JP5167263B2 - 中和度の低い、色安定性の吸水性ポリマー粒子の製造方法 - Google Patents
中和度の低い、色安定性の吸水性ポリマー粒子の製造方法 Download PDFInfo
- Publication number
- JP5167263B2 JP5167263B2 JP2009528696A JP2009528696A JP5167263B2 JP 5167263 B2 JP5167263 B2 JP 5167263B2 JP 2009528696 A JP2009528696 A JP 2009528696A JP 2009528696 A JP2009528696 A JP 2009528696A JP 5167263 B2 JP5167263 B2 JP 5167263B2
- Authority
- JP
- Japan
- Prior art keywords
- water
- polymer particles
- less
- polymer
- polymer gel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229920000642 polymer Polymers 0.000 title claims description 101
- 239000002245 particle Substances 0.000 title claims description 55
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 238000006386 neutralization reaction Methods 0.000 title description 14
- 239000000178 monomer Substances 0.000 claims description 42
- 238000001035 drying Methods 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000006116 polymerization reaction Methods 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 10
- 239000003431 cross linking reagent Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 5
- 229920003169 water-soluble polymer Polymers 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 239000004971 Cross linker Substances 0.000 claims description 3
- 230000007423 decrease Effects 0.000 claims description 3
- 125000000746 allylic group Chemical group 0.000 claims 1
- 239000000499 gel Substances 0.000 description 44
- 239000007789 gas Substances 0.000 description 30
- 239000000243 solution Substances 0.000 description 28
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 21
- 239000003570 air Substances 0.000 description 18
- 239000007864 aqueous solution Substances 0.000 description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 11
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 235000011187 glycerol Nutrition 0.000 description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 8
- 238000005119 centrifugation Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 238000010998 test method Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical class CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- -1 nicotinyl Chemical group 0.000 description 6
- 239000004745 nonwoven fabric Substances 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 5
- 229940048053 acrylate Drugs 0.000 description 5
- 125000004386 diacrylate group Chemical group 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000003472 neutralizing effect Effects 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- PUGOMSLRUSTQGV-UHFFFAOYSA-N 2,3-di(prop-2-enoyloxy)propyl prop-2-enoate Chemical compound C=CC(=O)OCC(OC(=O)C=C)COC(=O)C=C PUGOMSLRUSTQGV-UHFFFAOYSA-N 0.000 description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 3
- LXEKPEMOWBOYRF-UHFFFAOYSA-N [2-[(1-azaniumyl-1-imino-2-methylpropan-2-yl)diazenyl]-2-methylpropanimidoyl]azanium;dichloride Chemical compound Cl.Cl.NC(=N)C(C)(C)N=NC(C)(C)C(N)=N LXEKPEMOWBOYRF-UHFFFAOYSA-N 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 235000010323 ascorbic acid Nutrition 0.000 description 3
- 229960005070 ascorbic acid Drugs 0.000 description 3
