WO2014019813A1 - Odour-inhibiting mixtures for incontinence products - Google Patents

Odour-inhibiting mixtures for incontinence products

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Publication number
WO2014019813A1
WO2014019813A1 PCT/EP2013/064412 EP2013064412W WO2014019813A1 WO 2014019813 A1 WO2014019813 A1 WO 2014019813A1 EP 2013064412 W EP2013064412 W EP 2013064412W WO 2014019813 A1 WO2014019813 A1 WO 2014019813A1
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WO
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Prior art keywords
preferably
polymer
particles
wt
water
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PCT/EP2013/064412
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German (de)
French (fr)
Inventor
Asif Karim
Thomas Daniel
Original Assignee
Basf Se
Basf Schweiz Ag
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Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61FFILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, E.G. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00Bandages or dressings; Absorbent pads
    • A61F13/15Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
    • A61F13/84Accessories, not otherwise provided for, for absorbent pads
    • A61F13/8405Additives, e.g. for odour, disinfectant or pH control
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/18Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
    • A61L15/46Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
    • A61L15/60Liquid-swellable gel-forming materials, e.g. super-absorbents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/108Elemental carbon, e.g. charcoal
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/11Peroxy compounds, peroxides, e.g. hydrogen peroxide
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/20Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
    • A61L2300/23Carbohydrates
    • A61L2300/232Monosaccharides, disaccharides, polysaccharides, lipopolysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION, OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS, OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/20Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
    • A61L2300/252Polypeptides, proteins, e.g. glycoproteins, lipoproteins, cytokines
    • A61L2300/254Enzymes, proenzymes

Abstract

The invention relates to odour-inhibiting mixtures containing water-absorbing polymer particles and irregular, low-dust activated carbon for use in incontinence products.

Description

Odor-inhibiting compounds for incontinence articles

The present invention relates to odor-mixtures comprising water-absorbing polymer particles and irregular, dust-free activated carbon for use in incontinence articles.

Water-absorbing polymer particles are bound to produce diapers, tampons, women's and other hygiene articles, but also used as water-retaining agents in market gardening. The water-absorbing polymer particles are also referred to as superabsorbents.

The production of water-absorbing polymer particles is described in the monograph "Modern Su- perabsorbent Polymer Technology", FL Buchholz and AT. Graham, Wiley-VCH, 1998, pages 71 to 103. described.

The properties of water-absorbing polymer particles can be adjusted, for example via the amount of crosslinker used. With increasing amount of crosslinker the cen- decreases rifugenretentionskapazität (CRC) and the absorption under a pressure of 21, 0 g / cm 2 (AUL0.3 psi) passes through a maximum.

To improve the application properties, such as permeability of the swollen gel bed (SFC) in the diaper and Absorbency under a pressure of 49.2 g / cm 2

(AUL0.7 psi) are crosslinked water-absorbing polymer particles are generally oberflächennach-. Characterized the degree of crosslinking of the particle surface area increases, whereby the absorbency (CRC) can be at least partially decoupled under a pressure of 49.2 g / cm 2 (AUL0.7 psi), and centrifuge retention capacity. This surface can be performed in aqueous gel phase. Preferably, however, dried, ground and screened polymer particles (base polymer) are coated with a postcrosslinker on the surface and surface thermally surface postcrosslinked. Useful crosslinkers are compounds which can form covalent bonds with at least two carboxylate groups of the water-absorbing polymer particles. There has been no lack of attempts unpleasant odors in the application of hygiene products to prevent. According to US 2008/0179 A1, US 2008/0147028 A1, US 2010/0286645 A1, EP 1358894 A1 and WO 98/26808 A2 can for this purpose, for example, activated carbon can be used. Object of the present invention to provide an improved odor-mixtures for use in incontinence articles. The mixtures should in particular have a higher degree of whiteness. Furthermore, the parts of the plant used to prepare the odor-mixtures should be easy to clean, so that when changing products, contamination of the subsequent production campaign is avoided. The object is achieved by odor-mixtures comprising water-absorbing polymer particles and irregular particles of activated carbon having a dust figure of less than 50, preferably less than 45, more preferably less than 40, most preferably less than 35. Activated carbon is commonly referred to as powder, irregular particles or rod-shaped pellets used. The inventive irregular activated carbon particles is particularly low-dust activated carbon. Such particularly dust-free activated carbons are commercially available, for example, Norit GCN3070 (Norit Nederland BV, Amersfoort, Netherlands). The water-absorbing polymer particles are, for example, by polymerizing a monomer solution or suspension comprising a) at least one ethylenically unsaturated monomer bearing acid groups, which may be at least partially neutralized,

b) at least one crosslinker,

c) at least one initiator,

d) optionally one or more copolymerizable with the above-mentioned under a) monomers ethylenically unsaturated monomers and

e) optionally one or more water-soluble polymers produced, and are typically water insoluble.

