Lignin-cellulose materials and product made from said materials

FIELD: chemistry.

SUBSTANCE: absorbent material is made by treating lignin-cellulose material in the presence of a catalyst from a transition metal with oxidation. The oxidising agent is selected from a group consisting of hydrogen peroxide, hypochlorite, hypochloric acid or any combination thereof. The lignin-cellulose material is treated at pH from approximately 2 to approximately 6. The treated lignin-cellulose material has viscosity equal to or less than approximately 17 cP. The treated lignin-cellulose material is subjected to dry grinding. The dry ground lignin-cellulose treated material is used as an absorbent intermediate layer for making absorbents.

EFFECT: improved bacteria inhibition properties.

2 cl, 17 ex, 16 tbl

 

RELATED APPLICATIONS

This application claims the priority of patent application U.S. serial number 60/676828, filed may 2, 2005, and patent applications U.S. serial number 60/760073, filed January 19, 2006

The LEVEL of TECHNOLOGY

Pulp used in various absorbent articles for personal hygiene or medical care, such as diapers or products used in case of incontinence. One serious problem with these types of applications is the smell created by body fluids. In the case of diapers, the main problem is the smell of ammonia from urine. In other cases, unpleasant odors can be caused by other nitrogen-containing or sulfur-containing substances.

From published sources, it was to absorb odors are a variety of supplements. See, for example, U.S. patent No. 6765042 and 6852904 and patent application U.S. No. 00268281 A1.

BRIEF description of the INVENTION

In one aspect the present invention relates to a method including the processing of lignocellulosic material, preferably in the form of fibers or particles, and more preferably from hardwood, softwood, or a combination thereof, in the presence of a catalyst of a transition metal with an oxidant selected from the group consisting of hydrogen peroxide, hypochlorite, chlorine dioxide, chlorine is aristoi acid and any combination thereof, to obtain a treated lignocellulosic material having a viscosity equal to or greater than approximately 17 JV, and preferably with restoring a functional group selected from the group consisting of aldehyde functional groups and functional groups of the aldehyde type, such as hemiacetal that prevail in position C1. Used herein, the term "lignocellulosic material" means organic polymeric or oligomeric material having a substituted or unsubstituted carbohydrate (such as glucose, mannose, xylose, arabinose, galactose and the like) fragments, such as cellulose, hemicellulose and polysaccharides. Used herein, the term "prevail" means more than 50% of the total mass of regenerating functional groups. In the best variants of the invention, the treated lignocellulosic material preferably has a copper number is greater than about 0.5 and/or carboxyl number is greater than approximately 3.5 mEq/100 g

In another aspect the present invention relates to a treated lignocellulosic material with a viscosity equal to or less than approximately 17 SP. The material preferably has a reducing end groups selected from the group consisting of aldehyde functional groups and functional groups of the Alda is odnogo type, such as hemiacetal that prevail in position C1, i.e. at least about 50% of the total number of aldehyde functional groups and functional groups of the aldehyde of the type contained in the treated lignocellulosic material. The amount of aldehyde functional groups and functional groups of the aldehyde type in position C1 preferably more than about 75%, more preferably equal to or greater than about 80% and most preferably equal to or greater than approximately 90% of the total number of aldehyde functional groups and functional groups of the aldehyde of the type contained in the treated lignocellulosic material. In the best embodiment of the invention, the amount of aldehyde functional groups and functional groups of the aldehyde type in position C1 is approximately 95%. In the best variants of the invention, the treated lignocellulosic material preferably has a copper number is greater than approximately 4 and/or carboxyl number is greater than about 4.5 mEq/100 g

The treated lignocellulosic material of the present invention has one or more beneficial properties. For example, the material may have properties that prevent odors. Although we do not wish to be bound by any theory, we floor the guy, some materials resist odors through the formation of complexes with odorous substances, such as ammonia from the urine, and/or inhibiting growth of bacteria that convert urine into ammonia. Characteristics of counteracting smells of these lignocellulosic materials, particularly pulp, make them particularly suitable for use in the construction of absorbent personal care items such as diapers, feminine hygiene products, used older people with incontinence, etc. with SAC or without them. Some embodiments of the treated lignocellulosic material of the present invention have good strength properties of wet and/or dry. Some other embodiments of the present invention, in which the lignocellulosic material is the pulp, unexpectedly retain most of the mechanical properties of paper as compared with untreated pulp mass, except perhaps for tensile strength.

In another aspect the present invention relates to the subject of personal hygiene, absorbent, and this product contains:

at least one permeable to fluid top sheet layer and at least one impermeable to liquids lower sheet layer; and

absorbent m is a material predetermined sublayer, located between the top sheet layer and the lower sheet layer and the material of the underlayer contains a treated lignocellulosic material of the present invention.

In another aspect the present invention relates to a method of manufacturing an absorbent composite material suitable for use in the personal care items that contains:

getting dried minced processed hemicellulose material of the present invention, forming the absorbent sublayer consisting of loose wood pulp, treated in the mass;

receiving at least one top sheet layer, permeable to the liquid, and at least one back sheet layer, virtually impervious to liquid; and

accommodation material sublayer between the top sheet layer and the lower sheet layer.

In another aspect the present invention relates to a method of making paper or paperboard, containing the steps:

(a) obtaining a water supply for the manufacture of paper containing cellulose with a viscosity equal to or less than approximately 17 JV, and having a reducing end group selected from the group consisting of aldehyde functional groups and functional groups of the aldehyde type at positions C6 and C1, but prevailing in position C1;

(b) caused the deposits mentioned composition for forming a grid paper machine to obtain a wet paper web; and

(c) drying the aforementioned wet cloth paper or cardboard to get dry paper or paperboard.

In another aspect the present invention relates to a fibrous mass for the manufacture of paper or paperboard, containing cellulose and having a viscosity equal to or less than approximately 17 JV, and having a reducing end group selected from the group consisting of aldehyde functional groups and functional groups of the aldehyde type at positions C6 and C1, but prevailing in position C1.