- 239000011668 ascorbic acid Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229920005601 base polymer Polymers 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 150000002314 glycerols Chemical class 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 239000008107 starch Substances 0.000 description 3
- 235000019698 starch Nutrition 0.000 description 3
- 235000004835 α-tocopherol Nutrition 0.000 description 3
- 239000002076 α-tocopherol Substances 0.000 description 3
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 2
- LEJBBGNFPAFPKQ-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOC(=O)C=C LEJBBGNFPAFPKQ-UHFFFAOYSA-N 0.000 description 2
- 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
- IZXIZTKNFFYFOF-UHFFFAOYSA-N 2-Oxazolidone Chemical compound O=C1NCCO1 IZXIZTKNFFYFOF-UHFFFAOYSA-N 0.000 description 2
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 description 2
- BXAAQNFGSQKPDZ-UHFFFAOYSA-N 3-[1,2,2-tris(prop-2-enoxy)ethoxy]prop-1-ene Chemical compound C=CCOC(OCC=C)C(OCC=C)OCC=C BXAAQNFGSQKPDZ-UHFFFAOYSA-N 0.000 description 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 description 2
- ZMGMDXCADSRNCX-UHFFFAOYSA-N 5,6-dihydroxy-1,3-diazepan-2-one Chemical compound OC1CNC(=O)NCC1O ZMGMDXCADSRNCX-UHFFFAOYSA-N 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 2
- 229940087168 alpha tocopherol Drugs 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- GVJHHUAWPYXKBD-UHFFFAOYSA-N d-alpha-tocopherol Natural products OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 description 2
- 239000007863 gel particle Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 229940047670 sodium acrylate Drugs 0.000 description 2
- 229920000247 superabsorbent polymer Polymers 0.000 description 2
- 229960000984 tocofersolan Drugs 0.000 description 2
- 239000011732 tocopherol Substances 0.000 description 2
- 229930003799 tocopherol Natural products 0.000 description 2
- 235000010384 tocopherol Nutrition 0.000 description 2
- 229960001295 tocopherol Drugs 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- VPYJNCGUESNPMV-UHFFFAOYSA-N triallylamine Chemical compound C=CCN(CC=C)CC=C VPYJNCGUESNPMV-UHFFFAOYSA-N 0.000 description 2
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical class OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 2
- LGPAKRMZNPYPMG-UHFFFAOYSA-N (3-hydroxy-2-prop-2-enoyloxypropyl) prop-2-enoate Chemical class C=CC(=O)OC(CO)COC(=O)C=C LGPAKRMZNPYPMG-UHFFFAOYSA-N 0.000 description 1
- NQQRXZOPZBKCNF-NSCUHMNNSA-N (e)-but-2-enamide Chemical compound C\C=C\C(N)=O NQQRXZOPZBKCNF-NSCUHMNNSA-N 0.000 description 1
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 1
- TYMYJUHDFROXOO-UHFFFAOYSA-N 1,3-bis(prop-2-enoxy)-2,2-bis(prop-2-enoxymethyl)propane Chemical compound C=CCOCC(COCC=C)(COCC=C)COCC=C TYMYJUHDFROXOO-UHFFFAOYSA-N 0.000 description 1
- OYELEBBISJGNHJ-UHFFFAOYSA-N 1,3-oxazinan-2-one Chemical compound O=C1NCCCO1 OYELEBBISJGNHJ-UHFFFAOYSA-N 0.000 description 1
- HSOOIVBINKDISP-UHFFFAOYSA-N 1-(2-methylprop-2-enoyloxy)butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(CCC)OC(=O)C(C)=C HSOOIVBINKDISP-UHFFFAOYSA-N 0.000 description 1
