JP5290413B2 - 吸水性ポリマー粒子の製造方法 - Google Patents
吸水性ポリマー粒子の製造方法 Download PDFInfo
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- JP5290413B2 JP5290413B2 JP2011517851A JP2011517851A JP5290413B2 JP 5290413 B2 JP5290413 B2 JP 5290413B2 JP 2011517851 A JP2011517851 A JP 2011517851A JP 2011517851 A JP2011517851 A JP 2011517851A JP 5290413 B2 JP5290413 B2 JP 5290413B2
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- particles
- water
- sieving
- monomer
- reducing agent
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- 238000007873 sieving Methods 0.000 claims description 35
- 238000006116 polymerization reaction Methods 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 28
- 239000003638 chemical reducing agent Substances 0.000 claims description 17
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- 238000001035 drying Methods 0.000 claims description 12
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 10
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- 238000000576 coating method Methods 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 238000004132 cross linking Methods 0.000 claims description 8
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- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical group O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 3
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- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 3
- IZXIZTKNFFYFOF-UHFFFAOYSA-N 2-Oxazolidone Chemical compound O=C1NCCO1 IZXIZTKNFFYFOF-UHFFFAOYSA-N 0.000 description 3
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- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
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- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 description 2
- CEFDWZDNAJAKGO-UHFFFAOYSA-N 2-hydroxy-2-sulfoacetic acid Chemical compound OC(=O)C(O)S(O)(=O)=O CEFDWZDNAJAKGO-UHFFFAOYSA-N 0.000 description 2
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- 229920000954 Polyglycolide Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- ZZAGLMPBQOKGGT-UHFFFAOYSA-N [4-[4-(4-prop-2-enoyloxybutoxy)benzoyl]oxyphenyl] 4-(4-prop-2-enoyloxybutoxy)benzoate Chemical compound C1=CC(OCCCCOC(=O)C=C)=CC=C1C(=O)OC(C=C1)=CC=C1OC(=O)C1=CC=C(OCCCCOC(=O)C=C)C=C1 ZZAGLMPBQOKGGT-UHFFFAOYSA-N 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 229940048053 acrylate Drugs 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 1
- 150000008041 alkali metal carbonates Chemical class 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 229940087168 alpha tocopherol Drugs 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000011126 aluminium potassium sulphate Nutrition 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 229920006317 cationic polymer Polymers 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 150000005676 cyclic carbonates Chemical class 0.000 description 1