DETAILED description of the INVENTION

In one aspect the present invention relates to a method including the processing of lignocellulosic material, preferably in the form of fibers or particles, and more preferably from hardwood, softwood, or a combination thereof, in the presence of a catalyst of a transition metal with an oxidant selected from the group consisting of hydrogen peroxide, hypochlorite, chlorine dioxide, hypochlorous acid, and any combination thereof.

Lignocellulosic material may be in the form of fibers or particles, such as cellulose fibers, particulates and other fragments of cellulose, hemicellulose, particles and powder of starch and polysaccharides. Lignocellulosic material can also be in solution, as, for example, in a solution of cellulose derivatives, such as ka is maximalizalasa, hydroxypropylcellulose, etc.

The type of lignocellulosic material used in the method of the present invention, is not of great importance and can be used any such material. For example, suitable lignocellulosic materials include materials obtained from known sources, such as plants. Examples of suitable lignocellulosic materials are polysaccharides, such as starches. Suitable starches for the implementation of the present invention in practice are naturally occurring hydrocarbons synthesized in corn, tapioca, potato and other plants by polymerization of dextrose units. All such starches and their modified forms, such as starch acetates, polyesters, starch, polyethers starches, phosphate starches, xanthate starches, anionic starches, cationic starches, etc. that can be obtained by reaction of starch with a suitable chemical or enzymatic reagent, can be used in the practical implementation of the present invention. Suitable polysaccharides are hemicelluloses extracted from wood before cooking or extracted from wood fibers after cooking, and they can be the core fibers of corn, which can be enriched with xylanase, pulp, the collapse of Alami or a combination of any two or more such materials. An example of lignocellulosic materials suitable for implementing the method of the present invention, in practice, are also cellulose fibers used in the manufacture of napkins, towels, diapers, feminine hygiene products, used by older people with incontinence, and also used in the production of other types of pulp and paper production, paper and cardboard. Such fibers include fibers derived from hardwood, softwood, or from a combination of deciduous and coniferous wood, which has been prepared for use in compositions for making paper by any known means of cooking, refining and bleaching, as, for example, the well-known mechanical, thermomechanical, chemical and Poluchenie etc. Used herein, the term "fibrous pulp hardwood" refers to a fibrous mass, derived from the woody substance of deciduous trees (Metasperm), whereas the term "fibrous pulp coniferous wood" refers to fibrous masses, derived from the woody substance of coniferous trees (gymnosperms). Suitable cellulose fibers can be obtained from non-woody herbaceous plants, including, without limitation, kenaf, hemp, jute, flax, sisal or abaku, although legal restrictions and Dragasani can make use of hemp and other sources of fibers impractical or impossible. In the method of the present invention can be used bleached or unbleached cellulose fibers, such as unbleached Kraft pulp, bleached Kraft pulp or pulp from secondary sources. The fibrous mass may be subjected to any treatment, which is normal for receiving and bleaching of pulp, or may be intentionally modified, as, for example, by controlled pre-hydrolysis or extraction chip caustic alkali sulfate before cooking, acid or enzyme (cellulose and hemicelluloses) hydrolysis of sulphate pulp, treatment of pulp cold soda" (up to the strength of mercerized).

Preferred lignocellulosic materials are fibrous pulp of hardwood, fibrous mass of softwood, or a combination thereof. More preferred lignocellulosic materials are pulp from hardwood and softwood sulphate cooking or a combination thereof. The most preferred lignocellulosic materials are bleached hardwood and softwood pulp sulphate cooking or a combination thereof, especially softwood pulp sulphate cooking.

The catalyst of transition metal used in the practical implementation of the present invention may be any and can the be used by any transition metal. Examples of such metals are cu, Fe, Zn, Co, Ni, Mn, V, Mo, W, Zr, Ce, Cr and any combination of them. These metals are preferably used in the form of salts, preferably in the form of a water-soluble metal salts. The preferred metal salts are the halides, sulfates, nitrates, phosphates and carbonates, and combinations thereof. The most preferred metal salts are metal salts si (si+ and Cu2+), Fe (Fe3+, Fe2+) and Zn (Zn2+), and particularly preferred are metal salts of si and Fe.

The amount of metal catalyst used in the method of the present invention may vary within wide limits and can be used in any amount sufficient to obtain the desired processed lignocellulosic product. The amount of metal catalyst is usually at least about 0.005 wt.% from the dry lignocellulosic material, but may be used in large or small quantities. The amount of metal catalyst is preferably approximately 0.005 to 1 wt.% from the dry lignocellulosic material, more preferably approximately from 0.01 to 0.5 wt.% from the dry lignocellulosic material, and most preferably from about 0.01 to 0.1 wt.% from the dry lignocellulosic material.

The oxidizing agent for use in the method of this izaberete the Oia is selected from the group consisting of hydrogen peroxide, chlorine dioxide, hypochlorite, hypochlorous acid, and any combination thereof. Preferred oxidizing agents are hydrogen peroxide and hypochlorite, and the most preferred oxidizing agent is hydrogen peroxide.

The amount of oxidizing agent may vary within wide limits, and can be any amount sufficient to obtain the desired processed lignocellulosic product. The amount of oxidizing agent is typically at least about 0.1 wt.% from the dry lignocellulosic material, but can be used by smaller amounts, if they effectively give the desired lignocellulosic material. The amount of oxidant is preferably approximately from 0.1 to 10 wt.% from the dry lignocellulosic material, more preferably from about 0.1 to 5 wt.% from the dry lignocellulosic material, and most preferably from about 0.5 to 5 wt.% from the dry lignocellulosic material.

The temperature of treatment can vary widely, and may be any temperature sufficient to obtain the desired treated lignocellulosic material. Treatment temperature is typically at least about 20C, but can be used to lower the temperature if they effectively give the desired lignocellulosic material. Treatment temperature is preferably from about 20C to 120C, more preferably from about 40C to 120C and most preferably from about 40C. to 90C., and particularly preferred processing temperatures of approximately 60C to 90C.

The pH value during processing may vary within wide limits, and can be any value sufficient to obtain the desired treated lignocellulosic material. The pH value during processing is generally approximately from 1 to 9, but may be lower or higher pH values, if they effectively give the desired lignocellulosic material. The pH value when processing is preferably approximately from 2 to 8, more preferably from about 2 to 7 and most preferably from about 2 to 6.