- JHSWSKVODYPNDV-UHFFFAOYSA-N 2,2-bis(prop-2-enoxymethyl)propane-1,3-diol Chemical compound C=CCOCC(CO)(CO)COCC=C JHSWSKVODYPNDV-UHFFFAOYSA-N 0.000 description 1
- BWDHJINUKACSDS-UHFFFAOYSA-N 2,3-bis(prop-2-enoxy)propan-1-ol Chemical compound C=CCOC(CO)COCC=C BWDHJINUKACSDS-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- SJIXRGNQPBQWMK-UHFFFAOYSA-N 2-(diethylamino)ethyl 2-methylprop-2-enoate Chemical compound CCN(CC)CCOC(=O)C(C)=C SJIXRGNQPBQWMK-UHFFFAOYSA-N 0.000 description 1
- DPBJAVGHACCNRL-UHFFFAOYSA-N 2-(dimethylamino)ethyl prop-2-enoate Chemical compound CN(C)CCOC(=O)C=C DPBJAVGHACCNRL-UHFFFAOYSA-N 0.000 description 1
- TURITJIWSQEMDB-UHFFFAOYSA-N 2-methyl-n-[(2-methylprop-2-enoylamino)methyl]prop-2-enamide Chemical compound CC(=C)C(=O)NCNC(=O)C(C)=C TURITJIWSQEMDB-UHFFFAOYSA-N 0.000 description 1
- CARNFEUGBMWTON-UHFFFAOYSA-N 3-(2-prop-2-enoxyethoxy)prop-1-ene Chemical compound C=CCOCCOCC=C CARNFEUGBMWTON-UHFFFAOYSA-N 0.000 description 1
- XUYDVDHTTIQNMB-UHFFFAOYSA-N 3-(diethylamino)propyl prop-2-enoate Chemical compound CCN(CC)CCCOC(=O)C=C XUYDVDHTTIQNMB-UHFFFAOYSA-N 0.000 description 1
- UFQHFMGRRVQFNA-UHFFFAOYSA-N 3-(dimethylamino)propyl prop-2-enoate Chemical compound CN(C)CCCOC(=O)C=C UFQHFMGRRVQFNA-UHFFFAOYSA-N 0.000 description 1
- 125000004080 3-carboxypropanoyl group Chemical group O=C([*])C([H])([H])C([H])([H])C(O[H])=O 0.000 description 1
- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical compound C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 description 1
- ATVJXMYDOSMEPO-UHFFFAOYSA-N 3-prop-2-enoxyprop-1-ene Chemical compound C=CCOCC=C ATVJXMYDOSMEPO-UHFFFAOYSA-N 0.000 description 1
- JHWGFJBTMHEZME-UHFFFAOYSA-N 4-prop-2-enoyloxybutyl prop-2-enoate Chemical compound C=CC(=O)OCCCCOC(=O)C=C JHWGFJBTMHEZME-UHFFFAOYSA-N 0.000 description 1
- JAYRGGYYLFXBOK-UHFFFAOYSA-N 5-(2-hydroxyethyl)-2H-1,3-oxazol-2-id-4-one Chemical compound OCCC1C(N=[C-]O1)=O JAYRGGYYLFXBOK-UHFFFAOYSA-N 0.000 description 1
- XZIIFPSPUDAGJM-UHFFFAOYSA-N 6-chloro-2-n,2-n-diethylpyrimidine-2,4-diamine Chemical compound CCN(CC)C1=NC(N)=CC(Cl)=N1 XZIIFPSPUDAGJM-UHFFFAOYSA-N 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical class [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 1
- 229920002785 Croscarmellose sodium Polymers 0.000 description 1
- 244000007835 Cyamopsis tetragonoloba Species 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 238000006887 Ullmann reaction Methods 0.000 description 1
- NEGKNLJVKTUFJV-UHFFFAOYSA-N [1-(dimethylamino)-2,2-dimethylpropyl] 2-methylprop-2-enoate Chemical compound CN(C)C(C(C)(C)C)OC(=O)C(C)=C NEGKNLJVKTUFJV-UHFFFAOYSA-N 0.000 description 1
- KNUSQTXJWATMLJ-UHFFFAOYSA-N [1-(dimethylamino)-2,2-dimethylpropyl] prop-2-enoate Chemical compound CN(C)C(C(C)(C)C)OC(=O)C=C KNUSQTXJWATMLJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000007513 acids Chemical class 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
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 125000005370 alkoxysilyl group Chemical group 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000006286 aqueous extract Substances 0.000 description 1
