12 hours after treatment, natural calcium carbonate, as in this example, the pH value of the slurry (paste) is 7.2, which means the absence of any stability towards acid.

b) paper:

the results is serenia thickness:

for the original sample, control: 112 microns, with a weight of 75 g/m2;

for the prototype: 120 mm weight 75 g/m2that casting to the magnitude of the thickness of 112 μm gives a weight of 70 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 112 μm, achieve win in 5 g/m2or 6.6% in relation to the paper pulp, which means significant savings in relation to the environment.

Measurement of density printing was carried out according to the following method and the results are presented in table 1.

Optical density is a measure of the density in the reflected light image. According to the methodology, developed mainly by manufacturer Hewlett-Packard Corporation (HP)™ specific pattern printed on paper and using a densitometer to measure the optical density of the reflected light (Macbeth RD 918 ™ ) measure the optical density in the case of pure black, composite black and blue-green, Magenta, and yellow.

If only there is no opposite directions, this Protocol is suitable for all examples, including this dimension.

Carry out experiments according to table 1 for pulp and paper basis or on special paper when using the product, consisting of 100 parts of the test pigment, 15 parts of polyvinyl alcohol (PVA), 5 parts of additive is K-130 firms Stockhausen, moreover, the filler is one with a specific surface area of 70 m2/g attributable to the category of coarse filler with a high specific surface area.

Layering is performed using the device Erichsen bench coater ™ on paper, such as shown in table 1.

The first two experiences table 1 correspond to the uncoated pigment paper (pasted starch to the surface in the paper machine).

The following two experiences match the paper treated with synthetic silicates. Shows that you need to use special paper to achieve good optical density.

Two recent experience match the paper coated with the composition according to the invention. It is seen that according to the invention is comparable to the density of the fingerprint, you can use normal paper for inkjet printing, and not more expensive special paper.

In fact, state that the invention is far superior to the uncoated paper (1,40 compared to 1.20 and of 1.39 compared to 1,30), and that the value of 1.40, obtained according to the invention in the case of normal paper, it is absolutely comparable with the value of 1.40, obtained according to the prior art, but in the case of a special paper.

TABLE 1.

Density measurement inkjet printing the tee (the results of the experiments: the average of 15 measurements)
PaperPrintingAdjustmentsThe print density In (black)The print density (blue-green)The print density M (Magenta)The print density Y (yellow)
Muhlebach Multiline TopHP desk jet 895 Cxinormal paper1,921,381,401,30
Muhlebach

Multiline Top
Epson Stylus Color 500normal paper1,741,501,281,20
Epson Ink Jet paper 720 dpiHP deskjet 895 Cxithe inkjet paper with high gloss (white)1,951,381,231,08
Epson Ink

Jet Papier 720 dpi
Epson Stylus Color 500specially coated paper-720 dpi1,941,801,55the 1.44
The coating according to the inventionHP deskjet 895 Cxinormal paper1,94of 1.571,591,39
The coating according to the inventionEpson Stylus Color 500normal paper1,801,701,461,40

EXAMPLE 5

This example relation is seeking to use processed and unprocessed calcium carbonate coarse particles, but with a high specific surface, used as a filler in paper.

To accomplish this, natural calcium carbonate type of Norwegian marble with a grain size distribution such that 65 wt.% particles have a diameter less than 1 micrometer, defined with the help of the device Sedigraph 5100™ company Micromeritics™ and specific surface area BET, part of 15.5 m2/g (determined by BET method according to the standard ISO 9277), in the amount of 0.5 kg per dry pigment is diluted in a container with a capacity of 10 liters in the form of a dispersion or slurry with a concentration of dry matter equal to 75%, then diluted with water until obtaining a slurry with a dry matter concentration of 20 wt.% Then, the thus obtained slurry treated with 20% or 30% or 40% phosphoric acid in the form of 10 wt.%-aqueous solution at a temperature of 65° C, slightly stirring, with a flow rate of 30 l/min at atmospheric pressure in the lower part of the container and within 2 hours. After 2 hours, the suspension of calcium carbonate for 1 hour bubbled CO2.