Processing time may vary within wide limits, and can be used any time, giving the desired processed lignocellulosic product. Processing time is usually at least about 5 min, but can be used longer processing time, if it gives the desired lignocellulosic material. The processing time is preferably approximately from 5 minutes to 20 hours, more preferably from 15 minutes to approximately 0 hours and most preferably from about 30 minutes to 4 hours.

On the choice of the method of the present invention can be carried out in the presence of UV radiation, preferably at a time when as the oxidant is hydrogen peroxide. UV treatment is more effective at lower temperatures, such as room or ambient temperature)without the need for heating equipment, and can be used to extend the effective range of pH values. For example, the method can effectively be carried out in the presence of UV radiation at ambient temperature (or without heating) at neutral pH within a very short time, from several seconds to 1 hour, depending on the power of the ultraviolet lamp and the conditions of mixing of the fibers. The ultraviolet lamp used in the method of the present invention, preferably is a lamp of high brightness, such as a mercury arc lamp, medium-pressure or its variants, pulsed xenon flash lamp or an excimer lamp. It is most preferable to use a mercury arc lamp, medium pressure, which is low cost and always readily available. Ultraviolet lamp, which is inserted into the quartz sleeve can be entered (immersed) in a suspension of cellulose fibers for irradiation. Sometimes it may be more efficient to put ultraviolet is any over stir the suspension of lignocellulosic material. For this type of UV radiation can be used as a mercury arc lamp and electrodeless lamps (e.g., offered by Fusion UV). Preferably, the cellulose fibers were completely mixed during the reaction, because the penetration of UV radiation in water is very weak, and most chemical action must arise from the decomposition of the peroxide by UV light in aqueous solutions. UV treatment can be carried out with the addition of the catalyst to the system for UV-peroxide. Suitable catalysts vary within wide limits, and can be used any known catalyst of UV radiation, as, for example, water-soluble metal salts such as iron salts or salts of copper used in the method of the present invention, the photocatalysts with micro - or nanoparticles of titanium dioxide or zinc oxide, an organic catalyst based on athropy, such as water-soluble 4,4'-azobis(4-cyanovalerianic acid), 2,2'-azobis(2-methylpropionamidine), AIBN or Dupont Vazo catalyst 88; and 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO).

The method can be carried out in a periodic, continuous or semi-continuous mode. The method of the present invention can also be implemented as part of the pulping process, as part of the process at the end of the manual polychemicals or chemical the definition of the pulping process or as part of the process of blanching as a stage in the process, at the end of the blanching process. The method can also be used for processing groundwood or loose pulp for making paper, as, for example, by re-fill groundwood or loose cellulose in hydropulper or similar device. Processing hydropulper or similar device gives the possibility to adjust the conditions. For example, processing begins at acidic pH and after some period of time regulate to alkaline pH by adding caustic soda and continue the reaction at higher pH value. This combined acid-base treatment can also be used to change the relationship carboxyl and carbonyl groups in the treated lignocellulosic material.

The treated lignocellulosic material obtained by the method of the present invention, has a viscosity less than 17 JV, measured by TAPPI method T-230. This viscosity is different from the viscosity of the untreated fibrous mass, which is usually more than 17 SP. The treated lignocellulosic material preferably has a viscosity equal to or less than approximately 15 JV, more preferably equal to or less than approximately 12 JV or equal to or less than approximately 10 JV and most preferably from about 1 to 10 SP. In the best embodiment, the treated lignocellulosic material, obtained the method of the present invention, has a viscosity from about 2 to 7 SP. It is believed that the reduced viscosity of the pulp indicates increased reducing the number of functional groups in position C1 at the end of the molecular or oligomeric chains forming lignocellulosic material. Although we do not wish to be bound by any theory, we believe that this creates more binding sites for some transition metals, such as copper and some others, and that limit regenerating functional groups act as other functional places in addition to other oxidized groups on the chains of polysaccharides. Sometimes it may be advantageous to increase the number of reducing end functional groups provided by the present invention, for further processing of the treated lignocellulosic material at the stage of acid hydrolysis or enzymatic hydrolysis, which is thought to be even more properties counteract the odor of the treated lignocellulosic material.

The treated lignocellulosic material obtained by the method of the present invention has a degree of polymerization of less than about 1200. In the best options for implementation of the present invention the treated lignocellulosic material preferably has a degree of polymerization, ravno is or less than about 1000, and most preferably equal to or less than about 900. In the best embodiment of the present invention the treated lignocellulosic material obtained by the method of the present invention has a degree of polymerization of from about 100 to 800, or from 200 to 600. One of the best embodiment, the treated lignocellulosic material obtained by the method of the present invention, has a rejuvenating group selected from the group consisting of aldehyde functional groups and functional groups of the aldehyde type, such as hemiacetal, which predominate in the position S1, as a result, when the lignocellulosic circuit is cut off due to oxidation during the process, the degree of polymerization and the viscosity of the treated fibrous mass is reduced. The number of such end groups can be determined in the manner described in U.S. patent No. 6635755 and mentioned reference materials, and other methods known to experts in this field of technology. According to the invention restoring functional groups can be isomerized to other groups than the aldehyde functional group and a functional group aldehyde type. Because of the stochastic process of oxidation is also possible that the aldehyde functional group or a functional group aldagen the type may be present in the C6 position, and/or ketones may be represented in positions C3 and C4, although to a lesser degree. Preferably the amount of reducing aldehyde functional groups or restore functional groups of the aldehyde type, present in position 1, greater than about 75% of the total amount of aldehyde functional groups or functional groups of the aldehyde type. The amount of reducing aldehyde functional groups or restore functional groups of the aldehyde type in position C1 is more preferably equal to or greater than about 80% and most preferably equal to or greater than about 90% of the above. In the best embodiment, the amount of reducing aldehyde functional groups or restore functional groups of the aldehyde type, present in the position S1, approximately 95% of the total number of regenerating aldehyde functional groups or restore functional groups of the aldehyde type.

In the best options for implementation of the present invention the treated lignocellulosic material obtained by the method of the present invention has a copper number equal to or greater than approximately 3. The copper number is measured by Tappi method T-430 cm-99. Processed lignocellulosic the material preferably has a copper number, equal to or greater than an estimated 4.4, more preferably equal to or greater than 5 and most preferably equal to or greater than 5.5.