- WPCPXPTZTOMGRF-UHFFFAOYSA-K di(butanoyloxy)alumanyl butanoate Chemical compound [Al+3].CCCC([O-])=O.CCCC([O-])=O.CCCC([O-])=O WPCPXPTZTOMGRF-UHFFFAOYSA-K 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- KLSBASGQHCAVHQ-UHFFFAOYSA-L disodium;2-hydroxy-2-sulfinatoacetate Chemical compound [Na+].[Na+].[O-]C(=O)C(O)S([O-])=O KLSBASGQHCAVHQ-UHFFFAOYSA-L 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000002314 glycerols Chemical class 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
- 229920001477 hydrophilic polymer Polymers 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910003480 inorganic solid Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910001463 metal phosphate Inorganic materials 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- MENOBBYDZHOWLE-UHFFFAOYSA-N morpholine-2,3-dione Chemical compound O=C1NCCOC1=O MENOBBYDZHOWLE-UHFFFAOYSA-N 0.000 description 1
- BPLYVSYSBPLDOA-GYOJGHLZSA-N n-[(2r,3r)-1,3-dihydroxyoctadecan-2-yl]tetracosanamide Chemical compound CCCCCCCCCCCCCCCCCCCCCCCC(=O)N[C@H](CO)[C@H](O)CCCCCCCCCCCCCCC BPLYVSYSBPLDOA-GYOJGHLZSA-N 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- AHHWIHXENZJRFG-UHFFFAOYSA-N oxetane Chemical compound C1COC1 AHHWIHXENZJRFG-UHFFFAOYSA-N 0.000 description 1
- 150000002924 oxiranes Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 229940085991 phosphate ion Drugs 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 239000004633 polyglycolic acid Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229940050271 potassium alum Drugs 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000011127 sodium aluminium sulphate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- CSMWJXBSXGUPGY-UHFFFAOYSA-L sodium dithionate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)S([O-])(=O)=O CSMWJXBSXGUPGY-UHFFFAOYSA-L 0.000 description 1
- 229940075931 sodium dithionate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000011877 solvent mixture Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 229920000247 superabsorbent polymer Polymers 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229960000984 tocofersolan Drugs 0.000 description 1
- AOBORMOPSGHCAX-DGHZZKTQSA-N tocofersolan Chemical compound OCCOC(=O)CCC(=O)OC1=C(C)C(C)=C2O[C@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C AOBORMOPSGHCAX-DGHZZKTQSA-N 0.000 description 1
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 239000002076 α-tocopherol Substances 0.000 description 1
- 235000004835 α-tocopherol Nutrition 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS 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
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/60—Liquid-swellable gel-forming materials, e.g. super-absorbents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/126—Polymer particles coated by polymer, e.g. core shell structures