The filler has the following characteristics:

Example 5A: phosphoric acid, 20%:

(a) pigment:

- the average grain diameter determined visually under an electron microscope: 7 micrometers;

- BET specific surface (determined by BET method according to the standard ISO 9277): 38,5 m2/g;

b) for paper:

is serenia thickness:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 133 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot of 63.7 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win 11.3 g/m2or 15% in weight of the paper, which means significant savings in relation to the environment.

Example 5B: phosphoric acid, 30%:

(a) pigment:

- the average grain diameter determined visually under an electron microscope: 9 micrometers;

- BET specific surface (determined by BET method according to the standard ISO 9277): 44,2 m2/g;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 139 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot 61,0 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win in 14.0 g/m2or 18.7% in relation to the paper pulp, which means significant savings in relation to the environment.

Example 5C: phosphoric acid, 40%:

(a) pigment:

- the average grain diameter determined visually under an electron microscope: 13 Microm the TRS;

- BET specific surface (determined by BET method according to the standard ISO 9277): 58.4 m2/g;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 152 microns, with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot of 55.7 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win in 19.3 g/m2or 25.7% in relation to the paper pulp, which means significant savings in relation to the environment.

EXAMPLE 6

This example applies to ongoing continuous process for the preparation of the product according to the invention and use of treated or untreated calcium carbonate coarse particles, but with a high specific surface area BET, used as a filler in paper.

To accomplish this, natural calcium carbonate type of Norwegian marble with a grain size distribution such that 65 wt.% particles have a diameter less than 1 micrometer, defined with the help of the device Sedigraph 5100™ company Micromeritics™ and specific surface area BET, part of 15.5 m2/g (determined by BET method according to the standard ISO 9277), in the amount of 100 kg per dry pigment in the form of a dispersion or slurry with a concentration of dry matter, rawney%, with the dispersant of the type of sodium polyacrylate in a container with a capacity of 3000 litres diluted with water until obtaining a slurry with a dry matter concentration of 10 wt.% Then, the thus obtained slurry is treated with 10% or 20% or 30% phosphoric acid in the form of approximately 15 wt.%-aqueous solution at a temperature of 65° continuously in 4 chambers with a capacity of 25 liters, measuring 1/4 of phosphoric acid in each chamber, stirring slightly, and with a flow rate of 50 l/min at atmospheric pressure in the lower part of each chamber. Retention of the product in each of the chambers is 15 minutes.

The filler has the following characteristics:

Example 6A: phosphoric acid, 10.0%per:

(a) pigment:

the concentration of sludge: 7,8%;

- the average grain diameter, measured by a Sedigraph instrument 51 t )

- BET specific surface (determined by BET method according to the standard ISO 9277): 36,0 m2/g;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 123 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot 68,9 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win at 6.1 g/m2or 8.1% in relation to the paper pulp, which means significant savings in relation to the he environment.

Example 6B: phosphoric acid, 19.1%of:

(a) pigment:

the concentration of sludge: 7,8%;

- the average grain diameter determined visually under an electron microscope: 12 micrometers;

- BET specific surface (determined by BET method according to the standard ISO 9277): 49,9 m2/g;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 135 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot of 62.8 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win 12.2 g/m2or 16.6% in relation to the paper pulp, which means significant savings in relation to the environment.

Example 6C: phosphoric acid, 30%:

(a) pigment:

the concentration of sludge: 17,9%;

- the average grain diameter determined visually under an electron microscope: 12 micrometers;

- BET specific surface (determined by BET method according to the standard ISO 9277): 545,7 m2/g;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 158 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot of 53.6 g/m2.

It is seen that the experiences, if the thickness of the paper lead to the total value of 113 μm, achieve win 21.4 g/m2or 28.5% in relation to the paper pulp, which means significant savings in relation to the environment.