- 239000012223 aqueous fraction Substances 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 125000003289 ascorbyl group Chemical group [H]O[C@@]([H])(C([H])([H])O*)[C@@]1([H])OC(=O)C(O*)=C1O* 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 125000002619 bicyclic group Chemical group 0.000 description 1
- ZPOLOEWJWXZUSP-WAYWQWQTSA-N bis(prop-2-enyl) (z)-but-2-enedioate Chemical compound C=CCOC(=O)\C=C/C(=O)OCC=C ZPOLOEWJWXZUSP-WAYWQWQTSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 125000004106 butoxy group Chemical group [*]OC([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000007942 carboxylates Chemical group 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 150000005676 cyclic carbonates Chemical class 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- BNKAXGCRDYRABM-UHFFFAOYSA-N ethenyl dihydrogen phosphate Chemical class OP(O)(=O)OC=C BNKAXGCRDYRABM-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 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
- 235000019426 modified starch Nutrition 0.000 description 1
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 description 1
- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- MENOBBYDZHOWLE-UHFFFAOYSA-N morpholine-2,3-dione Chemical compound O=C1NCCOC1=O MENOBBYDZHOWLE-UHFFFAOYSA-N 0.000 description 1
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- AHHWIHXENZJRFG-UHFFFAOYSA-N oxetane Chemical compound C1COC1 AHHWIHXENZJRFG-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920000962 poly(amidoamine) Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 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
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing 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
- 230000003134 recirculating effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 229940035044 sorbitan monolaurate Drugs 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000003628 tricarboxylic acids Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/06—Conditioning or physical treatment of the material to be shaped by drying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/10—Conditioning or physical treatment of the material to be shaped by grinding, e.g. by triturating; by sieving; by filtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/16—Auxiliary treatment of granules
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/06—Treatment of polymer solutions
- C08F6/10—Removal of volatile materials, e.g. solvents
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B17/00—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement
- F26B17/02—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement with movement performed by belts carrying the materials; with movement performed by belts or elements attached to endless belts or chains propelling the materials over stationary surfaces
- F26B17/04—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement with movement performed by belts carrying the materials; with movement performed by belts or elements attached to endless belts or chains propelling the materials over stationary surfaces the belts being all horizontal or slightly inclined