The monomers a) are preferably water-soluble, that is, the solubility in water at 23 ° C is typically at least 1 g / 100 g water, preferably at least 5 g / 100 g water, more preferably at least 25 g / 100 g of water, most preferably at least 35 g / 100 g water.

Suitable monomers a) are for example ethylenically unsaturated carboxylic acids such as acrylic acid, methacrylic acid, and itaconic acid. Particularly preferred monomers are acrylic acid and methacrylic acid. Most particularly preferred is acrylic acid.

Further suitable monomers a) are, for example, ethylenically unsaturated sulfonic acids such as styrenesulfonic acid and 2-acrylamido-2-methylpropanesulfonic acid (AMPS).

Impurities can have a considerable influence on the polymerization. Therefore, the raw materials used should have the highest possible purity. Therefore, it is often advantageous to purify the monomers a) specifically. Suitable purification processes are beispiels-, in WO 2002/055469 A1, WO 2003/078378 A1 and WO 2004/035514 A1. A suitable monomer a) is, for example, according to WO 2004/035514 A1 purified acrylic acid having 99.8460 wt .-% of acrylic acid, 0.0950 wt .-% acetic acid,

0.0332 wt .-% water, 0.0203 wt .-% by weight of propionic acid, 0.0001 wt .-% furfurals, 0.0001 wt .-% of maleic anhydride, 0.0003 wt .-% diacrylic acid and 0.0050. -% hydroquinone monomethyl ether.

The proportion of acrylic acid and / or salts thereof to the total amount of monomers is preferably at least 50 mol%, particularly preferably at least 90 mol%, most preferably at least 95 mol%.

The acrylic acid used will usually contain polymerization inhibitors, preferably hy- rochinonhalbether, as a storage stabilizer. Therefore, the monomer solution comprises preferably up to 250 ppm by weight, preferably at most 130 ppm by weight, particularly preferably at most 70 ppm by weight, preferably at least 10 ppm by weight, particularly preferably at least 30 ppm by weight, especially around 50 ppm by weight, hydro- chinonhalbether, each relative to the unneutralized acrylic acid. For example, an acrylic acid can be used with an appropriate content of hydro chinonhalbether for preparing the monomer solution.

Preferred hydroquinone monoethers are hydroquinone monomethyl ether (MEHQ) and / or alpha-tocopherol (vitamin E). Suitable crosslinkers b) are compounds having at least two groups suitable for crosslinking. Such groups are for example ethylenically unsaturated groups which can be free-radically interpolymerized into the polymer chain and functional groups which can form covalent bonds with the acid groups of the acrylic acid. Also suitable are polyvalent metal salts which can form fertilize coordinative bond with at least two acid groups of the acrylic acid suitable crosslinkers b).

Crosslinkers b) are preferably compounds having at least two polymerizable groups which can be free-radically interpolymerized into the polymer network. Suitable crosslinkers b) are, for example, ethylene glycol dimethacrylate, diethylene glycol diacrylate, Polyethylenglykoldi- acrylate, allyl methacrylate, trimethylolpropane triacrylate, triallylamine, tetraallylammonium chloride, tetraallyloxyethane as described in EP 0530438 A1, di- and triacrylates as described in EP 0547847 A1, EP 0559476 described A1, EP 0632068 A1, WO 93/21237 A1, WO 2003/104299 A1, WO 2003/104300 A1, WO 2003/104301 A1 and DE 103 31 450 A1, mixed te acrylamide, the more well as acrylate ethylenically unsaturated groups, as described in DE 103 31 456 A1 and DE 103 55 401 A1, or crosslinker mixtures as described for example in DE 195 43 368 A1, DE 196 46 484 A1, WO 90/15830 A1 and WO 2002/032962 A2. Preferred crosslinking agents are b) pentaerythritol triallyl ether, tetraallyloxyethane, Methylenbismethac- rylamid, 15-tuply ethoxylated trimethylolpropane triacrylate, polyethylene glycol diacrylate, trimethylolpropane triacrylate and triallylamine.

Very particularly preferred crosslinkers b) are the acrylic acid or methacrylic acid to di- or triacrylates esterified multiply ethoxylated and / or propoxylated glycerols as described for example in WO 2003/104301 A1. Particularly advantageous are di- and / or triacrylates of 3- to 10-tuply ethoxylated glycerol. Very particular preference is given to di- or triacrylates of 1 - to 5-tuply ethoxylated and / or propoxylated glycerol. Most preferred are the triacrylates of 3- to 5-tuply ethoxylated and / or propoxylated glycerol, especially the triacrylate of 3-tuply ethoxylated glycerol.

The amount of crosslinker b) is preferably 0.05 to 1, 5 wt .-%, particularly preferably 0.1 to 1 wt .-%, most preferably 0.2 to 0.6 wt .-%, each based on acrylic acid. With increasing crosslinker content, the centrifuge retention capacity (CRC) and absorbance drops below a pressure of 21, 0 g / cm 2 passes through a maximum.