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/128—Polymer particles coated by inorganic and non-macromolecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/245—Differential crosslinking of one polymer with one crosslinking type, e.g. surface crosslinking
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
- C08J2300/14—Water soluble or water swellable polymers, e.g. aqueous gels
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Animal Behavior & Ethology (AREA)
- Hematology (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Crystallography & Structural Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Absorbent Articles And Supports Therefor (AREA)
Description
a)少なくとも1のエチレン性不飽和の、酸基を有するモノマー、これは少なくとも部分的に中和されていてよい、
b)少なくとも1の架橋剤、
c)少なくとも1の開始剤、
d)場合により1もしくは複数の、a)に記載したモノマーと共重合可能なエチレン性不飽和モノマー、および
e)場合により1もしくは複数の水溶性ポリマー
を含有するモノマー溶液またはモノマー懸濁液の重合により、吸水性ポリマー粒子を製造する方法であって、以下の工程:
i)モノマー溶液またはモノマー懸濁液を重合してポリマーゲルを得る工程、
ii)ポリマーゲルを乾燥させる工程、
iii)乾燥させたポリマーゲルを粉砕する工程、および
iv)分級し、その際、篩下粒子を分離する工程
を有し、この場合、分離した篩下粒子は、少なくとも部分的に工程ii)の前に返送される吸水性ポリマー粒子の製造方法において、返送される篩下粒子の少なくとも一部の量が、少なくとも1の還元剤および/または無機粒子により被覆されていることを特徴とする、吸水性ポリマー粒子の製造方法によって解決された。
測定は、その他の記載がない限り、23±2℃の周囲温度および50±10%の相対空気湿度で実施すべきものである。吸水性ポリマー粒子は、測定前に十分に混合される。
残留モノマー(Remos)は、EDANA(European Disposables and Nonwovens Association)により推奨される試験法No.WSP210.2−05「残留モノマー」により測定される。
粒径分布(PSD)は、EDANA(European Disposables and Nonwovens Association)により推奨される試験法No.WSP220.2−05「粒径分布」により測定される。
遠心分離保持容量(CRC)は、EDANA(European Disposables and Nonwovens Association)により推奨される試験法No.WSP241.2−05「遠心分離保持容量」により測定される。
21.0g/cm2の加圧下での吸収(AUL0.3psi)は、EDANA(European Disposables and Nonwovens Association)により推奨される試験法No.WSP242.2−05「加圧下での吸収(Absorption Under Pressure)」により測定される。
49.2g/cm2の加圧下での吸収(AUL0.7psi)は、EDANA(European Disposables and Nonwovens Association)により推奨される試験法No.WSP242.2−05「加圧下での吸収(Absorption Under Pressure)」により測定されるが、この場合、21.0g/cm2の圧力(AUL0.3psi)に代えて、49.2g/cm2の圧力(AUL0.7psi)に調整される。
膨潤速度(FSR)を測定するために、乾燥した吸水性ポリマー粒子1.00g(=W1)を25mlのガラスビーカー中に秤量し、かつその底に均一に分散させる。次いで、0.9質量%の食塩溶液20mlを第二のガラスビーカー中に供給する。このビーカーの内容物を第一のビーカーに素早く添加し、ストップウォッチを開始する。塩溶液の最後の1滴が吸収されたらストップウォッチを止めるが、これは液体表面上の反射の消失によって認識可能である。第二のガラスビーカーから注いだ液体および第一のガラスビーカー中のポリマーにより吸収された液体の正確な量を、第二のガラスビーカーの秤量により正確に測定する(=W2)。ストップウォッチで測定した、吸収のために必要とされた時間を、tとする。
FSR[g/gs]=W2/(W1×t)
色の測定はCIELAB法(Hunterlab、第8巻、1996年、第7号、第1〜4頁)に相応して実施した。この場合、色は三次元系の座標L*、a*およびb*により記載される。その際、L*は明度を表し、L*=0は黒色を、およびL*=100は白色を意味する。a*およびb*の値は、色軸の赤色/緑色もしくは黄色/青色上の色の位置を示し、+a*は赤色を、−a*は緑色を、+b*は黄色を、および−b*は青色を表す。色測定装置はModell LabScan XE S/N LX17309(Hunterlab、Reston、US)を使用した。
例1(ベースポリマーの製造)
37.3質量%のアクリル酸ナトリウム水溶液1028g、アクリル酸98g、水254gおよびエトキシ単位を3つ有するグリセリントリアクリレート0.59gを、2000mlの金属製ビーカー中に秤量した。中和度は75モル%であった。金属製ビーカーをParafilm(登録商標)でふさぎ、150l/hの窒素で不活性化した。不活性化の間、モノマー溶液を−0.5℃に冷却した。引き続き10質量%の過硫酸ナトリウムの10質量%水溶液6.47gおよび過酸化水素の1質量%水溶液5.88gを順次添加した。
