Aqueous compositions and their application in paper and carton making

FIELD: chemistry; textiles; paper.

SUBSTANCE: preparation method of polysilicate containing aqueous composition representing homogeneous liquid at 25°C, includes stages as follows: I) preparation of aqueous liquid containing silicate, II) reducing pH of the liquid to 2-10.5, III) ensured polymerisation time to actual completion resulted in making product containing gelled substance, IV) processing gelled substance with sufficient shearing to produce homogeneous liquid. Aqueous composition is prepared by the presented method. Aqueous composition contains polysilicate. This composition represents homogeneous liquid at 25°C. The composition develops viscosity at least 200 mPa·s when evaluated at concentration 2 wt % and at 25°C with using Brookfield viscosimeter at 20 rpm with shaft №2, with polysilicate of specific surface area not exceeding 2000 m2/g and S-value below 5%. Paper or carton making process includes preparation of cellulose suspension, with aqueous composition added, water drainage from suspension thus shaping wet paper web thereafter dried. Paper or carton making process includes preparation of cellulose suspension, added with mineral filler and exposed to drainage and containment system procedure, followed with water drainage from suspension thus shaping wet paper web thereafter dried. Mineral filler is aqueous composition. Before drainage and containment system is enabled, the suspension is exposed to at least, one shearing. This system implies adding aqueous composition to cellulose suspension, while shearing stage is specified from stirring, clarification and pumping.

EFFECT: improved quality of paper and carton.

46 cl, 16 tbl, 6 ex, 2 dwg

 

The present invention relates to water polysilicate compositions and to their preparation and application as either mineral fillers, additives to impart strength or additives that promote the retention/drainage, in the manufacture of paper and cardboard. Scope of the present invention also includes methods of making paper and paperboard, in which water polysilicate compositions include as mineral fillers and/or additives to impart strength and/or additives that promote the retention/drainage.

In the process of making paper of General practice is the inclusion of a mineral filler. For example, in EP-A-0880618 described methods of making paper with a filler, in which the pulp suspension include cationically precipitated calcium carbonate (COC), and preparation dilute the pulp for making paper containing COC. During the process using polymer promote retention additive having a characteristic viscosity at least 4 DL/g, and anionic material of the microparticles such as silica material of the microparticles and is able to swell the clay. This improves the retention of the filler, and the implementation of the method allows to produce highly filled paper.

WO-A-99/04092 regarding the Xia to the problems of low strength, which may arise in the case of highly filled paper. It is proposed a method in which the silicate composition is introduced into the pulp slurry and in which the silicate around the cellulose fibers forming a three-dimensional mesh structure. In one system (CA-Flocc) silicate such as sodium silicate, mixed with a calcium compound such as calcium oxide, the mixture is mixed with cellulose fiber, which is then acidified to a pH in the range of 7 to 9, and is the polymerization of the silicate. In another proposed system (Mg-Flocc) instead of calcium is used, for example, sodium silicate and a magnesium compound. In this case, the polymerization or gelatinization of the reaction mixture may be carried out partially without the presence of the fiber, although the mixture typically continues to polymerization in the presence of the fiber. In proposed another system (Si-Flocc) use silicate, which is then acidified to a pH of from about 7 to 9. In any of these three systems can be added to aluminum connections.

System Mg-Flocc and Si-Flocc can be implemented by the preparation of compositions, starting without the presence of fiber. Polysilicate systems provide an opportunity to cure, providing sufficient time for the formation of a sufficient number of cross-links, but in the preferred embodiment, the materials are mixed thus the om, that they are not super hard. The implementation of this method provides significant improvement in strength. However, in some cases, this can cause problems achieve the proper forming and it may cause sporadic loss of strength. In such cases, the paper may contain significantly more light spots and holes.

Therefore, there is a need to develop an improved method of making highly filled paper, which exhibits superior characteristics of the molding and more adequate high strength. There is also a need to develop a method, which enables the production of paper, with even more superior durability, mainly by strength in the wet state.

In the manufacture of paper and paperboard common practice is the use of additives that promote the retention and drainage. For example, a very effective additives that promote the retention/drainage used in the manufacture of paper, are cationic polyacrylamide and cationic starch. In the US 4388150 described composition binder comprising colloidal silica and cationic starch to be added to the fiber for making paper to enhance retention of the components of the hair is NISTO mass or to be added to the circulating water to reduce pollution issues and to recover valuable components of the fibrous mass. The colloidal silica may take various forms, including the form polysilicon acid, because the best results are achieved thanks to the use of silica in colloidal form. Itself polysilicon acid is, as it is written, unsolicited and without stabilization during storage spoils.

In the US 4954220 described the work, which shows that a certain time of storage or aging polysilicon acid is necessary. However, in this patent States that the complete gelatinization of aqueous solutions of poly acid should be avoided because after gelatinization these solutions possess a few advantages for use as an additive that promotes the retention and drainage. In the US 4954220 shown that storing or aging polysilicon acid, which leads to the formation of silica microgels, affects favorably, and the use of silica microgels with various cationic polymers provides, as I said, getting systems additives that promote the retention and drainage, which are at least equivalent, and in many cases superior to those which form a combination of colloidal silica/cationic starch. Silica microgels can be obtained by acidification of the silicate to a pH of from about 2 to 10.5; opportunities for established what I microgels polysilicon acid usually requires time storage or aging solution and after a period of aging, which can be very short (a few minutes or so), the solution is diluted to a concentration of about 1 wt.% or below in order to stabilize and slow down further growth of the microgels.

In EP-A-0235893 described method of manufacture of paper and cardboard by adding a cationic polymer of molecular weight of at least 500000 before stage shear impact and inorganic material comprising bentonite, after this stage, the shear effects. The implementation of this method provides significant advantages in terms of improved time drainage and retention increased amounts of fiber and filler.

However, despite these improvements, there is still a need for an alternative retention/drainage, which provides an equivalent or superior combination of retention and drainage. In addition, it is necessary, apparently, to develop a method of manufacturing paper and achieve improved visual properties and/or strength characteristics, mainly in the manufacture of paper with filler and, in particular, when the filler is a synthetic filler.