The initiators c) all -Create radicals under the polymerization de compounds can be used, for example, thermal initiators, redox initiators, photoinitiators. Suitable redox initiators are sodium peroxodisulfate / ascorbic acid, water peroxide / ascorbic acid, sodium peroxodisulfate / sodium bisulfite and hydro- gen peroxide / sodium bisulfite. Preferably, mixtures of thermal initiators and redox initiators are used, such as sodium / hydrogen peroxide / ascorbic acid. As reducing component is but is preferably a mixture of the sodium salt of 2-

Hydroxy-2-sulfinatoacetic acid, the disodium salt of 2-hydroxy-2-sulfonatoacetic acid and sodium bisulfite. Such mixtures are as Brüggolite® FF6 and FF7 Brüggolite® available (Bruggemann Chemicals; Germany; Heilbronn). With acrylic acid copolymerizable ethylenically unsaturated monomers d) are for example acrylamide, methacrylamide, hydroxyethyl acrylate, hydroxyethyl methacrylate, dimethylaminoethyl methacrylate, dimethylaminoethyl acrylate, dimethylaminopropyl acrylate, diethylaminopropyl acrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate. As water-soluble polymers e) include polyvinyl alcohol, polyvinylpyrrolidone, starch, starch derivatives, modified cellulose, such as methylcellulose or hydroxyethylcellulose, gelatin, polyglycols or polyacrylic acids, preferably starch, starch derivatives and modified cellulose may be used. Typically, an aqueous monomer solution is used. The water content of the monomer solution is preferably from 40 to 75 wt .-%, particularly preferably from 45 to 70% by weight, most preferably from 50 to 65 wt .-%. It is also possible Monomersuspensio- NEN, ie monomer solutions with excess acrylic acid, for example sodium use. With increasing water content, the energy consumption increases in the subsequent drying and, with falling water content, the heat of polymerization can only be removed inadequately.

The preferred polymerization inhibitors require dissolved oxygen for optimum effect. Therefore, the monomer solution before the polymerization by inertization, ie flowing through with an inert gas, preferably nitrogen or carbon dioxide, be freed of dissolved oxygen. Preferably, the oxygen content of the monomer solution before the polyvinyl lymerisation to less than 1 ppm by weight, particularly preferably very particularly preferably lowered to less than 0.5 ppm by weight to less than 0.1 ppm by weight.

Suitable reactors are, for example, kneading or belt reactors. In the kneader, polyvinyl formed during the polymerization of an aqueous monomer solution or suspension is lymergel by, for example, counter-rotating agitator shafts continuous comminution, as in

WO 2001/038402 A1. The polymerization on the belt is described for example in DE 38 25 366 A1 and US 6,241, 928th In the polymerization in a belt reactor a polymer gel which has to be comminuted in a further process step, for example in an extruder or kneader is produced.

For improving the drying properties of the crushed polymer gel obtained by means of a kneader, can also be extruded.

The acid groups of the polymer gels are typically partly neutralized. The neutralization is preferably carried out at the stage of the monomers. This is usually done by mixing in the neutralizing agent as an aqueous solution or else preferably as a solid. The degree of neutralization is preferably from 25 to 95 mol%, particularly preferably from 30 to 80 mol%, very particularly preferably from 40 to 75 mol%, for which the customary neutralizing agents can be used, preferably alkali metal hydroxides, alkali metal oxides, alkali metal carbonates or alkali metal hydrogencarbonates and mixtures thereof. Instead of alkali metal salts and ammonium salts can be used. Sodium and potassium are particularly preferred as alkali metals, but very particular preference is given to sodium hydroxide, sodium carbonate or sodium hydrogen carbonate and mixtures thereof.

However, it is also possible for the neutralization after the polymerization carried out at the stage of forming in the polymerization the polymer gel. Furthermore, it is possible up to 40 mol%, preferably 10 to 30 mol%, particularly preferably 15 to 25 mol%, to neutralize the acid groups before polymerization by already added to a portion of the neutralizing agent to the monomer solution and the desired final degree of neutralization only after the polymerization at the stage of the polymer gel is set. When the polymer gel at least partially neutralized after the polymerization, the polymer gel is preferably comminuted mechanically, for example by means of an extruder, wherein the neutralizing agent is sprayed on, sprinkled or poured on and then be carefully mixed. The gel mass obtained can be repeatedly extruded for homogenization.

The polymer gel is then preferably dried with a belt dryer until the residual moisture tegehalt preferably 0.5 to 15 wt .-%, particularly preferably 1 to 10 wt .-%, most preferably 2 to 8 wt .-%, by weight, wherein said residual moisture content according to the recommended by the EDA NA test method no. WSP 230.2-05 "Mass loss Upon Heating" is determined. At too high a residual moisture content, the dried polymer gel has too low a glass transition temperature T g and is difficult to process further. At too low a residual moisture the dried polymer is too brittle, and in the subsequent comminution steps, undesirably large amounts of polymer particles with too small a particle size ( "fines") in. The solids content of the gel before the drying is preferably from 25 to 90 wt. -.%, particularly preferably from 35 to 70 wt .-%, most preferably from 40 to 60 wt .-% can be optionally used for drying feltrockner but also a fluid bed dryer or a Schau-.