37.3質量%のアクリル酸ナトリウム水溶液1028g、アクリル酸98g、水254gおよびエトキシ単位を3つ有するグリセリントリアクリレート0.59gを、2000mlの金属製ビーカー中に秤量した。中和度は75モル%であった。金属製ビーカーをParafilm(登録商標)でふさぎ、150l/hの窒素で不活性化した。不活性化の間、モノマー溶液を−0.5℃に冷却した。引き続き過硫酸ナトリウムの10質量%水溶液6.47gおよび過酸化水素の1質量%水溶液5.88gを順次添加した。
例2に記載のとおりに行った。重合後に得られたポリマーゲルに混入した篩下粒子を、返送前に次亜リン酸ナトリウムで被覆した。
このために、例1からの篩下粒子84gを、キッチン用装置に充填し、撹拌した。撹拌される篩下粒子に、2流体ノズルで次亜リン酸ナトリウムの3質量%水溶液16.8gを噴霧し、かつ5分間、後攪拌した。被覆した篩下粒子を、4つのペトリ皿(直径13.5cm、高さ2.5cm)に分散させ、かつ150℃で30分間、循環空気式乾燥棚で乾燥させた。引き続き、コーヒーミルで脱凝集させ、かつ150μmに篩分した。
例2に記載のとおりに行った。重合後に得られたポリマーゲルに混入した篩下粒子を、返送前にBrueggolite(登録商標)FF7(Brueggemann Chemicals、Heilbronn、ドイツ)で被覆した。Brueggolite(登録商標)FF7は、2−ヒドロキシ−2−スルフィナト酢酸の二ナトリウム塩、2−ヒドロキシ−2−スルホナト酢酸の二ナトリウム塩および二亜硫酸ナトリウムからなる混合物である。
このために、例1からの篩下粒子84gを、キッチン用装置に充填し、撹拌した。撹拌された篩下粒子に、2流体ノズルでBrueggolite(登録商標)FF7の1質量%水溶液8.4gを噴霧し、かつ5分間、後攪拌した。被覆した篩下粒子を、4つのペトリ皿(直径13.5cm、高さ2.5cm)に分散させ、かつ150℃で30分間、循環空気式乾燥棚で乾燥させた。引き続き、コーヒーミルで脱凝集させ、かつ150μmに篩分した。
例2に記載のとおりに行った。重合後に得られたポリマーゲルに混入した篩下粒子を、返送前にSipernat(登録商標)D17(Evonik Industries AG、Essen、ドイツ)で被覆した。Sipernat(登録商標)D17は、熱分解法シリカである。
このために、篩下粒子84gおよびSipernat(登録商標)D17 0.25gを、250mlのガラス瓶に充填し、回転式ミキサーで30分間均質化した。
例2に記載のとおりに行った。重合後に得られたポリマーゲルに混入した篩下粒子を、返送前にリン酸三カルシウムC13−09(Chemische Fabrik Budenheim KG、Budenheim、ドイツ)で被覆した。
このために、篩下粒子84gおよびリン酸三カルシウムC13−09 0.42gを、250mlのガラス瓶に充填し、回転式ミキサーで30分間均質化した。
例1で製造したベースポリマーを表面後架橋した。
例7と同様に行った。例2で製造したベースポリマーを使用した。
例7と同様に行った。例3〜6で製造したベースポリマーを使用した。
Claims (11)
- a)少なくとも1のエチレン性不飽和の、酸基を有するモノマー、
b)少なくとも1の架橋剤、
c)少なくとも1の開始剤、
d)場合により1もしくは複数の、a)に記載したモノマーと共重合可能なエチレン性不飽和モノマー、および
e)場合により1もしくは複数の水溶性ポリマー
を含有するモノマー溶液またはモノマー懸濁液の重合により、吸水性ポリマー粒子を製造する方法であって、以下の工程:
i)モノマー溶液またはモノマー懸濁液を重合してポリマーゲルを得る工程、
ii)ポリマーゲルを乾燥させる工程、
iii)乾燥させたポリマーゲルを粉砕する工程、および
iv)分級し、その際、篩下粒子を分離する工程
を有し、この場合、分離した篩下粒子は、少なくとも部分的に工程ii)の前に返送される吸水性ポリマー粒子の製造方法において、吸水性ポリマー粒子を工程iv)の前に、表面後架橋させ、返送される篩下粒子の少なくとも一部の量が、少なくとも1の還元剤により、または還元剤および無機粒子により被覆されており、還元剤が、次亜リン酸の塩またはスルフィン酸の塩であることを特徴とする、吸水性ポリマー粒子の製造方法。 - 工程iii)の後かつ表面後架橋の前に、さらに分級し、篩下粒子を分離することを特徴とする、請求項1記載の方法。
- 表面後架橋の前に分離した篩下粒子を、工程iv)で分離した篩下粒子と一緒に返送することを特徴とする、請求項2記載の方法。
- 還元剤により、または還元剤および無機粒子により被覆されている、返送される篩下粒子のうち、モノマー溶液またはモノマー懸濁液の固体含有率に対して、1〜20質量%の量を、工程iv)の前に被覆することを特徴とする、請求項1から3までのいずれか1項記載の方法。
- 還元剤により、または還元剤および無機粒子により被覆されている、返送される篩下粒子のうち、モノマー溶液またはモノマー懸濁液の固体含有率に対して、1〜20質量%の量を、表面後架橋の後に被覆することを特徴とする、請求項1から4までのいずれか1項記載の方法。
- 分離した篩下粒子を工程i)の後に返送することを特徴とする、請求項1から5までのいずれか1項記載の方法。
- 還元剤により被覆される篩下粒子が、篩下粒子に対して0.01〜5質量%の還元剤により被覆されていることを特徴とする、請求項1から6までのいずれか1項記載の方法。
- 無機粒子により被覆される篩下粒子が、篩下粒子に対して0.05〜2質量%の無機粒子により被覆されていることを特徴とする、請求項1から7までのいずれか1項記載の方法。
- 無機粒子が、熱分解法ケイ酸であるか、または燐酸の水不溶性の塩であることを特徴とする、請求項1から8までのいずれか1項記載の方法。
- モノマーa)が、部分的に中和されたアクリル酸であることを特徴とする、請求項1から9までのいずれか1項記載の方法。
- 吸水性ポリマー粒子が、少なくとも15g/gの遠心分離保持容量を有することを特徴とする、請求項1から10までのいずれか1項記載の方法。
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