In accordance with the present invention include a water composition comprising a polysilicate, which is particularly effective either in ka is este mineral filler, or as an additive that promotes the retention/drainage. This aqueous composition when it is used as a mineral filler, creates the possibility for forming highly filled paper having a high strength and molding characteristics. In addition, when creating the present invention, it was found that when the aqueous composition is used at least as part of the system retention/drainage, retention and drainage are at least as effective as in cases of known systems using inorganic additives that promote the retention/drainage, for example systems based on silica particles or systems using can swell clay.

In one embodiment, the object of the present invention is a method for preparing aqueous composition comprising a polysilicate, where this composition is an essentially homogeneous liquid, when assayed at 25°comprising the following stages:

I) preparation of an aqueous fluid comprising a source of silicate,

II) bringing the pH of the liquid to range from approximately 2 to approximately 10,5 to thereby initiating polymerization of the silicate,

III) providing sufficient time for the occurrence of polymerization to the practical conclusion of the Oia and education in the product, including gelatinizing material

IV) processing gelatinizing material sufficient shear effect to obtain essentially homogeneous liquid.

Source of silicate may serve as a reasonable silicate compound, which is usually subjected to gelatinization to get polysilicate. In a suitable embodiment, such silicate compounds are water-soluble Monomeric silicates monovalent cations. In a preferred embodiment, the source of silicate is chosen from the group including sodium silicate, potassium silicate and lithium silicate.

It is necessary that the concentration of silicate was sufficient to ensure optimal polymerization. If the concentration is excessively low, then the polymerization does not usually occur, or usually proceeds at a rate that is unacceptably low. If the concentration is too high, then the rate of polymerization is probably unregulated. In a suitable embodiment, the concentration of sodium silicate should be in the range from 1 to about 7%, preferably from about 2 to about 3%.

It may be necessary to include in the aqueous liquid phase (I) aluminum compounds. The presence of aluminum ions typically have an inherent tendency to increase the rate of gelatinization and launched the Oia formation of cross-links. This may be favorable for reducing the reaction time. Aluminum compound, as a rule, is any acceptable water-soluble aluminum compound such as aluminum sulfate or alum. Aluminum compound, such as alum, as a rule, can be added in an amount up to about 0.4 g/g of the silicate. Thus, in a preferred form, the polysilicate is polyaluminosilicate.

The acidification can be achieved by the introduction of acidic compounds, such as mineral acids, or by the introduction of substances that are dissolved in the aqueous fluid with the formation of acid, such as carbon dioxide. Alternatively, the acidification can be achieved using ion-exchange resins. In a preferred embodiment, acidification achieved by adding gaseous carbon dioxide. Acidification should be brought to the pH values, which ensures optimal polymerization or gelatinization. In a suitable embodiment, at the stage (II) pH adjusted to the range from 4 to 9, preferably to the range from 6 to 8.

The polymerization of the silicate should be essentially to completion. In this context, "essentially to completion" means that no obvious further gelatinization does not occur, although there is the possibility that, to a certain extent, manchesteri reaction still proceeds. In one embodiment, the polymerization of an aqueous solution of silicate can be carried out in a vessel with getting the product, which is a homogeneous gelatinisation solid. However, in this embodiment, it may be less convenient to carry out shear processing at the final stage of the way. Therefore, during stage polymerization, it is generally preferable mixing liquid. Thus, in a preferred embodiment, the product formed in stage (III), includes amorphous gelatinisation solid particles dispersed in a liquid.

The first three stages of the method can be carried out similarly to the method described in WO-A-99/04092, mainly in regard to obtaining Si-Flocc in the absence of cellulose fibres, presented at SS. 19, 30 and 31. The resulting product typically contains gelatinizing the polysilicate, usually in the form of an amorphous solid particles dispersed in a relatively low viscosity liquid.

The final step of the method can be carried out using any conventional wysokosciowe equipment. In a suitable embodiment, the equipment for shear processing can serve as a homogenizer or a Silverson or Ultra Thurrax. In one preferred embodiment, the product containing gelatinizing silicate is subjected to shear treatment and the use of any installation of the equipment list for one minute at 8000 rpm Shear treatment should be sufficient to ensure that is formed essentially homogeneous liquid. By "essentially homogeneous liquid" it is meant that the liquid does not inherently contains polysilicate solid particles of a large size, which are clearly visible. This implies that particles of several millimeters or larger is essentially absent. However, there is a possibility that the composition includes a very small polysilicate particles. The diameter of such a very small polysilicate particles, typically less than 1 mm, for example, and at least a diameter of 90 wt.% one of them is less than 1 mm In the preferred embodiment, the amount of such very small polysilicate particles are less than 750 microns, preferably less than 500 μm. Usually the share of all polysilicate particles with a diameter greater than 150 microns should be less than one-third of the water composition. In a preferred embodiment, the composition typically comprises less than 20 wt.% polysilicate particles with a diameter greater than 150 microns, more preferably less than 10%. Especially preferred share of such polysilicate particles is, apparently, less than 1% and in particular less than 0.1%. Moreover, in the preferred embodiment, this aqueous composition does not contain any other solid particles, such as cellulose ox the con.

The aqueous composition obtained in this way is new. This song should be in the form of a homogeneous liquid. It can be, for example, in the form of a homogeneous gel-like paste. Composition, as a rule, is much more viscous than the dispersion of the amorphous polysilicate solid particles. In a preferred embodiment, the aqueous composition according to the invention typically exhibits a viscosity of at least 200 MPa·with (when it is determined at a concentration of 2 wt.% and at 25°using Brookfield viscometer at 20 rpm with shaft No. 2), preferably at least 300 or 400 MPa·s, and more preferably at least 600 MPa·C. In a particularly preferred embodiment, the viscosity is at least 1500 MPa·with (when it is determined at a concentration of 2 wt.% and at 25°using Brookfield viscometer at 20 rpm with shaft No. 3). The viscosity can be as high as 5000 MPa·C or higher. Typically, however, the viscosity is in the range from 1700 to 3000 MPa·C, preferably about 2000 MPa·C.