In the best options for implementation of the present invention the treated lignocellulosic material obtained by the method of the present invention has a carboxyl number equal to or greater than about 3.5 mEq/100 g of processed material in kiln drying. Carboxyl number is measured by Tappi method T-237 cm-98. The treated lignocellulosic material preferably has a carboxyl number is greater than 4, more preferably greater than 5 and most preferably greater than 5.5 mEq/100 g

In one best mode of implementing the present invention, the treated lignocellulosic material obtained by the method of the present invention has a property of counteracting odors, as measured by the ability to communicate or to form complexes with ammonia and its activity in the inhibition of bacteria. The material's ability to form complexes with ammonia determined in the following way: a laboratory hammer mill Kamas, equipped with a forming funnel, used to form fibrous mass into briquettes lignocellulosic material area of 50 cm2and a mass of 3.00, the Briquettes were placed in a container closed by a cover having a membrane as a sample open the I. The briquettes were added 500 microliters 0.6% solution of ammonia using an airtight syringe with needle, having a sufficient length to reach the surface of the briquette. After a period of equilibration within 45 minutes took 1 quart of gas from the upper space through the opening, using a calibrated hand pump and indicator tube for ammonia (i.e. system gas tubes Draeger), selecting the sample through a needle adapter connected to the tube. In the best variants of the invention, the amount of ammonia absorbed by the treated lignocellulosic material to 50%, preferably 60%, and more preferably 80% more than the amount of ammonia absorbed in the same or almost the same lignocellulosic material prior to processing by the method of the present invention. In the best options for implementation of the quantity absorbed ammonia by more than 90% more than untreated fibrous mass.

Property treated lignocellulosic material to inhibit bacteria determined using the test microorganisms Corynebacterium ummoniagenes, ATCC 6871, replicable in the environment of the urea (I--144 P) and cultivated at a temperature of 372C for 2-3 days in a shake flask, and Escherichia coli ATCC 11229, replicable in trypticase soy broth (I-053B) and grown at tempera is ur 372C for 18-24 hours in shake flask. Microorganisms were assigned unique codes to ensure the accuracy of the obtained data. Method ASTM E 2180-01 used to determine the microbial load and decrease in percent, reduce Log10or increasing Log10quantities of the test substance against the tested microorganisms with the following modifications:

A sterile Petri dish 15100 mm) containing the sample (diameter 50 mm (2 inches)), placed in a larger Petri dish containing 10 ml of water to increase humidity and prevent drying during the test period.

1) the Samples will be hydrogenate itself to inoculation of 0.5 ml of the test culture.

2) "Agar suspension" will not be used.

3) Samples will be evaluated in pairs.

4) the Samples will be maintained at a temperature of 352C in a humidified chamber for periods 3 and 8 hours (10 minutes).

5) the Converter will be a volume of 50 ml tripticase soy broth with 10% tween 80, 3% lecithin, 0.5% sodium thiosulfate and 0.1% histidine, pH 7,20,1(1-148) in sterile containers with a capacity of 2 oz.

6) Sample destroying ultrasound into the neutralizer for 1 min, then mix by shaking for 1 min before dilution.

7) will Be prepared solutions for serial dilution up to 10-5volume 9 ml 2 neutralizing buffer solution Difco. Will the prepared solutions for dilution up to 10 -6for the control sample duplicate cups method Spread Plate using agar urea (I-S) and agar McConkie (I-090B). The undiluted sample Converter (dissolving 10 C [50 ml]) is wiseana by spreading 1 ml three cups.

8) Incubation is carried out at a temperature of 352C for 3 days for agar urea and at 352C for 18-24 hours for agar, mcconkey.

9) Along the way will determine the efficiency of the Converter by checking using E. coli as the test organism.

The reliability of the results obtained by the above method depends on the demonstration that the test substance (or substances) is not inhibited in the test conditions, the reproduction of viable organisms that may be present, and that the environment used for testing, demonstrate appropriate neutralizing characteristics and characteristics of growth. To test the effectiveness of the neutralizer to restore bacteria sample of the test substance with a diameter of 2 inches will be placed in 50 ml of neutralizer (#6) above) and are subject to destruction by ultrasound, followed by stirring with shaking. Volume for dilution of the test microorganism to obtain ~ 10-100 colony forming units (CFU)/ml in final concentration is then Converter will be added to the container and mixed thoroughly. Capacity with a catalytic Converter without test substances, inoculated in a similar manner, will be the positive control sample. Duplicate aliquots of 0.5 ml from the tank will be made into cups on agar, mcconkey for the test substance and positive control samples. If the growth of the test microorganism in the cups containing the test substance, and the growth of the positive control sample will be compatible from the point of view of the number and development of the colonies, the system Converter would be considered adequate. After incubation, the Cup will be counted and recorded as CFU/ml Of this figure is then computed value CFU/sample. The decrease in interest and reduce Log10or the increase in the number of microorganisms (both types) in the sample compared to the control sample will be calculated for each period of exposure. The property of suppressing bacteria preferably 40% more than untreated fibrous mass, more preferably 50% greater and most preferably 60% more. In some embodiments, implement, where lignocellulosic material is a fibrous mass, preferably of wood fibrous mass, the treated lignocellulosic material of the present invention shows a marked improvement in tensile strength in the wet state. Fine the level of improvement may vary within wide limits, and besides the fact that it is influenced by the level of processing, it also depends on the type of compositions fibers and types of sheets, prepared for evaluation. For highly plasticised compositions fibrous mass, although the strength of the control sample at break in the wet state is extremely low, the improvement may be at least 1.5 or 2 times, and preferably 3 to 5 times greater than that of a control sample in the measurement method Tappi T 456 om-03. Sheet manual casting, not relevant Tappi, such as for wipes and other products, the rate of improvement may vary depending on the levels of treatment and compaction in wet conditions.

In some of the best options for implementation of the treated lignocellulosic material of the present invention exhibits good property drainage, measured way T 221 cm-99.