The dried polymer is then ground and classified, useful grinding apparatus typically single- or multi-stage rolling mills, preferably two- or three-stage roll mills, pin mills, hammer mills or vibratory mills are used.

In a preferred embodiment of the present invention, an aqueous monomer solution is dropletized and the droplets obtained in a heated carrier gas stream Siert polymerized. Here, the process steps of polymerization and drying can be summarized as described in WO 2008/040715 A2, WO 2008/052971 A1 and in particular in WO

201 1/026876 A1. In this preferred embodiment, the particle size over the size of droplets produced is adjusted.

The average particle size of the water absorbing polymer particles is preferably at least 200 μηη, particularly preferably μηη from 250 to 600, especially from 300 to 500 μηη. The mean particle size can be found in "Particle Size Distribution" by the EDANA recommended test method No. WSP 220.2-05., The mass of the screen fractions are plotted in cumulated form and the mean particle size is determined graphically. The mean particle size here is the value of the mesh size which gives rise to a cumulative 50 wt .-%.

The proportion of particles having a particle size of greater than 150 μηη is preferably at least 90 wt .-%, particularly preferably at least 95 wt .-%, most preferably at least 98 wt .-%. Polymer particles with too small a particle size lower the permeability (SFC). Therefore, the content should be ( "fines") be low for small polymer particles. Too small polymer particles are therefore typically removed and recycled into the process. This is preferably done before, during or immediately after polymerization, that is, before the drying of the polymer gel. The too small polymer particles can be wetted with water and / or aqueous surfactant before or during the recirculation.

It is also possible in later process steps to separate excessively small polymer particles, for example, after the surface or another coating step. In this case, the recycled are surface to small polymer particles or otherwise coated, for example with fumed silica. When a kneading reactor used for polymerization, the small polymer particles are preferably added during the last third of the polymerization.

If the added very early small polymer particles, for example, to the monomer solution, so characterized the centrifuge retention capacity (CRC) of the water obtained is lowered absorbent polymer particles. but this can be compensated, for example, by adjusting the use amount of crosslinker b).

If the added very late excessively small polymer particles, for example, only in a downstream of the polymerization reactor, for example, an extruder, then the excessively small polymer particles can become difficult to incorporate into the resulting polymer. Insufficiently incorporated, excessively small polymer particles dissolve during the grinding process again, are from the dried polymer in classifying therefore removed again and increase the amount of excessively small polymer particles. The proportion of particles μηη with a particle size of at most 850, is preferably at least 90 wt .-%, particularly preferably at least 95 wt .-%, most preferably at least 98 wt .-%.

The proportion of particles having a particle size μηη of 150 to 850, is preferably at least 90 wt .-%, particularly preferably at least 95 wt .-%, most preferably at least 98 wt .-%.

Polymer particles with too large particle size lower the swell rate. The proportion of excessively large polymer particles should also be low.

Excessively large polymer particles are therefore typically removed and recycled into the grinding of the dried polymer gel.

The polymer particles can be networked oberflächennachver- to further improve the properties. Suitable surface postcrosslinkers are compounds containing groups which can form covalent bonds with at least two carboxylate groups of the polymer particles. Suitable compounds are, for example, polyfunctional amines, polyfunctional amidoamines, polyfunctional epoxides, as described in EP 0083022 A2, EP 0543303 A1 and EP 0937736 A2, di- or polyfunctional alcohols as described in DE 33 14 019 A1, DE 35 described 23 617 A1 and EP 0450922 A2, or .beta.-hydroxyalkylamides such as in DE 102 04 938 A1 and US 6,239,230 described.

Further, in DE 40 20 780 C1 cyclic carbonates, by DE 198 07 502 A1 2- oxazolidinone and its derivatives, such as 2-hydroxyethyl-2-oxazolidinone, in DE 198 07 992 C1 bis- and poly-2-oxazolidinones, in DE 198 54 573 A1 2-oxotetrahydro-1, 3-oxazine and its derivatives, by DE 198 54 574 A1 N-acyl-2-oxazolidinones, DE 102 04 937 A1 cyclic ureas, in DE 103 34 584 A1 bicyclic Amidoacetale, in EP 1199327 A2 oxetanes and cyclic ureas and 2003/031482 A1 morpholine-2,3-dione and its derivatives as described in WO suitable surface postcrosslinkers.

Preferred surface are ethylene carbonate, ethylene glycol diglycidyl ether, conversion reduction products of polyamides with epichlorohydrin and mixtures of propylene glycol and 1, 4-butanediol.

Very particularly preferred surface postcrosslinkers are 2-hydroxyethyl-2-oxazolidinone, 2-oxazolidinone and 1, 3-propanediol.