The polysilicate included in the aqueous composition typically has a relatively large specific surface area in comparison with many conventional mineral fillers, such as powdered calcium carbonate. However, compared with many of the polysilicate is diversified products from the microparticles, such as polysilicate the microgels, the polysilicate is usually characterized by having a relatively small specific surface area. Usually the polysilicate has a specific surface area less than 2000 m2/g, preferably in the range of from 750 to 1250 m2/g, more preferably about 1000 m2/year

S-value indicates the level of aggregation or the formation of microgels, and low S-value is indicative of a higher degree of aggregation. S-value can be determined and calculated as described in the work of Iler&Dalton in J.Phys.Chem. 60 (1956), 955-957. As a rule, polysilicates the microgel shows the S-value of about 12% or higher. The polysilicate included in the aqueous composition of the present invention typically has an S-value below 5%. In a preferred embodiment, the polysilicate usually has an S-value in the range from 1 to 4%, preferably from about 2.5 to 3.5%.

The water composition in accordance with the present invention is a new object and can be characterized by a unique combination of parameters. Thus, it is proposed aqueous composition comprising a polysilicate, where this composition is an essentially homogeneous liquid, when assayed at 25°C, exhibits a viscosity of at least 200 MPa·with (when it is determined at a concentration of 2 wt.% and at 25�B0; With using a Brookfield viscometer at 20 rpm with shaft No. 2), preferably at least 300 or 400 MPa·s, and more preferably at least 600 MPa·and in this polysilicate composition has a specific surface area less than 2000 m2/g and has an S-value below 5%. In a particularly preferred embodiment, the viscosity is at least 1500 MPa·with (when it is determined at a concentration of 2 wt.% and at 25°using Brookfield viscometer at 20 rpm with shaft No. 3). Preferred variants can be characterized more specific parameters of viscosity, specific surface area and S-value mentioned above.

The water composition in accordance with the present invention can be prepared in any convenient form. This aqueous composition generally includes SiO2in a concentration that is at least 0.01 wt.%, preferably from about 1 to about 45 wt.%. In a more preferred embodiment, the concentration is in the range from about 1 to 7 wt.%, most preferably in the range of 2 to 3 wt.%. A special advantage of this aqueous composition is that it can be added to the pulp suspension without prior modification.

Water polysilicate composition according to the invention is particularly suitable for p is imeneniya in the manufacture of paper or cardboard or as a mineral filler as an additive to impart strength, or as an additive for facilitating drainage/retention.

Scope of the present invention encompasses a method of making paper or paperboard comprising preparing a cellulosic suspension, draining water from the suspension by forming a wet paper web and the subsequent drying of this paper, characterized in that the pulp suspension add water polysilicate composition in accordance with any of the options presented in the present description.

Moreover, the object of the present invention is also a method of making paper or paperboard comprising preparing a cellulosic suspension, draining water from the suspension by forming a wet paper web and the subsequent drying of this paper, in which the pulp suspension add aqueous polysilicate, where the aqueous polysilicate is prepared by a method comprising the following stages:

I) preparation of an aqueous fluid comprising a source of silicate,

II) bringing the pH of the liquid to within from about 2 to about 10.5 and thereby initiating polymerization of the silicate,

III) providing sufficient time for the occurrence of polymerization up to practical completion and education in the product, including gelatinizing material, characterized by the fact that h is about before adding to a pulp slurry of the product of stage (III) is treated with shear effect.

When creating the present invention, it was found that the processing gelatinizing polysilicate material shear effect before adding it to the pulp suspension inherent advantages. Thus, in particular, when creating the present invention, it was found that at equivalent concentrations of filler can be achieved by increasing the strength.

In yet another embodiment, the object of the present invention is a method of making paper or paperboard comprising preparing a cellulosic suspension, adding to this suspension of mineral filler, draining water from the suspension by forming a wet paper web and the subsequent drying of this paper, characterized in that the mineral filler is a water polysilicate composition in accordance with any of the options presented in the present description.

The implementation of such a method makes it possible to produce highly filled paper, which exhibits high strength and molding characteristics. Thus, in particular, the paper, which is made by this method has adequately high quality and demonstrates the absence of light spots or holes.

Water polysilicate composition should be added to the pulp suspension in Koli is the EU ETS, the topics, which are usually used as mineral fillers. In a suitable embodiment, the aqueous composition is added in an amount of from 20 to 250 kg/ton, calculated on the dry weight of the pulp suspension. The polysilicate this aqueous suspension can be only used filler or alternatively, you can use the optional fillers. In the case when in addition to water compositions using other fillers, these fillers can be, for example, organic pigments to improve the opacity of the paper. Another option in addition to the aqueous composition can be used at least one additional mineral filler. These additional mineral fillers can be any of the usual fillers, they usually include precipitated calcium carbonate (COC), ground calcium carbonate, clay, soda clay, talc, zeolites, silicas, titanium dioxide and structured pigments.

Before adding to a pulp slurry water polysilicate composition and additional filler can be combined. However, in the preferred embodiment, the aqueous composition and the additional filler is added separately. In some situations it may be advisable to add water the composition is in conjunction with additional filler, although it is generally assumed, apparently, their sequential addition. In some manufacturing processes of paper may be necessary to add water compositions in the pulp suspension before additional filler. Typically, in the preferred embodiment, this additional topping add first.

In the paper manufacturing process may also be necessary to include in the pulp suspension system for retention and drainage. It can be, for example, any of the usual additives that promote the retention and drainage, which is technically available. In a preferred embodiment, the system for retention and drainage typically includes a polymer additive that promotes retention/drainage, and additive of particles, facilitating the retention/drainage. Polymer additives that promote the retention/drainage, can be any from the group comprising essentially a water-soluble anionic, nonionic, cationic and amphoteric polymers. Polymers can serve as natural polymers such as starch and harowie gums, which can be modified or unmodified. Alternatively the polymer can serve as synthetic polymers such as the polymers obtained by the polymerization of water soluble ethylene is easymenu monomers, such as acrylamide, acrylic acid, acrylates of alkali metals and ammonium, or quaternion dialkylaminoalkyl(meth)acrylates or (meth)acrylamide. Typically, these polymers have high molecular weight, for example at least 500000. In a preferred embodiment, the polymers generally have molecular weights in the range from at least one million to 20 or 30 million or higher. Typically, the polymers have molecular weights in the range from 5 to 15 million

The addition of microparticles that promote the retention/drainage, may be based on a crosslinked organic polymer. Such polymers generally can be in the form of microemulsions, such as that described in EP-484617 and are the products of the company Ciba Specialty Chemicals under the trade name Polyflex. Alternatively the addition of microparticles that promote the retention/drainage may be inorganic, such as silica microgels, colloidal silica sols of silica, silica gels, polysilicates, aluminosilicates, polyaluminosilicate, borosilicate, polyborazylene, zeolites and able to swell the clay.