In some of the best options for implementation of the treated lignocellulosic material of the present invention contains a linked metal derived from the catalyst. It is believed that the associated metal has a beneficial effect on the bactericidal activity of the treated lignocellulosic material. Used herein, the term "associated" refers to the element metal, which remains in the fibrous mass and not washed out by flushing the fibrous mass. How famous is, the nature of the relationship of metal with a fibrous mass refers to ionic interactions and complex formation with the functional groups of the fibrous mass, such as carbonyl or carboxyl, and enhanced by the present invention. The amount of bound metal is determined by conventional analysis methods such as the method of atomic absorption analysis with induced plasma, and is at least 10 parts per million, preferably from 20 to 700, more preferably from 20 to 150 and most preferably from about 20 to 100 parts per million.

The treated lignocellulosic material of the present invention may be subjected to subsequent processing some ways to further modify the properties of the material. For example, the treated lignocellulosic material can be subsequently processed cationic agent, which is thought to be associates restoring functional groups of the treated materials. As appropriate, you can use different cationic materials, including polymers containing cationic nitrogen, such as polyamine, 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC), hexadimethrine, polyethylenimine (linear and branched), copolymers of diallyldimethylammoniumchloride (DADMAC), copolymers of vinylpyrrolidone (VP) with quaternaire the data by diethylaminoethylmethacrylate (DEAMEMA). polyamides, cationic polyurethane latex, cationic polyvinyl alcohol, polyallylamine, dicyandiamide copolymers, polymers attach aminoglycoside, poly[oksietilenom (dimethylimino) ethylene (dimethylimino) ethylene] dichloride, polyvinyliden with high charge density, allylamine (RAS), poly (hexamethylenebiguanide) (RNPS), polyamidoamine (or polyethylenimine); cationic ions of metals, such as water-soluble aluminum salts, calcium salts, and salts of zirconium; and these related ions can act as active sites for complexation sizing and other substances used in the manufacture of paper, and cationic dendrimers, such as dendrimers FRAMES (polyamidoamine) with surface amino groups and dendrimers polypropylenimine with surface amino groups. It is believed that the processing of such cationic materials can modify properties such as to increase the amount of paper that it is desirable for thin paper, cardboard, napkins, towels and absorbent products, while maintaining good durability, and obtaining reduced values of water retention and increased the degree of grinding.

The treated lignocellulosic material can also be subsequently processed micro - or nanoparticles of metal oxides such as aluminum oxide. titanium oxide, zinc oxide and the dioxide of silicon, which are treated lignocellulosic material and modify its properties, such as fixation of the pigment, dye or optical Brightener, printable and/or prevention of odors. The treated lignocellulosic material can be subsequently processed cross-linking agent, such as, for example, dispersible or water-soluble bi - or multifunctional carbodiimide and/or polycarbamide, such as 1,6-hexamethylene-bis(ethylcarbodiimide); 1,8-octamethylene-bis (ethylcarbodiimide); 1,10-decametre-bis(ethylcarbodiimide); 1,12-dodecamethyl-bis(ethylcarbodiimide); PEG-bis(propyl(ethylcarbodiimide)); 2,2'-Dityatin-bis(ethylcarbodiimide); 1,1'-dithio-p-phenylene-bis(ethylcarbodiimide) and 1,1'-dithio-m-phenylene-bis(ethylcarbodiimide). during the manufacture of paper or the formation of a fibrous network. Bi - or multifunctional carbodiimide groups react with reducing functional groups of the material, stitching and fixing fiber material in the structure of the paper or fibrous network.

The treated lignocellulosic material of the present invention can be used for ordinary purposes on site or after you obtain in pure form using known methods to obtain in pure form. For example, the treated lignocellulosic material of the present invention may be COI is used for the manufacture of paper or cardboard bases or paintings. Methods and devices for the preparation of the foundations of the lignocellulosic fibers are well known in the pulp and paper industry. See, for example, "Handbook For Pulp & Paper Technologies" (guidelines for pulp and paper technology), 2ndEdition, G.A. Smook, Angus Wilde Publications (1992) and specified reference material. You can use any known method and device. Preferably the method comprises: a) obtaining a water suspension of lignocellulosic fibers; b) deposition of the aforementioned composition for forming a grid paper machine for the formation of wet canvas paper or paperboard; (C) drying the wet cloth paper or cardboard to get dry cloth paper or cardboard and d) calendering the dry leaf of paper or cardboard. In addition to these steps of the method can be applied additional steps known to experts in the art, for example, the step of applying one or more surfaces of the dry leaf of paper or paperboard coating containing a binder with a pigment dispersant or the stage of processing of the dry leaf of paper or paperboard in the sizing press, a sizing agent such as starch.

For example, the materials can be used for absorbent articles such as diapers, napkins, towels, personal hygiene items, using known methods. Such isdel the I and methods for their production are known to experts in the art and will not be described in detail. See, for example, U.S. patent No. 6063982 and 5766159 and the reference materials. The processed fiber Kraft pulp of the present invention can be used for the manufacture of impregnated Kraft paper. Impregnated Kraft paper is a paper made from unbleached sulphate pulp (a mixture of primarily deciduous with some softwood pulp, for example, from bog pine), which is used as the basis for impregnation and curing of synthetic resins. Impregnated Kraft paper is used as home and office construction material, for example, for the device roof of the kitchen. A useful property of impregnated Kraft paper is to control the permeation rate of a liquid (solution of the synthetic resin in the sheet while maintaining the porosity and density of the sheet. All fibre sulphate hardwood pulp in the impregnated sheet may be replaced by the coniferous cellulose, for example, sulfate pulp of bog pine (pine Kraft pulp grades used for the manufacture of plasterboard), processed by the method of the present invention to impart impregnated Kraft paper good properties of the transfer fluid. Although we do not wish to be bound by any theory, we believe that the layers of hemicelluloses and hydrocarbon topochemically located on the inside and Kraft fiber, oxidized by the method of the present invention, increasing the absorption liquid resin sheet.

The present invention will now be described with reference to the examples below. These examples are given as illustrative, and the invention is not limited to the materials, conditions, or parameters of the method indicated in these examples.