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/06—Controlling, e.g. regulating, parameters of gas supply
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
- C08F222/103—Esters of polyhydric alcohols or polyhydric phenols of trialcohols, e.g. trimethylolpropane tri(meth)acrylate
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Materials Engineering (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Epidemiology (AREA)
- Hematology (AREA)
- Dispersion Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Absorbent Articles And Supports Therefor (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Description
a)55mol%未満中和されている、酸基を有する少なくとも1のエチレン不飽和モノマー、
b)少なくとも1の架橋剤、
c)選択的に、a)で言及したモノマーと共重合可能な1またはそれ以上のエチレン不飽和モノマー、および/またはアリル不飽和モノマー、および
d)選択的に1またはそれ以上の水溶性ポリマー
を含むモノマー溶液を重合させることによる吸水性ポリマー粒子の製造方法(この際、該モノマー溶液を重合させ、かつ得られるポリマーゲルを加熱されたガス流によって乾燥させる)によって解決され、前記乾燥を少なくとも2の温度帯域で行い、この際少なくとも2の温度帯域のガス入口温度は、TnがTn+aより大きいという条件を満たし[式中、指数nとaはその都度0より大きい整数である]、ならびに温度帯域Tnにおけるガス入口温度が175℃未満であり、かつ温度帯域TnとTn+aのガス入口温度の温度差が10℃超であることを特徴とする。
によって計算することができる。
バッチ法での、または管式反応器でのゲル重合、および引き続いた粉砕機、押出機、または混練機での粉砕(EP445619A2、DE19846413A1)、
例えば対向撹拌軸による連続的粉砕による、混練機での重合(WO2001/38402A1)、
ベルト上での重合、および引き続いた粉砕機、押出機、または混練機での粉砕(DE3825366A1、US6241928)、
既に比較的狭いゲル粒径分布のパール重合体が生じるエマルション重合(EP457660A1)
によって得ることができる。
i)重合導入され、55mol%中和されている、酸基を有する少なくとも1のエチレン不飽和モノマー、
ii)重合導入された少なくとも1の架橋剤
iii)選択的に、i)で言及したモノマーと共重合可能な、1またはそれ以上の重合導入されたエチレン不飽和モノマー、および/またはアリル不飽和モノマー
iv)選択的に、i)で言及したモノマーを少なくとも部分的にグラフト重合させてある1またはそれ以上の水溶性ポリマー、
を含む吸水性ポリマー粒子であって、この際このポリマー粒子は15質量%未満の水含分、および少なくとも60のHunter60値を有し、ならびにこのHunter60値が70℃で、かつ相対空気湿度90%で一週間貯蔵の間、初期値の10%未満しか減少しない。
特に言及しない限り、測定は23±2℃の周囲温度、かつ相対空気湿度50±10%で行う。吸水性ポリマーは測定前、良好に完全混合する。
吸水性ポリマー粒子の水含分は、EDANA(Europian Disposables and Nonwovens Association)推奨試験法No.430.2−02""Moisture content"に従って測定する。
吸水性ポリマー粒子の遠心分離時保水力はEDANA(Europian Disposables and Nonwovens Association)推奨試験法No.441.2−02"Centrifuge retention capacity"に従って測定する。
色の測定のために、Hunterlab LabScan測色計(LS−5100型)を使用した。
実施例1〜7
37.3質量%のナトリウムアクリラート水溶液1235.1g、アクリル酸529.31g、水1182.77g、尿素1.32g、3回エトキシ化されたグリセリントリアクリラート1.32gを秤量し、5,000mlのガラスビーカーに入れた。中和度は40mol%であった。その後、この溶液を金属フリットを用いて100l/hの窒素で30分間、不活性化した。さらに、溶液を撹拌した(〜100rpm)。撹拌の間、モノマー溶液を10℃に冷却した。冷却槽は開始剤添加の直前に取り除いた。引き続き、3質量%の2,2’−アゾビス−(2−アミジノプロパン)ジヒドロクロリド水溶液10.0g、3質量%の過硫酸ナトリウム水溶液30.0g、3質量%の過酸化水素水溶液7.0g、および1質量%のアスコルビン酸水溶液4.5gを添加した。反応開始後、撹拌器具と金属フリットを反応溶液から取り除いた。30分間の反応時間後、ゲルを取り出し、有孔板を備える粉砕機で粉砕した(有孔直径6mm)。
37.3質量%のナトリウムアクリラート水溶液2478.79g、アクリル酸275.41g、水192.91g、3回エトキシ化されたグリセリントリアクリラート4.13gを秤量し、5,000mlのガラスビーカーに入れた。中和度は72mol%だった。その後、この溶液を金属フリットを用いて100l/hの窒素で30分間、不活性化した。さらに、溶液を撹拌した(〜100rpm)。撹拌の間にモノマー溶液を10℃に冷却した。冷却槽は、開始剤添加の直前に取り除いた。引き続き、3質量%の2,2’−アゾビス−(2−アミジノプロパン)ジヒドロクロリド10.0g、3質量%の過硫酸ナトリウム水溶液30.0g、3質量%の過酸化水素水溶液7.0g、および1質量%のアスコルビン酸水溶液4.5gを添加した。反応開始後、撹拌器具と金属フリットを反応溶液から取り除いた。30分間の反応時間後、ゲルを取り出し、そして有孔板を備える粉砕機を用いて粉砕した(有孔直径6mm)。
アクリル酸117.62g、水223.05g、および50質量%の水酸化ナトリウム水溶液52.28gを、温度が35℃超に上がらないように混合した。引き続き尿素0.18g、および3回エトキシ化されたグリセリントリアクリラート0.18gを秤量し、600mlのガラスビーカーに入れた。中和度は40mol%だった。この溶液を金属フリットを用いて100l/hの窒素で30分間、不活性化した。この溶液をさらに撹拌した(〜100rpm)。撹拌の間にモノマー溶液を10℃に冷却した。冷却槽は、開始剤添加の直前に取り除いた。引き続き、モノラウリン酸ソルビタン0.16g、3質量%の2,2’−アゾビス−(2−アミジノプロパン)ジヒドロクロリド水溶液1.33g、3質量%の過硫酸ナトリウム水溶液4.0g、3質量%の過酸化水素水溶液0.93g、および1質量%のアスコルビン酸水溶液0.6gを添加した。反応開始後、撹拌器具と金属フリットを溶液から取り除いた。30分間の反応時間後、ゲルを取り出し、有孔板を備える粉砕機を用いて粉砕した(有孔直径6mm)。