As swelling clays, as a rule, can be used, for example, clay, bentonite compounds, preventing type. Preferred swelling in water of clay, these include clay, which in the water are exposed to the EU is the natural enemy swelling, and clay, which can be modified, for example by ion exchange, to give them swelling in water. Suitable swelling in water of clay include, though not limited to, clay, often referred to as hectorite, smectites, montmorillonite, nontronite, saponite, sekonic, gormiti, attapulgite and sepiolites. Typical anionic swelling clay is described in EP-A 235893 and EP-A 335575.

The aqueous composition can be added to the pulp slurry as a filler in the form of a diluted source material, i.e. after dilution. Alternatively it can be added, in addition, in the previous part of the system, for example in a dense fibrous mass mixer or mixing pool. The insertion point can be varied in accordance with the specific layout of the paper machine and the filler, which is added at the insertion point, which usually ensures the best possible introduction to pulp and environment and optimal retention. In a preferred embodiment, the aqueous composition as a filler certainly mix in the pulp suspension before the system retention and drainage. Therefore, in a preferred embodiment, the retention system and drainage applied to the pulp slurry after the addition of mineral filler.

In accordance with Ni is sustained fashion option of carrying out the invention the aqueous composition, comprising a polysilicate, is a part of or the whole system retention and drainage. Thus, when creating the present invention, it was found that the water composition can function similarly to the existing additives that promote the retention/drainage, in particular the products of microparticles, such as sols of silica and able to swell clay.

Therefore, in accordance with this object the invention proposes a method of making paper or paperboard comprising preparing a pulp slurry, the applied suspension system retention and dewatering, draining water from the suspension with the formation of the paper web and the subsequent drying of this paper, characterized by the fact that the system of retention and dewatering involves mixing in the pulp suspension in water polysilicate composition in accordance with any of the options presented in the present description.

When it is used as an additive for facilitating retention/drainage, water polysilicate composition expediently added to the cellulosic suspension in an amount of at least 100 g/t in terms of the mass of silicon dioxide on dry weight of suspension. In the preferred embodiment, this amount is usually at least 500 g/t, and as a rule is, much more, mainly when it is used essentially in the absence of additives from microparticles that promote the retention/drainage. When creating the present invention, it was found that in some cases the optimal retention and drainage achieve with the use of such high concentrations as 250 kg/T. In one preferred embodiment, the concentration is in the range from 20 to 250 kg/so

Water polysilicate composition, as a rule, is part of a system of retention and drainage. Thus, in addition to water composition system retention and drainage in a preferred embodiment, further includes an adulteration of the pulp suspension polymer additives that promote the retention/drainage, and/or supplements of the particles, facilitating the retention/drainage. However, usually water polysilicate composition is used as a partial or complete substitute supplements from particulate matter, contributing to the retention/drainage, and thus, as a rule, used in the system, which includes the use of polymer additives that promote the retention/drainage.

Polymer additive that promotes retention/drainage, can be selected from the group comprising essentially a water-soluble anionic, not omogenia, cationic and amphoteric polymers. These polymers may be any of the above-mentioned polymer additives that promote the retention/drainage.

The addition of microparticles that promote the retention/drainage, may be based on a crosslinked organic polymers, for example as described in EP-A-484617. Alternatively the addition of microparticles that promote the retention/drainage may be inorganic, such as silica microgels, colloidal silica sols of silica, silica gels, polysilicates, aluminosilicates, polyaluminosilicate, borosilicate, polyborazylene, zeolites and able to swell the clay. The addition of microparticles that promote the retention/drainage, can be, for example, clay, bentonite compounds, preventing type, such as described in EP-A-235893, but in suitable option, you can use any of those materials from the microparticles as described above.

In one preferred embodiment, a polymeric additive that promotes retention/drainage, mix in the pulp suspension before at least one stage of shear exposure. Stage shear effects can be, for example, the stage of mixing, light or delivery, including, for example, the use of centrifugal pumps, centrifugal sorts itd Then after this stage, the shear effects may be additive introduced, facilitating the retention/drainage, which is an aqueous polysilicate composition. Thus, the polymeric additive that promotes retention/drainage, can be added to the pulp suspension, followed by one or more shear stages of the impact, and then in the pulp slurry can add water polysilicate composition. In an alternative after this stage, the shear effects in the pulp suspension also introduce additive of particles, facilitating the retention/drainage.

However, in another embodiment, the invention features a method of making paper or paperboard comprising preparing a pulp slurry, the mixing in the pulp suspension of mineral filler, apply in respect of such suspension system retention and dewatering, draining water from the suspension by forming a wet paper web and drying of this paper, characterized in that the mineral filler is a water polysilicate composition according to the invention, before application of the system of retention and dewatering the suspension is passed through at least one stage of shear exposure, where retention system and drains the simulation includes the introduction in the pulp suspension in water polysilicates compositions according to the invention and where the phase shift effects are selected from the stages of mixing, clarification and pumping.

In one preferred form of this variant in the pulp suspension type COC as a mineral filler and the suspension is passed through at least one stage of shear exposure. Later in the pulp suspension as part of the mineral filler mixed with water polysilicate composition according to the invention. In a more preferred embodiment, after addition of the mineral filler, which is an aqueous polysilicate composition, the pulp suspension is passed through at least one phase shift exposure followed by the addition of polymeric additives that promote the retention/drainage. Then the pulp suspension is passed through at least one additional phase shift exposure, after which the pulp suspension add an additive that promotes the retention/drainage, which is an aqueous polysilicate composition according to the invention. The addition of microparticles that promote the retention/drainage, can also be added to the pulp suspension before adding, simultaneously with or after the addition of additives that promote the retention/drainage, which is an aqueous polysilicate composition.