Example 6D

This example applies to ongoing continuous process for the preparation of the product according to the invention and use of treated or untreated calcium carbonate coarse particles, but with a high specific surface area BET, used as a filler in paper.

To accomplish this, natural calcium carbonate type of Norwegian marble with a grain size distribution such that 65 wt.% particles have a diameter less than 1 micrometer, defined with the help of the device Sedigraph 5100™ company Micromeritics™ and specific surface area BET, part of 15.5 m2/g (determined by BET method according to the standard ISO 9277), in the amount of 100 kg per dry pigment in the form of a dispersion or slurry with a concentration of dry matter equal to 75%, dispersant type polyaspartate sodium in a container with a capacity of 3000 litres diluted with water until obtaining a slurry with a dry matter concentration of 10 wt.% Then, the thus obtained slurry is treated with 10% or 20% or 30% phosphoric acid in the form of approximately 15 wt.%-aqueous solution at a temperature of 65°C continuously for 4 cameras with a capacity of 25 liters, measuring 1/4 phosphoric acids, each of the second camera, slightly stirring and with a flow rate of 50 l/min at atmospheric pressure in the lower part of each chamber. Retention of the product in each of the chambers is 15 minutes.

The filler has the following characteristics:

(a) pigment:

the concentration of sludge: 8,9%;

the average grain diameter, determined by means of a device Sedigraph 5100™ company Micromeritics™ : 1.9 micrometers;

- BET specific surface (determined by BET method according to the standard ISO 9277): 39,1 m2/g;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 113 μm with a weight of 75 g/m2;

for the prototype: 123 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 113 μm gives a lot of 68.8 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 113 μm, achieve win 6.2 g/m2or 8.1% in relation to the paper pulp, which means significant savings in relation to the environment.

EXAMPLE 7

This example refers to the use of a mixture of treated and untreated calcium carbonate as filler paper pulp.

a) Preparation of the treated pigment:

Natural calcium carbonate type of Norwegian marble with a grain size distribution such that 65 wt.% particles have a diameter less than 1 micrometer, defined with the help of the device Sedigraph 5100™ the Irma Micromeritics™ and a specific surface area BET, part 8.4 m2/g (determined by BET method according to the standard ISO 9277), in the amount of 0.6 kg per dry pigment is diluted in a container with a capacity of 1 l in the form of a dispersion or slurry with a concentration of dry matter equal to 20%, then diluted with water until obtaining a slurry with a concentration of dry matter of 10.2 wt.% Then, the thus obtained slurry is treated with 70% phosphoric acid 10 wt.%-aqueous solution at a temperature of 60° C, under stirring and in the course of 1 hour. After 1 hour through the suspension of calcium carbonate for 0.5 hours bubbled CO2.

b) preparation of a mixture of treated and untreated pigment:

Mixed under stirring for 15 minutes. The filler has the following characteristics:

Example 7A: 100% processed pigment

(a) pigment:

- grain size distribution such that 21 wt.% particles have a diameter less than 1 micrometer, which is determined with the help of the device Sedigraph 5100™ company Micromeritics™ ;

- BET specific surface (determined by BET method according to the standard ISO 9277): 44,5 m2/g;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 115 μm with a weight of 75 g/m2;

for the prototype: 162 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 115 μm gives a weight of 5.2 g/m 2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 115 μm, achieve win 22.7 g/m2or 30.3 per cent in relation to the paper pulp, which means significant savings in relation to the environment.

Example 7B: 21,5% of the treated pigment according to example 7A and 78.5% of the untreated pigment

Result

(a) pigment:

- grain size distribution such that 63 wt.% particles have a diameter less than 1 micrometer, which is determined with the help of the device Sedigraph 5100™ company Micromeritics™ ;

- BET specific surface (determined by BET method according to the standard ISO 9277): 15,5 m2/g;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler):

115 μm with a weight of 75 g/m2;

for the prototype: 124 microns, with a weight of 75 g/m2that casting to the magnitude of the thickness of 115 μm gives a lot of 69.5 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 115 μm, achieve win 5.5 g/m2or 7.3% in relation to the paper pulp, which means significant savings in relation to the environment.