Furthermore, surface postcrosslinkers which comprise additional polymerizable ethylenically unsaturated groups as described in DE 37 13 601 A1

The amount of surface postcrosslinker is preferably from 0.001 to 2 wt .-%, particularly preferably 0.02 to 1 wt .-%, most preferably from 0.05 to 0.2 wt .-%, each based on the polymer particles.

In a preferred embodiment of the present invention before, during or after the surface in addition to the Oberflächennachvernetzern polyvalen- te cations on the particle surface.

The usable in the inventive method polyvalent cations include for example divalent cations such as the cations of zinc, magnesium, calcium, iron and strontium, trivalent cations such as the cations of aluminum, iron, chromium, rare earths and manganese, tetravalent cations such as the cations of titanium and zirconium. Possible counterions are hydroxide, chloride, bromide, sulfate, hydrogensulfate, carbonate, hydrogencarbonate, nitrate, phosphate, hydrogen phosphate, dihydrogen phosphate and carboxylate, such as acetate, citrate and lactate. There are also possible salts having different counter ions, for example, basic aluminum salts such as aluminum mono Aluminiummonoacetat or lactate. miniummonoacetat aluminum sulfate, aluminum lactate, and aluminum are preferred. Apart from metal salts poly- amines can be used as polyvalent cations. The amount of polyvalent cation used is, for example, 0.001 to 1, 5 wt .-%, preferably 0.005 to 1 wt .-%, particularly preferably 0.02 to 0.8 wt .-%. based in each case on the polymer particles. The surface postcrosslinking is typically performed such that a solution of the surface postcrosslinker is sprayed onto the dried polymer particles. Subsequent to the spraying, the polymer particles are coated with surface thermal drying, wherein the surface postcrosslinking can take place both before and during drying.

The spraying of a solution of the surface postcrosslinker is preferably performed in mixers with moving mixing tools, such as screw mixers, disk mixers and shovel mixers. Particular preference is given to horizontal mixers such as paddle mixers, very particular preference to vertical mixers. The distinction in the horizontal mixer and vertical mixer via the bearing of the mixing shaft, ie horizontal mixer having a horizontally mounted mixing shaft and vertical mixers have a vertically mounted mixing shaft. Suitable mixers Horizontal Ploughshare® mixers include for example (Gebr Lödige Maschinenbau GmbH;. Paderborn, Germany), Vrieco-Nauta continuous mixers (Hosokawa Micron BV, Doetinchem, Netherlands), Processall® Mixmill Mixer (Processall® Incorporated; Cincinnati; USA) and Schugi Flexomix® (Hosokawa Micron BV, Doetinchem, Netherlands). but it is also possible the surface postcrosslinker spraying in a fluidized bed.

The surface postcrosslinkers are typically used as an aqueous solution. the input can be set penetration depth of the surface postcrosslinker into the polymer particles on the content of nonaqueous solvent and total amount of solvent.

If only water is used as solvent, a surfactant is advantageously added. Characterized the wetting behavior is improved and reduces the tendency to agglomerate. Preferably, however, solvent mixtures are used, for example, isopropanol / water, 1, 3-propanediol / water and propylene glycol / water, wherein the mixing mass ratio is preferably from 20:80 to 40:60.

The thermal drying is preferably in contact dryers, more preferably paddle dryers, most preferably disk dryers. Suitable dryers are, for example, Hosokawa Bepex® horizontal paddle driers (Hosokawa Micron GmbH;

Leingarten; Germany), Hosokawa Bepex® Disc driers (Hosokawa Micron GmbH; Leingarten, Germany), Holo-Flite® dryers (Metso Minerals Industries Inc .; Danville, USA) and Nara Paddle Dryer (NARA Machinery Europe; Frechen; Germany). Moreover, fluidized bed dryers can be used.

Drying may take place in the mixer itself, by heating the jacket or blowing in warm air. Equally suitable is a downstream dryer, such as a hearing is dentrockner, a rotary tube oven or a heatable screw. Particularly advantageous is mixed in a fluid bed dryer and dried.

Preferred drying temperatures are in the range 100 to 250 ° C, preferably 120 to 220 ° C, particularly preferably 130 to 210 ° C, most preferably 150 to 200 ° C. The preferred residence time at this temperature in the reaction mixer or dryer is preferably at least 10 minutes, more preferably at least 20 minutes, most preferably at least 30 minutes and usually at most 60 minutes. In a preferred embodiment of the present invention, the water-absorbing polymer particles are cooled after the thermal drying. The cooling is preferably in contact coolers, more preferably paddle coolers, disk coolers very particularly preferably carried out. Suitable coolers include, for example Hosokawa Bepex® Horizontal Paddle Cooler (Hosokawa Micron GmbH; Leingarten, Germany), Hosokawa Bepex® Disc Cooler (Hosokawa Micron GmbH; Leingarten, Germany), Holo-Flite® coolers (Metso Minerals Industries Inc .; Danville, USA ) and Nara paddle cooler (NARA Machinery Europe; Frechen; Germany). Moreover, fluidized bed coolers can be used.