As one illustration of the invention odourisation composition is prepared first obtaining amorphous silica gel with 2 wt.% SiO 2the addition of carbon dioxide in a dilute solution of liquid glass (28,5% soluble silicate from 9.2% sodium oxide). Before carbonization significant number (perhaps to more than 50%) of the silicate can be replaced or decaborate sodium or sodium aluminate, or other materials. The solution is acidified to pH 6.9 to 7.1 and with limited mixing, allow the gel to completely form a suspension of silica-containing solid pieces of gel and less viscous solution. This suspension gel process shear impact using installation Silverson at 8000 rpm for one minute to obtain a homogeneous viscous solution.

Then, in addition, promote the retention and drainage in a fibrous pulp for making paper with the aim of increasing the ash content of the paper while maintaining the strength of the paper add this homogeneous viscous solution polysilicate.

Examples

The preparation of an aqueous polysilicate composition (MIC) in all examples

Through a solution of sodium silicate with 2 wt.% SiO2(Na (3,27) 38/40 F Akzo-PQ Silica) was barbotirovany constant stream of CO2. Using a calibrated pH electrode was periodically monitored for pH.

Manufacturer of paper paintings in all cases

For each of the options presented below, five paper paintings is zagotavlivali with compliance with the following procedures add.

In the manufacture of all sheets of paper handmade character without MIC as an additive that promotes the retention and drainage, standard added portion was 0.5 kg/t of cationic polyacrylamide (CPAM) and 2.0 kg/t for bentonite compounds, preventing suspension (BentS). When the MIC is used in the form of microparticles, as cationic materials used 0.5 kg/t of cationic polyacrylamide. Concentrations were calculated on the dry weight of the pulp suspension (fiber weight). In further carried out the following processing:

Fibrous mass5C shear effects 1000 rpmCUC5C shear effects 1000 rpm(VPK)5C shear effects 1000 rpmKAM50C shear effects 1000 rpm(BentS) or (VPK)15C shear effects 500 rpm

Sheets of paper with a handmade character received after the final stage of mixing and drying for 2 h at 60°on a rotating drying cylinder.

Test paper web

The paper web was tested for tensile strength at break using a bursting machine brand "Instron" 4400 at UMIST in accordance with the test method Tbpr T 494 OM-88.

Used d the I the strength test samples of paper were then used to determine the total content of filler in the paper manual low tide by ashing at 500° C for 2 hours

Example 1 - Preparation of an aqueous polysilicate composition (VPK)

Getting the MIC was carried out in accordance with the above. Watched pH and recorded in table 1.

Table 1
Time (minutes)PH
011,05Weight of sodium silicate (liquid glass): 69,97 g
110,13Weight of sodium silicate + H2About: 1007,3 g
2-
38,99
48,14
57,10
67,02
77,02
87,02The gelatinization after 7 min
97,05
107,06
157,06

Example 2 - Effect of shear effects on the performance properties MIC

100 ml MIC subjected to shear processing within a reasonable time at 20,000 rpm using a homogenizer Ultra Turrax. The results are presented in table 2.

Table 2
No.OptionThe point of adding VPKAsh content (%)Breaking length(m)
15,0% MIC (no shift)5 before polymer41,01548,9
25,0% MIC (30 offset)5 before polymer39,22163,2
35,0% MIC (60 offset)5 before polymer38,12202,7
45,0% MIC (15 offset)5 before polymer38,72076,7

All papers contained 35% of JCC to the target ash content of paper paintings 40%.

From the obtained results it is clear that shear processing water polysilicate composition improves the strength of paper.

Example 3 - Effect of point additions to operating properties MIC

In all cases used subjected to shear processing VPK (1 min at 20,000 rpm using a homogenizer Ultra Thurrax). The results are presented in table 3.

Option
Table 3
No.The point of adding VPKAsh content (%)Breaking length(m)
195% MIC (shear processing)10 min before polymer37,72241,0
205%MIC (shear processing)5 min before polymerof 37.92258,8
215% MIC (shear processing)1 min before the polymerto 38.32077,1
225% MIC (shear processing)5 before polymer38,22140,5
235% MIC (shear processing)Before BentS41.31624,9
No.OptionThe point of adding VPKAsh content (%)Breaking length(m)
245% MIC (shear processing)After BentS40,61592,2
255% MIC (shear processing)Instead BentS39,72093

All papers contained 35% of JCC to the target ash content of paper paintings 40%.

These results demonstrate the improved strength when using subjected to shear is the processing of water polysilicate composition, mainly when it is added before the polymer.

Example 4 - Getting aluminized specimens MIC. Obtaining samples

Table 4

100% aluminized MIC
Time (min)pHMass of sodium aluminate: 5.53 g
Weight of sodium silicate: 0,00
0-The mass of solid particles and water: 200,1 g
0 (after Al)12,4
111,03After 20 with the addition of CO2
formed white cloudy precipitate
210,46
39,38
47,
57,3
77,15
97,12
117,11
137,11
157,11

Table 5

50% aluminized MIC
Time (min)pHMass of sodium aluminate: 2,77 g
Weight of sodium silicate: 7,05 g
011,10The mass of solid particles and water: 201,3 g
0 (after Al)12,3
110,38After 1 min of addition of CO2
was ultinationals to solid
state
29,81
3for 9.47Samples were taken
49,07
58
77,4
9of 6.96
119,92
136,89
156,89

tr>
Table 6

10% aluminized MIC
Time (min)pHMass of sodium aluminate: 0,553 g
Weight of sodium silicate: 12,21 g
011,07The mass of solid particles and water: 200,4 g
0 (after Al)11,41
19,12During carboxylation
26,98gelatinization carboxypropanoyl
36,83the mixture was observed. After 1 h
46,83standing the sample was ultinationals
56,82
76,82
96,82
116,82
136,82
158,62Samples were taken