Example 7C: 35,5% of the treated pigment according to example 7A and 64.5% of the raw pigment

a) a mixture of pigments:

- grain size distribution such that 60,0 wt.% particles have a diameter less than 1 micrometer, which is determined with the help of the device Sedigraph 5100™ the company Micromeritics™ ;

- BET specific surface (determined by BET method according to the standard ISO 9277): 20,0 m2/g;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 115 μm with a weight of 75 g/m2;

for the prototype: 130 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 115 μm gives a lot to 66.3 g/m2.

It is seen that in this experience, if the thickness of the paper lead to an overall size of 15 μm, achieve win-8.7 g/m2or 11.6% in relation to the paper pulp, which means significant savings in relation to the environment.

Example 7D: 50,0% of the treated pigment according to example 7A and 50.0% of the raw pigment

a) to a mixture of pigments:

- grain size distribution such that 42,0 wt.% particles have a diameter less than 1 micron, determined with the help of the device Sedigraph 5100™ company Micromeritics™ ;

- BET specific surface (determined by BET method according to the standard ISO 9277): 28,0 m2/g;

b) for paper:

thickness measurement:

for the original sample, the control (untreated filler): 115 μm with a weight of 75 g/m2;

for the prototype: 137 μm with a weight of 75 g/m2that casting to the magnitude of the thickness of 115 μm gives a lot to 62.9 g/m2.

It is seen that in this experience, if the thickness of the paper lead to the total value of 115 μm, reach win the 12.1 g/m 2or 16.0% in relation to the paper pulp, which means significant savings in relation to the environment.

EXAMPLE 8

This example relates to the use in paint treated or untreated calcium carbonate.

To accomplish this, natural calcium carbonate type of Norwegian marble with a grain size distribution such that 70% by weight particles have a diameter less than 1 micrometer, defined with the help of the device Sedigraph 5100™ company Micromeritics™ in the amount of 5 tons per dry pigment in the form of a precipitate on the filter with a brush in a container with a capacity of 45 m3distilled water until obtaining a slurry with a dry matter concentration of 25 wt.% Then, the thus obtained slurry is treated with phosphoric acid in the form of 10 wt.%-aqueous solution in an amount corresponding to 0.20 mol H3About+per mole of caso3at a temperature of 60° and stirring for 2 hours with speed stirrer at 200 rpm.

After 2 hours, the suspension of calcium carbonate for 5 hours bubbled CO2with the increased pressure of 50 mbar so that the ratio (volume of suspension:volume of gaseous CO2) was about 1:0.15 in.

After conditioning for 24 hours, the slurry is dried by spray drying and preparing emulsion paint containing as n is Suppl part test of dry calcium carbonate.

The method paint preparation:

In the dispersant capacity 1 m3prepare a paint by dispersion in water, additives and pigments for 10 minutes at a stirring speed of 3000 rpm, then the speed is reduced to 1000 rpm and add the latex. Was dispersed for 10 minutes.

The results of the colouring, and the control is a water emulsion paint with 18% TiO2:

Whiteness and opacity control sample and with two identical prototype according to the invention with -15% and -30% pigment TiO2

the dry film thickness104 mcm113 mcm112 microns
the mass of the dry film177 g/m2166 g/m2163 g/m2

It is seen that in this experiment to achieve a thickness of 104 μm as a control mass film with calcium carbonate according to the invention is only 153 and 151 g/m2accordingly against 177 g/m2and if the thickness of the ink layer is brought up to a total value of 104 μm, achieve win 24 and 26 g/m2respectively, or to 13.5 and 14.7% respectively in relation to the weight of the paint, which means significant savings in relation okrujaushei environment.