Example 1

Bleached Kraft pulp of bog pine was treated with a 1% hydrogen peroxide and 0.03% iron sulfate at pH 4 and a temperature of 75C for 1 hour. The treated pulp was then washed with deionized water, was formed into paper sheets and dried. Viscosity, copper and a carboxyl number of processed cellulose was determined using the above methods. The viscosity of the pulp was 6.2 SP. The copper number of the pulp was 4.5. Carboxyl number of the pulp was 5.5 mEq/100 g Pulp was also estimated to determine the amount of bound metal. The sample contained 43,4 parts per million Fe bound to the cellulose, which is not washed with water. Properties of cellulose to inhibit bacteria was estimated using the above procedure. The test results on the inhibition of bacteria are shown in Table 1 below.

Table 1
Reduction of E. coli in % after 8 hours against untreated control pulpReduction (E. coli+Ammoniagenes) in % after 8 hours against untreated control pulp
Cellulose treated with 1% hydrogen peroxide and 0.03% iron sulfate38%23%

Example 2

Bleached Kraft pulp of bog pine was treated with a 1% hydrogen peroxide and 0.03% copper sulfate at pH 4 and temperature of 80C for 1 hour. The viscosity of the pulp was 5.7 SP. The copper number of the pulp was 4.6. Carboxyl number of the pulp was 4.1 mEq/100 gorubathan pulp is then washed with deionized water, was formed into paper sheets and dried. The sample contained 90,8 parts per million of copper bound to the cellulose.

The cellulose was examined to counter the smell of ammonia and the inhibition of bacteria against the raw cellulose as a control using the above procedure. The results are shown in Table 2.

Table 2
The metal content in the celluloseReduction of E. coli in % after 8 hours p is otiv untreated control pulp Reduction (E. coli+Ammoniagenes) in % after 8 hours against untreated control pulp
Cellulose treated with 1% hydrogen peroxide and 0.03% copper sulfate90,8 ppm C58%68%
Cellulose treated with only 0.03% of copper sulfate93 parts per million C44%17%

Example 3

The bleached pulp from bog pine was treated by oxidation with 1% hydrogen peroxide with copper or iron catalyst at pH 4 and temperature of 80C for 1 hour. The treated pulp was then washed with deionized water, was formed in dry paper sheets for grinding into fibers in a laboratory hammer mill Kamas. This example used the hydrogen peroxide 1% and 2%, also changing the amount of catalyst. Cellulose was examined to counter the smell of ammonia using the above procedure. The results are shown in Table 2.

Results in neutralizing the smell of ammonia are shown in Table 3 below.

Example 4

The experiments were conducted with the use of metals at a temperature of 80C, pH 4 for 1 hour with a small spacecraft is in example 3) and very high doses of both metals, used in the absence of an oxidant. Cellulose was examined to counter the smell of ammonia against the raw cellulose as a control using the procedure described above. The results are shown below in table 4.

Table 4
The concentration of ammonia gas in the upper spaceTraces of metal bound to the cellulose, in parts per million
Untreated control cellulose35 ppm NH33 parts per million Fe
Cellulose treated with only 0.03% of copper sulfate on our way-washed (oxidizers none)16 ppm NH393 parts per million C
Cellulose treated with only 0.03% of ferrous sulfate on our way - washed (oxidizers none)to 14.5 ppm NH3109 ppm Fe
Cellulose treated with only 0.3% of copper sulfate on our way - washed (oxidizers none) 5 ppm NH3283 ppm C
The cellulose. processed only 0.3% of iron sulfate on our way - washed (oxidizers none)4 parts per million of NH3635 ppm Fe

Example 5

Conducted experiments using metals at a temperature of 80C, pH 4 for 1 hour. Determine the values of the viscosity of the cellulose and checked cellulose to counter the smell of ammonia against the raw cellulose as a control using the above procedure. The results are shown in Table 5.

Table 5
The concentration of ammonia gas in the upper spaceThe pH value of the pulp after washingThe viscosity of the cellulose
Untreated control cellulose43 parts per million of nh36,418 SP
Cellulose treated with 0.02% zinc sulfate, 2% peroxide41 part per million of NH3 6,316,7 SP
Cellulose treated with 0.02% zinc sulfate, 0.01% ferric sulfate, 2% peroxide11 ppm NH36,44,9 SP

Example 6

This example should demonstrate the advantage of the wet strength of the material after treatment with peroxide with a metal catalyst, especially in the preferred pH range of the present invention. Bleached sulfate pulp from bog pine was treated with 2% and 3% hydrogen peroxide from 0.03% iron sulfate at a temperature of 80C for 1 hour. The pH was varied from pH 4 to pH 10 at the end of the reaction. Standard sheet density of 1.2 g by Tappi produced using the method Tappi T 205 sp-02 and determined the tensile strength in the dry state, the strength of tweezing and tensile strength in wet state was determined using methods Tappi T 494 om-01, Tappi T414 om-01 and Tappi T 456 om-03, respectively. The values of tensile strength in wet/dry conditions was calculated based on the values of the tensile strength in the dry state, tensile plucking in the dry state and the tensile strength in the wet state. The results are shown in table 6 below.

Example 7

Drying obrabotannoi pulp will reduce the number of carboxyl groups, created on the fibers. This does not apply to the United cases paper/cardboard or dry powdery cellulose and dry-pressing, when the treated pulp is dried only once. However, this will affect the paper or cases napkins/towels when buying dried processed fibrous mass, then re-processed in hydropulper and again made paper products wet methods of drying. The effects of drying on the content of carboxyl groups in cellulose are shown in table 7 below.

Table 7
Carboxyl groups, mEq/100 g, wet pulpCarboxyl groups, mEq/100 g, dried and re-wetted cellulose
Untreated bleached pulp3,33,7
Cellulose treated with 2% hydrogen peroxide, 0.03% iron sulfate, at pH 4, 80C for 1 hour5,53,7

Example 8

Unbleached sulphate pulp was used to demonstrate the improved strength in the wet state. Unbleached sulphate pulp in the high Kappa number was treated with 2% hydrogen peroxide 0.04% of iron sulfate at pH 4 and temperature of 80C for one hour. The treated cellulose and untreated control pulp was refined using a hammer mill Valley and was formed into sheets manual casting density of 300 g/m2, extruded wet and dried flat on the dryer. The effect on sheet strength in the wet state are shown in table 8 below.