Table 7

5% aluminized MIC
Time (min)pHMass of sodium aluminate: 0,277 g
Weight of sodium silicate: 13,26 g
011,00The mass of solid particles and water: 200,9 g
0 (after Al)11,34
1to 9.32During carboxylation
28,23gelatinization of carboxyl vannoy mixture was observed. After 1 h
36,87
46,84standing sample as usual
56,83was ultinationals
76,83
96,83
116,83
136,83
156,83Samples were taken

Table 8

Standard MIC
Time (min)pHMass of sodium aluminate: 0.9 g
Weight of sodium silicate: 14,00
010,98The mass of solid particles and water: 199,6 g
0 (after Al)9,82
1scored 8.38The sample was ultinationals
26,95after 7 min
36,92
46,93
56,92
76,92
96,92
116,92
136,92
156,83Samples were taken

Table 9
OptionThe point of adding VPKBreaking length (m)The average ash content (%)
30% CUCN/a3122,130,6
50 kg/t standard MICBefore the system/D4412,519,0
50 kg/t 50% Al MICReplacement BentS4149,523,9
50 kg/t standard MICReplacement BentS3886,825,2
25% CUCN/a3868,924,4
5 0 kg/t 10%Al MICReplacement BentS3903,126,0
50 kg/t 5% Al MICBefore the system/D4178,421,8
50 kg/t standard MICReplacement BentS3964,724,2
50 kg/t 10% Al MICBefore the system/D4165,921,4
50 kg/t 50% Al MICBefore the system/D 4392,4to 19.9
20% CUCN/a4115,620,6
50 kg/t 5% Al MICReplacement BentS3861,4to 25.3
50 kg/t 100% Al MICReplacement BentS3436,224,2
15% CUCN/a4839,216,0

All included MIC options contained 20% of the OCC to the target ash content of the finished paper web 25%.

Example 5 - Effect polyaluminosilicate microgel (MG) when the added amounts MIC

Table 10
OptionThe point of adding VPKBreaking length(m)The average ash content (%)
5% standard MICBefore the system/D3671,823,4
5% MGBefore the system/D5714,76,9
30% CUCN/a2016,833,1
25% CUCN/a2814,124,7
20% CUCN/a3104,719,6
15% CUCN/a3794,015,2
0% JCCN/a 6412,90,4

All included MIC options contained 20% of the OCC, to target the ash content of the finished paper web 25%.

Example 6

Using samples of the MIC, subjected to shear processing to varying degrees with a number of homogenizers, and holding shift processing for different periods of time have produced a number of sheets of paper handmade character.

Subjected to shear processing of the samples, the MIC was evaluated to determine the viscosity and mass of lumps. Manufactured paper web was tested for tensile strength at break and the ash content was estimated by the appearance.

Sample preparation VPK

The sample with 2.0 wt.% MIC was prepared in accordance with the method, in General terms presented in the first paragraph in the section "Examples".

200 ml of sample MIC subjected to shear processing during different periods of time by using a homogenizer or Silverson at 2000 rpm or Ultra Thurrax at 13500 rpm

td align="center"> Shift 3
Table 11

Shear effects used for samples VPK
SampleMixerTime (s)
Shift 1Without shear effects0
Shift 2Ultra Thurrax, 13500 rpm120
Ultra Thurrax, 13500 rpm15
Shift 4Silverson, 2000 rpm60
Shift 5Silverson, 2000 rpm30
Shift 6Silverson, 2000 rpm15

Preparing a sample of cationic polyacrylamide (CPAM) concentration of 1 wt.% and the sample suspension bentonites (BentS) concentration of 5 wt.%.

Preparing a mixture of hardwood and softwood 50/50 crushed to the consistency of grind 55° (define method of Shopper-Rigler) and was diluted to a solids content of 0.5%.

Preparing a 10%suspension of the product Calopaque F (COC).

Before adding to the fibrous mass cationic polyacrylamide and bentonite compounds, preventing the suspension was diluted to 0.1%.

Manufacturer of paper paintings handmade character

5 sets of paper webs for each of the options below, made by compliance with the following procedures add.

In the manufacture of all sheets of paper handmade character used standard added portions of 0.5 kg/t of cationic polyacrylamide and 2.0 kg/t of bentonite compounds, preventing suspension.

Carried out the following sequence.
Fibrous mA is sa 5C shear effects 1000 rpmCUC5C shear effects 1000 rpm(VPK)5C shear effects 1000 rpmKAM50C shear effects 1000 rpm(BentS) or (VPK)15C shear effects 500 rpm

Sheets of paper with a handmade character received after the final stage of mixing and drying for 2 h at 65°on a rotating drying cylinder.

Table 13
No.Option
1320% of JCC and 5% MIC (shift 2)
1520% of JCC and 5% MIC (shift 1)
1620% of JCC and 5% MIC (shift 3)
1720% of JCC and 5% MIC (shift 4)
1820% of JCC and 5% MIC (shift 5)
1920% of JCC and 5% MIC (shift 6)
2615% CUC
2720% CUC
2825% CUC
2930% CUC
3035% CUC

Assessment VPK

Samples subjected to (and not subjected to shear processing), the MIC was evaluated using a Brookfield viscometer at 20 rpm for opredelyayuschego viscosity and mass of lumps. A lot of lumps was determined by sampling 100 ml sample of the MIC, dilution to 500 ml of tap water and filtered through pre-weighed 150-micrometer sieve. Next MIC washed with an additional 100 ml of tap water with the subsequent removal of the sieve of all excess water using colored blue pellets. Then the sieve again weighed and counted a lot of lumps MIC.

Test paper web manual low tide

Then using a scanner to assess the transparency of the dried paper web was evaluated on appearance with getting the print paper web to the gray scale with gel stains encountered on the image in the form of light spots.

Before testing the tensile strength at break at UMIST sheets of paper handmade character was kondicionirovanie at 23°and at 50%humidity.