In the cooler, the water absorbing polymer particles to 20 to 150 ° C, preferably 30 to 120 ° C, particularly preferably 40 to 100 ° C, most preferably 50 to 80 ° C cooled.

Subsequently, the surface polymer particles can be classified again, be excessively small and / or separated into large polymer particles and recycled to the process.

The surface postcrosslinked polymer particles can be coated or to further improve the properties moistened. The subsequent moistening is preferably carried out at 30 to 80 ° C, particularly preferably at 35 to 70 ° C, very particularly preferably at 40 to 60 ° C. At excessively low temperatures, the water-absorbing polymer particles tend to agglomerate and at higher temperatures, water already evaporates appreciably. The amount of water used for remoisturizing is preferably from 1 to 10 wt .-%, more preferably from 2 to 8 wt .-%, most preferably from 3 to 5 wt .-%. Through the subsequent moistening the mechanical stability of the polymer particles is increased, and reduces their tendency to static charge. the subsequent moistening is advantageously carried out in the cooler by thermal drying.

Suitable coatings for improving the swell rate and the permeabilized ty (SFC) are, for example, inorganic inert substances, such as water-insoluble metal salts, organic polymers, cationic polymers and di- or polyvalent metal cations. Suitable coatings for dust binding are, for example, polyols. Suitable coatings against the undesired caking tendency of the polymer particles include for example fumed silica such as Aerosil® 200, and surfactants, such as Span® 20th

The water-absorbing polymer particles have a centrifuge retention capacity (CRC) of typically at least 15 g / g, preferably at least 20 g / g, preferably at least 22 g / g, more preferably at least 24 g / g, most preferably at least 26 g / g. The centrifuge retention capacity (CRC) of the water-absorbing polymer particles is typically less than 60 g / g. The centrifuge retention capacity (CRC) is determined according to the EDANA recommended test method No. WSP 241.2-05. "Fluid Retention Capacity in Saline, after Centrifugation".

The mixtures according to the invention preferably contain at least 80 wt .-%, preferably at least 85 wt .-%, more preferably at least 90 wt .-%, most preferably at least 95 wt .-%, water-absorbing polymer particles.

The irregular activated carbon particles have a surface area of preferably 10 to 10,000 m 2 / g, particularly preferably from 100 to 5000 m 2 / g, most preferably from 1, 000 to 2,000 m 2 / g. The average particle size of the irregular particles of activated carbon is preferably at least 300 μηη, particularly preferably μηη of 350 to 550, especially 400 to 500 μηη. The average particle size of the product fraction can be found in "Particle Size Distribution" by the EDANA recommended test method No. WSP 220.2-05., The mass of the screen fractions are plotted in cumulated form and the mean particle size is determined graphically. The mean particle size here is the value of the mesh size which gives rise to a cumulative 50 wt .-%.

The percentage of irregular particles of activated carbon μηη having a particle size of 300 to 600, is preferably at least 90 wt .-%, particularly preferably at least 95 wt .-%, most preferably at least 98 wt .-%.

The mixtures according to the invention preferably contain at least 0.1 wt .-%, particularly preferably at least 0.5 wt .-%, preferably 1 wt .-% at least, very particularly preferably at least 5 wt .-%, irregular particles of activated carbon.

The manner of mixing is not limited, and may be carried out post-crosslinking or the subsequent sizing, or in a special mixer during the production of the water-absorbing polymer particles, for example in cooling after the surface. Suitable mixers have already been described above for the surface postcrosslinking of water-absorbing polymer particles. The present invention is based on the recognition that low-dust activated carbon particles have a higher abrasion resistance and mostly isolated are present in the blends of this invention in addition to the water-absorbing polymer particles. The formation of particulate matter or a coloring the water-absorbing polymer particles by abrasion is avoided.

The odor-inhibiting mixtures may additionally contain metal peroxides, oxidases and / or zeolites. The metal peroxide is preferably the peroxide is a metal of the first Main group, the second

Main group and / or the second subgroup of the Periodic Table of the Elements, most preferably the peroxide is a metal of the second transition group of the Periodic Table of Elements.

Suitable metal peroxides are, for example lithium peroxide, strontium peroxide, barium peroxide, sodium peroxide, magnesium peroxide, calcium peroxide and potassium hyperoxide, particularly preferably zinc peroxide.

The mixture according to the invention preferably contains 0.001 to 5 wt .-%, preferably from 0.01 to 3 wt .-%, particularly preferably from 0.1 to 1, 5 wt .-%, most preferably from 0.2 to 0 8 wt .-%, of metal peroxide.

Metal peroxides, zinc peroxide, in particular, have a good odor-inhibiting effect, and the mixtures thus produced have a high storage stability. The mixtures preferably contain less than 1 ppm, more preferably less than 10 ppm, most preferably less than 5 ppm, heavy metal ions. Heavy metal ions, especially iron ions, lead to the catalytic decomposition of the metal peroxides and thus reduce the storage stability of the mixtures. Suitable zeolites are, for example, zeolites with cations of main group 1, the second main group, of the first Sub-group and / or the second subgroup of the Periodic Table of Elements.