Claims (16)
- a) 55mol%未満中和されている、酸基を有する少なくとも1のエチレン不飽和モノマー
b) 少なくとも1の架橋剤
c) 選択的に、a)で言及したモノマーと共重合可能な1またはそれ以上のエチレン不飽和モノマー、および/またはアリル不飽和モノマー、および
d)選択的に、1またはそれ以上の水溶性ポリマー
を含むモノマー溶液の重合による(この際、前記モノマー溶液を重合させ、かつ得られたポリマーゲルを加熱されたガス流により乾燥させる)吸水性ポリマー粒子の製造方法において、
前記乾燥を、異なったガス入口温度を有する少なくとも2の温度帯域で行い、この際少なくとも2の温度帯域における異なったガス入口温度は、T n およびT n+a [式中、記号nとaはそれぞれ0より大きい整数である]により定義され、この際、ガス入口温度は、T nがTn+aより大きいという条件を満たし、ならびにガス入口温度T n は175℃未満であり、かつガス入口温度T n とT n+a との温度差は、10℃超であり、乾燥機におけるポリマーゲルの滞留時間が、10〜120分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。 - ポリマーゲルの水含分が、ガス入口温度T n を有する温度帯域に入る際に少なくとも30質量%であることを特徴とする、請求項1に記載の方法。
- 前記ポリマーゲルが1の界面活性剤、無機粉末、または有機粉末を含むものであることを特徴とする、請求項1または2に記載の方法。
- 乾燥させる前記ポリマーゲルの層厚が10cm未満であることを特徴とする、請求項1から3までのいずれか1項に記載の方法。
- ポリマーゲル層を貫流させるガス流の速度が0.5〜5m/秒であることを特徴とする、請求項1から4までのいずれか1項に記載の方法。
- 乾燥機におけるポリマーゲルの滞留時間が、15〜80分であることを特徴とする、請求項1から5までのいずれか1項に記載の方法。
- 乾燥機におけるポリマーゲルの滞留時間が、20〜60分であることを特徴とする、請求項1から6までのいずれか1項に記載の方法。
- 前記乾燥の際の圧力が大気圧より低いことを特徴とする、請求項1から7までのいずれか1項に記載の方法。
- 前記乾燥をベルト式乾燥機で行うことを特徴とする、請求項1から8までのいずれか1項に記載の方法。
- 前記ポリマーゲルが乾燥後に2〜10質量%の水含分を有することを特徴とする、請求項1から9までのいずれか1項に記載の方法。
- i)55mol%未満中和されている、重合導入された、酸基を有する少なくとも1のエチレン不飽和モノマー、
ii)重合導入された少なくとも1の架橋剤、
iii)選択的に、i)で言及したモノマーと共重合可能な、1またはそれ以上の重合導入されたエチレン不飽和モノマー、および/またはアリル不飽和モノマー、
iv)選択的に、i)で言及したモノマーを少なくとも部分的にグラフトさせてある、1またはそれ以上の水溶性ポリマー
を含む吸水性ポリマー粒子であって、
前記ポリマー粒子が10質量%未満の水含分、および少なくとも60のHunter60値を有し、ならびに70℃で、かつ相対空気湿度90%で一週間貯蔵する間に、Hunter60値が初期値の15%未満しか減少しない、吸水性ポリマー粒子。 - 前記ポリマー粒子が10未満のb*値を有し、ならびにこのb*値が70℃で、かつ相対空気湿度90%で一週間貯蔵する間に初期値の75%未満しか上昇しないことを特徴とする、請求項11に記載のポリマー粒子。
- 150μmより小さい直径を有する粒子の割合が、10質量%未満であることを特徴とする、請求項11または12に記載のポリマー粒子。
- 前記ポリマー粒子が、少なくとも20g/gの遠心分離時保水力(CRC)を有することを特徴とする、請求項11から13までのいずれか1項に記載のポリマー粒子。
- 前記ポリマー粒子が、300〜600μmの範囲の平均粒子直径を有することを特徴とする、請求項11から14までのいずれか1項に記載のポリマー粒子。
- 請求項11から15までのいずれか1項に記載の吸水性ポリマー粒子を含む、衛生用品。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP06120881 | 2006-09-19 | ||
EP06120881.5 | 2006-09-19 | ||
PCT/EP2007/059759 WO2008034786A1 (de) | 2006-09-19 | 2007-09-17 | Verfahren zur herstellung farbstabiler wasserabsorbierender polymerpartikel mit niedrigen neutralisationsgrad |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2010503758A JP2010503758A (ja) | 2010-02-04 |
JP5167263B2 true JP5167263B2 (ja) | 2013-03-21 |
Family
ID=38859045
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2009528696A Active JP5167263B2 (ja) | 2006-09-19 | 2007-09-17 | 中和度の低い、色安定性の吸水性ポリマー粒子の製造方法 |
Country Status (5)
Country | Link |
---|---|
US (1) | US7960490B2 (ja) |
EP (1) | EP2074153B1 (ja) |
JP (1) | JP5167263B2 (ja) |
CN (1) | CN101516925B (ja) |
WO (1) | WO2008034786A1 (ja) |
Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20100062932A1 (en) * | 2007-02-06 | 2010-03-11 | Basf Se A German Corporation | Method for Producing Water-Absorbent Polymer Particles by the Polymerization of Droplets of a Monomer Solution |
EP2424900B1 (de) * | 2009-04-30 | 2013-04-03 | Basf Se | Verfahren zur abtrennung metallischer verunreinigungen |
JP5616347B2 (ja) | 2009-08-28 | 2014-10-29 | 株式会社日本触媒 | 吸水性樹脂の製造方法 |
US8623994B2 (en) | 2010-01-20 | 2014-01-07 | Nippon Shokubai, Co., Ltd. | Method for producing water absorbent resin |