Table 8
The beating degree of the pulpThe tensile strength in the wet state, lb
Untreated control cellulose610 csf4,8
Cellulose treated with 2% hydrogen peroxide, 0.04 ferric sulfate625 csf10.9

Example 9

Wet sulfate pulp from bog pine was treated with 1% hydrogen peroxide at pH 4 with drawing on cellulose 0.02% iron sulfate. The processing carried out in the mill installation blanching at 80C for 1 hour. When another processing in the laboratory used 3% hydrogen peroxide and 0.04% iron sulfate; the treatment was carried out at 80C for 2 hours. Processed cellulo the s and control (original) pulp without finishing tested at the carbonyl and carboxyl groups. The results are shown in table 9 below.

Table 9
Copper numberCarboxyl (mEq/100 g)
The control pulp0,13a 4.9
Factory cellulose treated with 1% hydrogen peroxide4,05,5
Laboratory pulp treated with 3% hydrogen peroxide6,97,6

As shown in table 9, cellulose, treated with 1% hydrogen peroxide is increasing the copper number (30 times) and the number of carboxyl groups (12% more). Intensive treatment with 3% activated peroxide gave copper a number greater than 52 times and increase the number of carboxylic groups by 55%.

Example 10

Dried plant commercial sulphate pulp from bog pine was again turned into a fibrous mass. This pulp was treated with 2% hydrogen peroxide at pH 4 with 0.04% of iron sulfate at a temperature of 80C for 1 hour. Identified copper number of treated and untreated cellulose. The results are shown in table 10 below.

Table 10
Copper numberCarboxyl (mEq/100 g)
Control dry cellulose0,233,1
Processed dry cellulose5,64,1

The results in table 10 show that the treated pulp had a copper number 23 times more and the number of carboxylic groups by 32% more than untreated control pulp.

Example 11

Liquid fiber in Example 11 was treated with 1% hydrogen peroxide with 0.02% iron sulfate at pH 4 and temperature of 80C for 1 hour. Copper increased from 0.23 to 5.3. The treated pulp and the control pulp after it has processed polyvinylene with high charge density and sformovat in sheets manual casting by Tappi using the method Tappi T 205 sp-02. Basic mass and thickness of the sheets manual castings were determined by the methods Tappi T 410 om-02 and Tappi T 411 om-05, respectively, and bulk density of the control and the treated pulp was calculated on the base weight and thickness. The results are shown in table 11 below.

Example 12

Wet bleached Sul is atnow pulp of bog pine was treated with 1% hydrogen peroxide and 0.02% iron sulfate at pH 4 for 1 hour at a temperature of 80C. Of processed cellulose and the control of pulp produced sheets manual casting Williams. Then the leaves are hand-casting after drying loosened in a laboratory mill Kamas. Tested ability to absorb liquid (SCAN method). The results are shown in table 12 below.

Table 12
The control pulpThe treated cellulose
The ability to absorb liquid by the method of SCAN, g/g8,99,6

From the results shown in table 12, it is seen that the treated cellulose is increased compared with the control, the ability to absorb liquid. In fact, this increased ability to absorb the liquid, in combination with increased destruction fiber bog pine because of our treatment of the activated peroxide makes the treated pulp from the swamp pine perfectly acceptable for the manufacture of some hygiene items, which are not used overabsorbed particles (SAC).

Example 13

Mercerized Kraft pulp was obtained by treatment of sulphate pulp from bog pine with a solution of caustic soda (con what entrala 10%) for 5 minutes at 40C. Mercerized pulp was then treated with 1% hydrogen peroxide in the presence of 0.02% iron sulfate at pH 4 and temperature of 80C for 1 hour. The degree of grinding of rough and mercerized pulp was evaluated methods Tappi T 227 om-99, and the average length of the fibers treated and untreated mercerized pulp was determined by the method of Cajani (Kajanni). Processed and unprocessed mercerized pulp was formed into sheets manual casting by Tappi method Tappi T 205 sp-02, and basic mass and internal communication sheets manual castings were determined by the methods Tappi T 410 om-02 and Tappi T 569 om-00 respectively. Bulk density was calculated by the thickness and the base mass, as described above. The results are shown in table 13 below.

Example 14

Delignification oxygen sulphate pulp from bog pine treated pulp enzyme (Multifect A40 Genencor) at a dose of 0.2% on the cellulose. This is processed by the enzyme cellulose is then treated with 1.5% hydrogen peroxide with 0.02% iron sulfate at pH 4 and temperature of 80C for 1 hour. The degree of grinding and the average length of the fibers treated and untreated mercerized pulp was determined by the methods specified in the examples above. Treated and untreated pulp was formed into a fibrous fabric, and this fabric of razril is whether using a laboratory hammer mill Kamas. Determined energy loosening. The results are shown in table 14.

Table 14
The degree of grinding, CSFThe average fiber length FQA, L(L)mmEnergy loosening, kJ/kg
The raw pulp from southern pine7432,68223
Cellulose treated with enzyme7402,62,13-
Cellulose treated with enzyme and then treated with 1.5% of the activated peroxide740
607
470
2,61
1,26
1,07
201

Example 15

Sulphate pulp from bog pine varieties of plasterboard (Kappa 110) were subjected to the processing of low value with 2% activated peroxide and 0.04% iron sulfate at pH 4 and temperature of 80C for 1 hour. The degree of grinding the treated pulp was determined using the method specified in the examples above. For comparison also determined the degree of grinding a mixture of the C 80% raw hardwood pulp and 20% of the raw pulp of bog pine. The leaves are hand-cast in Tappi, molded from 100% processed pulp from bog pine and from a mixture of 80% raw hardwood pulp/20% raw cellulose from bog pine, were evaluated to determine the porosity Gurley (Tappi T 536 om-02) and the average value PHST (Tappi T 530 om-02 with liquid phenolic resin), respectively. The results are shown in table 15 below.