1. Aqueous suspension of one or more pigments, fillers or minerals containing natural carbonate and, if necessary, a polymer dispersant as a stabilizer rheology of the suspension, characterized in that it further comprises the product or the reaction products of the above carbonate with gaseous CO2and the product or the reaction products of the above carbonate with one or more donors N3About+from the average force to strong, has a pH value above 7.5, measured at a temperature of 20° and the above-mentioned pigments can reduce a lot of paper at a constant surface.

2. Aqueous suspension according to claim 1, characterized in that the natural carbonate is a natural calcium carbonate and preferably marble, calcite, chalk or containing dolomite carbonate.

3. Aqueous suspension according to any one of claim 1 or 2, characterized in that the strong donor or strong donor ions H3About+choose among hydrochloric or sulfuric acid or mixtures thereof and the donor or donor ions H3About+the average power is selected among H2SO3, S4

-
N3RHO4, oxalic acid or mixtures thereof.

4. Aqueous suspension according to any one of claims 1 to 3, from ecaudata fact, the number of moles of donor ions H3About+from the average force to strong relative to the number of moles of caso3is generally 0.1 to 2, preferably 0.25 to 1.

5. Aqueous suspension according to any one of claims 1 to 4, characterized in that the pigment, filler or mineral has a BET specific surface, determined according to the standard ISO 9277, component 5-200 m2/g, preferably 20-80 m2/g and particularly preferably 30-60 m2/year

6. Aqueous suspension according to any one of claims 1 to 5, characterized in that the pigment, filler or mineral has the following characteristics: average diameter of the grain, as measured by the method of sedimentation on the device Sedigraph 5100™ is 50-0,1 μm; BET specific surface, determined according to the standard ISO 9277 is 15-200 m2/g; and a pigment, filler or mineral has the following characteristics: average diameter of the grain, as measured by the method of sedimentation on the device Sedigraph 5100™ is 25-0,5 μm; BET specific surface, determined according to the standard ISO 9277 is 20-80 m2/year

7. Aqueous suspension according to claim 6, characterized in that the pigment, filler or mineral has the following characteristics: average diameter of the grain, as measured by the method of sedimentation on the device Sedigraph 5100™ is 7-0,7 μm; BET specific surface, determined according to the standard ISO 9277 is 30-60 m2/is.

8. The pigment, filler or mineral in a dry state, wherein it is obtained by drying the aqueous suspension according to any one of claims 1 to 7.

9. The method of processing of pigments, fillers or minerals in aqueous suspensions containing natural carbonate, characterized in that the pigment, filler or mineral is treated by a combination of one or more donor ions H3About+from the average power to the strong and gaseous CO2and use natural carbonate, which allows to reduce the weight of the paper at a constant surface.

10. The method according to claim 9, characterized in that use CO2supplied externally recirculated CO2or CO2formed by the continuous addition of the same or a different donor ions H3About+from the average power to the strong, or due to the pressure of CO2, preferably 0.05-5 bar.

11. The method according to any of claim 9 or 10, characterized in that it includes the following 3 stages: a) treatment with donor or donor ions H3About+from the average force to the strong;

b) treatment with gaseous CO2formed in stage a), or CO2supplied from the outside, and in the latter case, the supply of CO2carried out simultaneously with the introduction of donor ions H3About+or after suggesting the donor ions H 3About+;

(C) raising the pH value, measured at a temperature of 20° C, above 7.5 in the time interval after the end of stages a) and b)of 1-10 hours, preferably 1-5 hours without addition of base, or immediately at the end of stages a) and b) adding the base, and stage C) is the last stage of the method.

12. The method according to claim 11, characterized in that stage a) and (b) can be repeated several times.

13. The method according to any of PP-12, characterized in that the pH value, measured at a temperature of 20° is 3-7,5 during stages a) and b) processing and treatment temperature is 5-90° C, preferably 45-60° C.

14. The method according to any of PP-13, characterized in that the concentration of gaseous CO2in suspension by volume such that the ratio of the volume of suspension : volume of gaseous CO2is 1:0.05 to÷ 1:20 when the above ratio of 1:1÷ 1:20 at the stage a) and 1:0.05 to÷ 1:1 to stage b).