The ash content of the paper handmade character was determined by conducting the experiment at 500°C for 2 hours

Results

Sample preparation

Table 14

Standard MIC
Time (min)pHWeight of sodium silicate: 70,05 g
010,98The mass of solid particles and water: 999,6 g
19,82
2scored 8.38
36,95
46,92
56,93
6
76,92After 7 min the sample was ultinationals
116,92
136,92
156,92

Assessment VPK

Table 15

Discodiva the viscosity of the military-industrial complex and the number of lumps
Sample123456
Shift (speed)No shiftUT (13500)UT (13500)Silv. (2000)Silv. (2000)Silv. (2000)
Time shift (s)12015603015
Viscosity, shaft No.122222
Results27,532,734,5 20,024,819,5
29,532,630,519,022,6of 17.5
31,531,032,520,523,018,4
31,531,932,320,124,016,9
27,531,519,2
Viscosity (MPa·)147,5638,8649,25395,2472.0 M.364,0
The mass of lumps and sieve (g)141,796,548101,76113,25117,67129,09
The mass of the sieve (g)96,41896,51596,73096,67696,28996,298
Mass clumps (g)45,3220,0335,03016,57421,38132,792

Test paper web manual low tide

Table 16

The results determine the strength and ash content
No.OptionsBreaking length m) Ash content (%)
1320% of JCC and 5% MIC (shift 2)4062,619,4
1520% of JCC and 5% MIC (shift 1)2539,931,0
1620% of JCC and 5% MIC (shift 3)3054,927,5
1720% of JCC and 5% MIC (shift 4)3220,627,3
1820% of JCC and 5% MIC (shift 5)2837,529,2
1920% of JCC and 5% MIC (shift 6)2787,829,9
2615% CUC4244,115,8
2720% CUC3613,920,9
2825% CUC3146,825,4
2930% CUC2672,730,0
3035% CUC2158,635,1

The results determine the strength was averaged according to the two dimensions of each of the 5 paper paintings. Each of the five paper paintings ash content was determined separately.

In test 13 subjected to shear effects polysilicate composition in accordance with the present invention provided is equivalent to the ash content (meaning the number of EmOC is nitela, detained in paper canvas), as in experiment 27 polysilicate composition was absent, but has been demonstrated to increase the strength of more than 12%. In addition, although the polysilicate is not subjected to shear effects in experiment 15, under equivalent conditions, the OCC and polysilicate was demonstrated higher ash content, and all thrown shear processing polysilicate provided increased strength.

Graphical representation of data table 15 can be found in figures 1 and 2.

The effect of shearing treatment on MIC

If to judge according to table 15, the mass of lumps MIC, remaining on the sieve was found to be inversely proportional to the degree of shear processing. While definitions of viscosity with increasing trial testimony viscometer Brookfield significantly decreased (all indications were removed after three revolutions of the shaft at 20 rpm).

The influence of shear processing MIC on the strength of the paper web

For this system the degree of shear processing optimized in terms of strength. Most of the increase shown in figure 2, which corresponds to shear processing VPK for 1 min at 2000 rpm using a Silverson mixer. Loss of strength at lower degrees of shear effects could be explained by the inhomogeneous nature of the suspension dioxide is Rennie, allowing the silica to remain as separate particles and bind them rather than with fibres and fillers.

The influence of shear processing MIC on the appearance of the paper web

Even shear a low magnitude impact eliminates the appearance of visible gel spots. The higher the degree of shear effects on silicon dioxide, the less gel spots. The paper web was acceptable when the shear impact of all levels.

The appearance of the paper web can be improved by resolving gel stains caused by not subjected to shear processing MIC.

1. The method of preparation of the aqueous composition comprising a polysilicate, where this composition is an essentially homogeneous liquid, when assayed at 25°comprising the following stages:

I) preparation of an aqueous fluid comprising a source of silicate,

II) bringing the pH of the liquid to the range of 2 to 10.5 with thereby initiating polymerization of the silicate,

III) provision of time for the occurrence of polymerization up to practical completion and education in the product, including gelatinizing material

IV) processing gelatinizing material shear effect to obtain essentially homogeneous liquid.

2. The method according to claim 1, in which the torus source of silicate is chosen from the group including sodium silicate, potassium silicate and lithium silicate.

3. The method according to claim 1 or 2, in which the aqueous liquid at the stage (I) also includes an aluminum connection.

4. The method according to claim 1, wherein in stage (II) pH adjusted to the range from 4 to 9, preferably to the range from 6 to 8.

5. The method according to claim 1, in which the liquid to stage (III) is subjected to stirring.

6. The method according to claim 1, in which the product formed in stage (III), includes amorphous gelatinisation solid particles dispersed in a liquid.

7. The water composition, including polysilicate, which can be prepared by the method according to one of claims 1 to 6.

8. The aqueous composition according to claim 7, which exhibits a viscosity of at least 200 MPa·with (when it is determined at a concentration of 2 wt.% and at 25°using Brookfield viscometer at 20 rpm with shaft No. 2).

9. The aqueous composition according to claim 7 or 8, which exhibits a viscosity of at least 1500 MPa·with (when it is determined at a concentration of 2 wt.% and at 25°using Brookfield viscometer at 20 rpm with shaft No. 3).

10. The aqueous composition according to claim 7, in which the polysilicate has a specific surface area less than 2000 m2/year

11. The aqueous composition according to claim 7, in which the polysilicate has an S-value below 5%.

12. Aqueous composition comprising a polysilicate, where this composition represents the t is essentially homogeneous liquid, when assayed at 25°and the composition exhibits a viscosity of at least 200 MPa·with (when it is determined at a concentration of 2 wt.% and at 25°using Brookfield viscometer at 20 rpm with shaft No. 2), and where the polysilicate has a specific surface area less than 2000 m2/g and has an S-value below 5%.

13. The aqueous composition according to item 12, which exhibits a viscosity of at least 1500 MPa·with (when it is determined at a concentration of 2 wt.% and at 25°using Brookfield viscometer at 20 rpm with shaft No. 3).

14. The aqueous composition according to claim 7 or 12, in which the polysilicate has a specific surface area in the range from 750 to 1250 m2/year

15. The aqueous composition according to claim 7 or 12, in which the polysilicate is polyaluminosilicate.

16. The aqueous composition according to claim 7 or 12, in which the concentration of SiO2is at least 0.01 wt.%, preferably from about 1 to about 45%.

17. Method of making paper or paperboard comprising preparing a cellulosic suspension, draining water from the suspension by forming a wet paper web and the subsequent drying of this paper, characterized in that the pulp suspension is added to an aqueous composition according to one of claims 7 to 16.