Table 15
80% deciduous/20% softwood pulp100% treated softwood pulp
The degree of grinding, CSF600682 (fiber length 2.3 mm)
Density11,912,5
Porosity Gurley22,122,9
The average value of the PHST, seconds60 on the side29 on the side

The data in table 15 show that the treated pulp from the swamp pine can be used to replace all hardwood pulp with low yield in the production of impregnated Kraft paper.

Example 16

Bleached sulfate pulp from bog pine was mixed with 2% hydrogen peroxide in the presence of 0.02% iron sulfate at pH 4, pH 7 and pH 12, respectively. Pulp with a consistency of 1% was kept under stirring at room temperature. On top of the pulp was placed a quartz plate. Poster ultraviolet device PS2 (mercury medium pressure lamp was used for irradiation of pulp through the quartz plate. With this processing, the duration of exposure to UV radiation was 15 minutes. After irradiation residual peroxide was not detected. The temperature of the pulp during processing is not increased. The viscosity of the pulp was 3, JV at pH 4, 3,9 SP at pH 7 and 10.6 SP at pH 10. Cellulose treated at pH 7, had a copper number of 6.2.

Example 17

Bleached sulfate pulp from bog pine was treated with hydrogen peroxide with iron, copper or combined Fe/Cu catalyst at pH 4 and temperature of 80C for 1.5 hours. The treated pulp and the control pulp was washed to pH 6 and made the dry leaves. Dry leaves loosened in a hammer mill as described above, and tested for absorption of ammonia. The results of the absorption of ammonia are shown in table 16 below.

Table 16
The viscosity of cellulose, SPThe concentration of ammonia gas in the space above the pulp% reduction in ammonia
Untreated control cellulose21,4300 ppm NH3-
Cellulose treated with 1% hydrogen peroxide, 0.03% iron sulfate4,550 ppm NH383%
Cellulose treated with 2% hydrogen peroxide, 0.03% iron sulfatea 3.926 ppm NH391%
Cellulose treated with 3% hydrogen peroxide, 0.04% of iron sulfate3,211 ppm NH396%
Cellulose treated with 1% hydrogen peroxide and 0.04% copper sulfatethe 9.7130 ppm NH357%
Cellulose treated with 1% hydrogen peroxide, 0.04% of sulfate IU the and 7,2105 ppm NH364%
Cellulose treated with 2% hydrogen peroxide and 0.04% copper sulfatethe 5.741 part per million of NH386%
Cellulose treated with 2% hydrogen peroxide. 0.04% of copper sulfate5,548 ppm NH384%
The cellulose. treated with 2% hydrogen peroxide. 0.02% copper sulfate8,980 ppm NH373%
Cellulose treated with 2% hydrogen peroxide, 0.02% copper sulfate6.575 ppm NH374%

In conclusion, in the light of the above description of possible deviations from the above examples. Therefore, although the present invention has been described with reference to specific the best ways to exercise, you need to understand what can be developed, and other songs that nevertheless fall within the scope and essence of the invention defined in the attached formula the image is to be placed. The above description of the different and best of embodiments are presented for illustrative purposes only, and it is understood that they may be made of numerous modifications, changes and additions without departing from the spirits or scope of the invention defined in the following claims.

1. A method of manufacturing absorbent material used in personal hygiene and having elevated properties of inhibition of bacteria, determined according to method ASTM E-01, which contains:
processing of lignocellulosic material in the presence of a catalyst of a transition metal with an oxidant selected from the group comprising hydrogen peroxide, hypochlorite, hypochlorous acid, and any combination thereof at pH from about 2 to about 6, to obtain a treated lignocellulosic material having a viscosity equal to or less than approximately 17 JV, and having elevated properties of inhibition of bacteria, determined according to method ASTM E180-01,
dry grinding the treated lignocellulosic material to form the absorbent material of the intermediate layer;
receiving at least one top sheet layer, permeable to fluid and at least one lower sheet layer essentially impermeable to liquid the spine, and the introduction of the material of the intermediate layer between the top sheet layer and the lower sheet layer.

2. The method according to claim 1, characterized in that the available functional groups of lignocellulosic material is selected from the group consisting of aldehyde functional groups, hemiacetal functional groups or combinations thereof.

3. The method according to claim 1, characterized in that the treated lignocellulosic material has a carboxyl number equal to or greater than about 3.5 mEq/100 g of processed material in kiln drying.

4. The method according to claim 3, characterized in that the treated lignocellulosic material has a carboxyl number equal to or greater than about 4 mEq/100 g of processed material in kiln drying.

5. The method according to claim 4, characterized in that the treated lignocellulosic material has a carboxyl number equal to or greater than about 5 mEq/100 g of processed material in kiln drying.

6. The method according to claim 5, characterized in that the treated lignocellulosic material has a carboxyl number equal to or greater than approximately 5.5 mEq/100 g of processed material in kiln drying.

7. The method according to claim 1, characterized in that the treated lignocellulosic material has a viscosity equal to or less than about 15 CP.

8. The method according to claim 7, characterized in that the treated lignocellulosic material which has a viscosity, equal to or less than approximately 12 SP.

9. The method according to claim 8, characterized in that the treated lignocellulosic material has a viscosity equal to or less than about 10 CP.

10. The method according to claim 9, characterized in that the treated lignocellulosic material has a viscosity from about 1 to 10 SP.

11. The method according to claim 9, characterized in that the treated lignocellulosic material has a viscosity from about 2 to 7 SP.

12. The method according to claim 1, characterized in that the treated lignocellulosic material absorbs, adsorbs or absorbs and adsorbs 50% more ammonia than with the same amount of raw lignocellulosic material.

13. The method according to claim 1, characterized in that the treated lignocellulosic material absorbs, adsorbs or absorbs and adsorbs 60% more ammonia than with the same amount of raw lignocellulosic material.

14. The method according to claim 1, characterized in that the treated lignocellulosic material absorbs, adsorbs or absorbs and adsorbs up to 80% more ammonia than with the same amount of raw lignocellulosic material.

15. The method according to claim 1, characterized in that the treated lignocellulosic material absorbs, adsorbs or absorbs and adsorbs 90% more ammonia n is compared with the same amount of raw lignocellulosic material.

16. The method according to claim 1, where the specified lignocellulosic material is wood pulp.

17. The absorbent product obtained by the method according to claim 1.



 

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