Suitable cations are, for example, zinc cations, silver and copper cations cations, particularly preferably titanium cations.

The mixture according to the invention preferably contains 0.001 to 5 wt .-%, preferably from 0.01 to 3 wt .-%, particularly preferably from 0.1 to 1, 5 wt .-%, most preferably from 0.2 to 0 8 wt .-%, of the zeolite.

Zeolites also have a good odor-inhibiting effect. Suitable oxidases are oxidases of the group EC 1 .1 .3.x as glucose oxidases (EC number 1 .1 .3.4), the group EC 1 .3.3.x as bilirubin oxidases (EC number 1.3.3.5), the group EC 1 .4.3.x as Glyzinoxidasen (EC number 1 .4.3.19), the group EC 1 .5.3.x as Polyaminoxi- Dasen (EC number 1.5.3.1 1), the group EC 1.6.3. x, such as NAD (P) H oxidases (EC number 1 .6.3.1), the group EC 1.7.3.x, such as Hydroxylaminoxidasen (EC number 1.7.3.4), the group EC 1.8.3.x, as Sulfitoxidasen (EC number 1 .8.3.1), the group EC 1.9.3.x, such as Cytochro- moxidasen (EC number 1.9.3.1), the group EC 1 .10.3.x as catechol (EC-number 1 .10.3.1), the group EC 1.16.3.x as ferroxidase (EC number 1.16.3.1), the group EC 1 .17.3.x as xanthine oxidases (EC number 1.17.3.2), and the group EC 1 .21 .3.z as Reticu- linoxidasen (EC number one .21.3.3).

a glucose oxidase (EC number 1.1.3.4) is advantageously used. Is even more advantageous when the glucose very little or no catalase (EC number 1.1 1 .1.6) contains is. The specific catalytic oxidase activity of the odor-inhibiting mixture is preferably from 0.01 to 1000 g μηηοΙ substrate _1 min -1, more preferably from 0.1 to 100 g _1 μηηοΙ substrate -min -1, most preferably from 1 to 10 g substrate μηηοΙ _1 min -1.

The specific catalytic oxidase activity of the mixture is deter- mined by conventional methods. but is better the catalytic activity of the oxidase itself to determine and identify the specific catalytic oxidase activity of the mixture by calculation.

Oxidases can reduce unpleasant odors caused by sulfur compounds particularly unpleasant odors. Maybe this is effected generated by see as a result of catalytic oxidase hydrogen peroxide. Therefore, concomitant use of peroxidases should be avoided.

The odor-mixtures can additionally contain the substrate of the oxidase. A Substart is a compound that is converted by the enzyme is in a chemical reaction. The first step in an enzymatic reaction is the formation of an enzyme-substrate complex that leads to the reaction the release of product and enzyme, so that the catalytic cycle can be run through again. An enzyme may possibly transpose several different substarte that are often chemically similar. Substrates in the sense of the present invention are substrates of the invention can be used according oxidases, for example, .beta.-D-glucose for glucose oxidase.

There are preferably from 0.5 to 25 wt .-%, particularly preferably from 5 to 20 wt .-%, most preferably from 8 to 15 wt .-% of the substrate used, based on the water-absorbing polymer particles.

The substrates can also be used encapsulated, so that they are available only with the addition of liquid of the oxidase available, for example, by coating with water soluble polymers such as polyvinyl alcohol. but it is also possible instead, or in addition to encapsulate according to invention oxidases.

Another object of the present invention are hygienic articles comprising a dung inventions proper mixture, in particular hygiene products for light and heavy incontinence.

The hygiene articles usually comprise a water-impermeable back side, a water-permeable top and therebetween an absorbent core of the present invention water-absorbing polymer particles and fibers, preferably cellulose. The proportion of the water-absorbing polymer particles in the absorbent core according to the invention is preferably 20 to 100 wt .-%, preferably 50 to 100 wt .-%.

Methods: The measurements should, unless stated otherwise, be carried out at an ambient temperature of 23 ± 2 ° C and a relative humidity of 50 ± 10%. The water-absorbing polymer particles are mixed thoroughly before the measurement.

CIE color number (L, a, b)

The color measurement is made in accordance with the CIELAB procedure (Hunterlab, volume 8, 1996, issue 7, pages 1 to 4) with a colorimeter, Model "LabScan XE S / N LX17309" (hunger terLab, Reston, US). This the colors via the coordinates L, a and b of a three-dimensional system will be described. Here, L indicates the brightness, where L = 0 means black and L = 100 white. the values ​​for a and b indicate the position of the color on the color axes red / green and yellow / blue respectively, where + a is red, -a represents green, + b yellow and -b for blue. According to the formula HC60 = L-3b, the HC60 value is calculated.