15. The method according to 14, characterized in that the concentration of gaseous CO2in suspension by volume such that the ratio of the volume of suspension : volume of gaseous CO2is 1:0.05 to÷ 1:10 when the above ratio of 1:0.5 to÷ 1:10 in stage a) and 1:0.05 to÷ 1:1 to stage b).

16. The method according to any of PP-15, characterized in that the duration of a hundred is AI b) treatment lasts 0-10 h, preferably 2-6 hours

17. The method according to any of p-16, characterized in that the pigment, filler or mineral containing natural carbonate, choose among natural calcium carbonate or carbonate containing dolomite, and mixtures thereof with talc, and/or kaolin and/or titanium dioxide TiO2, magnesium oxide MgO and other minerals, inert in relation to the donor ions H3About+from the average power to a strong, well-known in the field of paper industry.

18. The method according to 17, wherein the natural calcium carbonate chosen from among marble, calcite or chalk.

19. The method according to any of PP-18, characterized in that the strong donor or strong donor ions H3About+choose among hydrochloric or sulfuric acid and the donor or donor ions H3About+the average force is chosen among N2SO3, HSO4

-
N3RHO4, oxalic acid.

20. A method of obtaining a water suspension, characterized in that after the three stages of the method of processing of pigments, fillers or minerals in claim 11 use of dispersant and, if necessary, carry out a stage of re-concentration.

21. Aqueous suspension of one or more pigments, napolnitelyami minerals, containing natural carbonate, characterized in that the carbonate reduces the mass of the paper at a constant surface and they are obtained by the process according to any one of p-20.

22. Aqueous suspension according to item 21, wherein the pigment, filler or mineral containing natural carbonate selected among natural calcium carbonate or carbonate containing dolomite, and mixtures thereof with talc, and/or kaolin and/or titanium dioxide Tio2, magnesium oxide MgO and other minerals, inert in relation to the donor ions H3About+from the average power to a strong, well-known in the field of paper industry.

23. The pigment, filler or mineral in a dry state, wherein it is obtained by drying the aqueous suspension according to any one of p-22.

24. Compositions for use in the paper industry, characterized in that they contain at least one aqueous suspension according to any one of claims 1 to 7 or 21-22.

25. Means for layering paper, characterized in that it is an aqueous suspension according to any one of claims 1 to 7 or 21-22.

26. Means for filling paper pulp, characterized in that it is an aqueous suspension according to any one of claims 1 to 7 or 21-22.

27. Means for p, characterized in that the mass produced paper at a constant surface reduced by 3-15%.

28. The method of stratifying and/or pigmentation treatment is ncacii the paper surface characterized in that the suspension according to any one of claims 1 to 7 or 21-22 simultaneously used as filler paper pulp and nalivaeva salt solution and/or pigmentation of the surface of the paper.

29. Means for coloring, characterized in that it is an aqueous suspension according to any one of claims 1 to 7 or 21-22.

30. A method of manufacturing a sheet of paper, cardboard or the like, characterized in that it includes the introduction of a suspension according to any one of claims 1 to 7 or 21-22 at the stage of preparing a thick paste or diluted paste or both of these stages, depending on the manufacturing process of paper one or more times.

31. The method according to item 30, characterized in that it includes the introduction of a suspension or of a composition according to any one of claims 1 to 7 or 21, 22, or 24, recycled lead water or also recycled waste due to breaks when layering.

32. The method according to item 30 or 31, characterized in that the method according to any of PP-20 apply to recycled lead water or waste due to breaks when layering.

33. The method according to any of p-32, characterized in that it is used for making paper based on cellulose fibres from wood of deciduous or coniferous trees.

34. The method according to any of p-32, characterized in that it is used for making paper, produced from synthetic hair is he.

35. Paper, cardboard or a similar product, characterized in that they are obtained by the process according to any one of p-34.

36. Paper on p for use preferably in digital inkjet printing.



 

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