18. The method according to 17, in which the pulp suspension mixed with mineral Napo is the preserver, where the mineral filler is an aqueous composition according to one of claims 7 to 16.

19. The method according to p, in which the aqueous composition is added to the cellulosic suspension in an amount of from 20 to 250 kg/ton, calculated on the dry weight of polysilicate and dry weight of the pulp suspension.

20. The method according to claim 19, in which the pulp suspension is mixed with at least one additional filler, where the filler is a mineral filler, or/and an organic pigment.

21. The method according to claim 20, in which an additional filler selected from the group comprising precipitated calcium carbonate (COC), ground calcium carbonate, clay, whether clay, talc, zeolites, silicas, titanium dioxide and structured pigments.

22. The method according to claim 20 or 21, in which before adding to the pulp suspension in water composition and the additional filler unite.

23. The method according to claim 20 or 21, in which the aqueous composition and the additional filler is added to the pulp suspension separately.

24. The method according to item 23, in which the aqueous composition and the additional filler is added to the pulp suspension in series, preferably by adding the first additional filler.

25. The method according to p, in which in relation to the pulp suspension is applied to the retention system and d is tiravanija.

26. The method according A.25 in which the system of retention and dewatering involves mixing in the pulp suspension polymer additives that promote the retention/drainage, and supplements from particulate matter, contributing to the retention/drainage.

27. The method according to p, in which the polymer additive that promotes retention/drainage, chosen from the group comprising essentially a water-soluble anionic, nonionic, cationic and amphoteric polymers.

28. The method according to p, in which the additive of the particles, facilitating the retention/drainage, chosen from the group comprising crosslinked organic polymers, silica microgels, colloidal silicon dioxide, sols of silica, silica gels, polysilicates, aluminosilicates, polyaluminosilicate, borosilicate, polyborazylene, zeolites and able to swell the clay.

29. The method according to one of PP-28, in which the retention system and drainage applied to the pulp slurry after addition of the mineral filler.

30. Method of making paper or paperboard comprising preparing a pulp slurry, the applied suspension system retention and dewatering, draining water from the suspension with the formation of the paper web, and then drying this paper web, wherein the retention system and d is tiravanija includes mixing in the pulp suspension aqueous composition according to one of claims 7 to 16.

31. The method according to item 30, in which the aqueous composition is mixed with the pulp suspension in the amount of at least 100 g/t, preferably at least 500 g/t, in terms of the mass of silicon dioxide on the dry weight of the pulp suspension.

32. The method according to item 30, in which the retention system and drainage further includes mixing the pulp suspension polymer additives that promote the retention/drainage, and/or supplements of the particles, facilitating the retention/drainage.

33. The method according to p, in which the polymer additive that promotes retention/drainage, chosen from the group comprising essentially a water-soluble anionic, nonionic, cationic and amphoteric polymers.

34. The method according to p, in which the additive of the particles, facilitating the retention/drainage, chosen from the group comprising crosslinked organic polymers, silica microgels, colloidal silicon dioxide, sols of silica, silica gels, polysilicates, aluminosilicates, polyaluminosilicate, borosilicate, polyborazylene, zeolites and able to swell the clay.

35. The method according to item 30, in which the polymer additive that promotes retention/drainage, mix in the pulp suspension before at least one stage of the shear impact of selected stages of mixing, clarification, and is Ericaceae, and then after this stage, the shear effects in the pulp suspension add an additive that promotes the retention/drainage, which is an aqueous composition.

36. The method according to p, in which, after the stage of shear effects in the pulp suspension also add a Supplement of particulate matter, contributing to the retention/drainage.

37. Method of making paper or paperboard comprising preparing a pulp slurry, the mixing in the pulp suspension of mineral filler, applied to the suspension system retention and dewatering, draining water from the suspension by forming a wet paper web and drying of this paper, characterized in that the mineral filler is an aqueous composition according to one of claims 7 to 16, before application of the system of retention and dewatering the suspension is passed through at least one stage of shear exposure, where retention system and drainage includes the introduction in the pulp suspension aqueous composition according to one of claims 7 to 16, and where the phase shift effects choose from the stages of mixing, clarification and pumping.

38. The method according to clause 37, in which the pulp suspension is mixed with at least one additional filler, where the filler is either mine the filler material, or/and organic pigment.

39. The method according to § 38, in which an additional filler selected from the group comprising precipitated calcium carbonate (COC), ground calcium carbonate, clay, whether clay, talc, zeolites, silicas, titanium dioxide and structured pigments.

40. The method according to § 38, in which before adding to the pulp suspension in water composition and the additional filler unite.

41. The method according to § 38, in which the aqueous composition and the additional filler is added to the pulp suspension separately.

42. The method according to paragraph 41, in which the aqueous composition and the additional filler is added to the pulp suspension in series, preferably by adding more filler first.

43. The method according to clause 37, in which the pulp suspension type COC as a mineral filler and the suspension is passed through at least one stage of shear effects and then in the pulp suspension mixed with the aqueous composition according to one of claims 7 to 14.

44. The method according to clause 37, in which, after adding mineral filler, which is an aqueous composition according to one of claims 7 to 16, the pulp suspension is passed through at least one phase shift exposure followed by the addition of polymeric additives that promote the retention/Dreux is the key, and then the pulp suspension is passed through at least one additional phase shift exposure, after which the pulp suspension add an additive that promotes the retention/drainage, which is the composition according to one of claims 7 to 16.

45. The method according to item 44, in which an additional Supplement of particulate matter, contributing to the retention/drainage, added to the pulp suspension prior to, simultaneously with or after the addition of additives that promote the retention/drainage, which is an aqueous composition.

46. Method of making paper or paperboard comprising preparing a cellulosic suspension, adding to the pulp slurry additives to impart strength, draining water from the suspension by forming a wet paper web and drying of this paper web, wherein the additive for durability is an aqueous composition according to one of claims 7 to 16.

Priority items:

02.04.2003 - according to claims 1-7, 9-11, 13-16, 18-21, 25-37;

22.01.2004 - PP, 12, 17, 22-24, 38-46.



 

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