The color measurement complies with the three-range method of DIN 5033-6.

dust count

In determining the number of dust dusting amounts of solids which formed after a defined stress on the material (free fall and impact) are recorded quantitatively.

The dust number of water-absorbing polymer particles by means of the dust measuring device type DustView (Palas GmbH, Karlsruhe, Germany) determined.

The mechanical part of the measuring device consists of hopper with flap, dust drop tube and housing with a removable dust box. The down pipe has a length of 780 mm. The dust case has a length of 195 mm, a width of 190 mm and a height of 185 mm. The sample amount is 30 g. For measurement, the sample falls through the downcomer in the dust box.

The evaluation is carried optoelectronic. The dusty solids content leads to the attenuation of a light beam, which is detected photometrically. The measurement is carried out 130 mm above the bottom of the dust casing. is measured, the percentage attenuation of the

Lichtstrrahls. A reading of 100 corresponds to a complete slowdown. The

Measured value recording and evaluation takes place in the control unit. The following measurements are displayed as a numerical value on the control unit:

1 . Initial value (measured value after 0.5 seconds)

2. Dust value (measured value after 30 seconds)

3. dust count The dust number is the sum of the initial value and dust level.

Examples Examples 1 to 5

55 g of water-absorbing polymer particles (HySorb® B7055; BASF SE; DE) and 2.75 g of irregular particles of activated carbon were weighed into a 100ml plastic square bottle. This mixture was homogenized for 15 minutes at 49Upm tumbled and analyzed. The results of ER are summarized in Table 1 (sample A).

Then the 100ml plastic square bottle was empty and not cleaned. There were weighed 55g water-absorbing polymer particles again, but no activated carbon. This mixture was also homogenized for 15 minutes at 49Upm tumbled and analyzed. The results are summarized in Table 1 (sample B).

Tab. 1: addition of different activated carbons to HySorb® B7055

Figure imgf000017_0001

*) Not inventive

Examples 1 to 5 were with HySorb® B7055 (BASF SE; Ludwigshafen; Germany), commercially available surface-postcrosslinked water-absorbing polymer particles on Natriu- macrylatbasis with a degree of neutralization of 70 mol%, performed. Such oberflachennachvernetzte water-absorbing polymer particles are, for example, by BASF Aktiengesellschaft (trade name HySorb®), from Stockhausen GmbH (trade name Favor®) and Nippon Shokubai Co., Ltd. (Trade name Aqualic®) commercially available.

As irregular particles of activated carbon 1 to 4 dust-free activated carbon were used in Examples of the type Norit GCN3070 (Norit Nederland BV, Amersfoort, Netherlands), optionally mixed with active coal dust, are used.

(Germany Sig- ma-Aldrich Chemie GmbH;; Steinheim) was used as irregular particles of activated carbon in Example 5, activated carbon type Supelco 31,616th

Claims

claims
1 . Odor-mixtures comprising water-absorbing polymer particles and irregular particles of activated carbon having a dust figure of less than 50th
2. Mixtures according to claim 1, characterized in that the mixtures contain at least 80 wt .-% water-absorbing polymer particles.
3. Mixtures according to claim 1 or 2, characterized in that the wasserabsor--absorbing polymer particles μηη have an average particle size of 250 to 600 bar.
4. Mixtures according to one of claims 1 to 3, characterized in that the water absorbing polymer particles μηη comprise at least 90 wt .-% having a particle size of 150 to 850th
5. Mixtures according to one of claims 1 to 4, characterized in characterized in that the water-absorbing polymer particles have a Zentrifugenretenti- onskapazität of at least 15 g / g.
6. Mixtures according to one of claims 1 to 5, characterized in that the mixtures contain at least 1 wt .-% activated carbon irregular particles.
7. Mixtures according to one of claims 1 to 6, characterized in that the irregular particles of activated carbon μηη have an average particle size of 350 to 550.
8. Mixtures according to one of claims 1 to 7, characterized in that the irregular particles of activated carbon μηη comprise at least 90 wt .-% having a particle size of 300 to 600 bar.
9. Mixtures according to one of claims 1 to 8, characterized in that the irregular activated carbon particles have a surface area of 10 to 10,000 m 2 / g.
10. Mixtures according to one of claims 1 to 9, characterized in that the mixtures additionally contain a metal peroxide.
1. 1 Mixtures according to claim 10, characterized in that the metal peroxide is zinc peroxide.
12. Mixtures according to one of claims 1 to 1 1, characterized in that the mixtures additionally contain an oxidase.
13. Mixtures according to claim 12, characterized in that the oxidase is gluco- seoxidase.
14. Mixtures according to claim 13, characterized in that the mixtures additionally contain lent glucose.
15. A hygiene article comprising mixtures according to one of claims 1 to 14.
PCT/EP2013/064412 2012-07-30 2013-07-08 Odour-inhibiting mixtures for incontinence products WO2014019813A1 (en)

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