WO2011090130A1 (ja) | 2010-01-20 | 2011-07-28 | 株式会社日本触媒 | 吸水性樹脂の製造方法 |
WO2011099586A1 (ja) | 2010-02-10 | 2011-08-18 | 株式会社日本触媒 | 吸水性樹脂粉末の製造方法 |
JP5818821B2 (ja) * | 2010-02-24 | 2015-11-18 | ビーエーエスエフ ソシエタス・ヨーロピアBasf Se | 吸水性ポリマー粒子の製造法 |
US9272068B2 (en) | 2010-03-12 | 2016-03-01 | Nippon Shokubai Co., Ltd. | Process for producing water-absorbing resin |
WO2011117263A1 (en) * | 2010-03-24 | 2011-09-29 | Basf Se | A process for producing water-absorbent polymer particles by polymerizing droplets of a monomer solution |
JP5616437B2 (ja) | 2010-04-27 | 2014-10-29 | 株式会社日本触媒 | ポリアクリル酸(塩)系吸水性樹脂粉末の製造方法 |
EP2615120B2 (en) * | 2012-01-12 | 2022-12-21 | Evonik Superabsorber GmbH | Process for the continuous preparation of water-absorbent polymers |
WO2015007749A1 (en) * | 2013-07-17 | 2015-01-22 | Bp Exploration Operating Company Limited | Oil recovery method |
JP7128980B1 (ja) | 2022-03-30 | 2022-08-31 | Sdpグローバル株式会社 | 吸水性樹脂組成物の製造方法、吸水性樹脂組成物、これを用いた吸収体、及び吸収性物品 |
Family Cites Families (24)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3609545A1 (de) * | 1986-03-21 | 1987-09-24 | Basf Ag | Verfahren zur diskontinuierlichen herstellung von vernetzten, feinteiligen polymerisaten |
EP0289338B2 (en) * | 1987-04-30 | 2000-03-22 | Nippon Shokubai Co., Ltd. | Hydrophilic polymer and method for production |
JP2555159B2 (ja) * | 1987-08-10 | 1996-11-20 | 株式会社日本触媒 | 吸水性樹脂の製造方法 |
JP2700531B2 (ja) * | 1994-09-05 | 1998-01-21 | 三洋化成工業株式会社 | 含水ゲル状重合体の連続的乾燥方法 |
US5668252A (en) * | 1995-09-11 | 1997-09-16 | Nippon Shokubai Co., Ltd. | Drying process of viscous solution containing (meth)acrylic acid-based polymer |
DE19756633A1 (de) * | 1997-12-19 | 1999-06-24 | Hoechst Ag | Verfahren zur unterkritischen Trocknung von Lyogelen zu Aerogelen |
US6444744B1 (en) | 1998-03-11 | 2002-09-03 | Nippon Shokubai Co., Ltd. | Hydrophilic resin, absorbent article, and acrylic acid for polymerization |
US6207796B1 (en) * | 1998-11-18 | 2001-03-27 | Nippon Shokubai Co., Ltd. | Production process for hydrophilic polymer |
DE60014054T2 (de) | 1999-03-12 | 2005-02-03 | Basf Ag | Farbstabile superabsorbierende polymerzusammensetzung |
EP1457519A1 (en) | 1999-03-12 | 2004-09-15 | Basf Aktiengesellschaft | Color-stable superabsorbent polymer composition |
JP4717979B2 (ja) * | 2000-02-04 | 2011-07-06 | 三洋化成工業株式会社 | 吸水性樹脂の製造法 |
US6927268B2 (en) | 2000-06-21 | 2005-08-09 | Nippon Shokubai Co., Ltd. | Production process for water-absorbent resin |
ES2271287T3 (es) | 2001-06-28 | 2007-04-16 | Basf Aktiengesellschaft | Hidrogeles acidos altamente capaces de hincharse. |
KR100549717B1 (ko) | 2001-12-19 | 2006-02-07 | 니폰 쇼쿠바이 컴파니 리미티드 | 아크릴산 조성물 및 그의 제조방법, 및 그 아크릴산조성물을 사용하는 수흡수성 수지의 제조방법, 및수흡수성 수지 |
TW200500046A (en) | 2003-03-26 | 2005-01-01 | Basf Ag | Color-stable superabsorbent polymer composition |
US7528291B2 (en) | 2003-03-26 | 2009-05-05 | Basf Aktiengesellschaft | Color-stable superabsorbent polymer composition |
JP4500134B2 (ja) * | 2003-09-02 | 2010-07-14 | 株式会社日本触媒 | 粒子状吸水性樹脂組成物 |
EP1512417B1 (en) * | 2003-09-02 | 2013-06-19 | Nippon Shokubai Co., Ltd. | Particulate water-absorbent resin composition |
DE102004019264B4 (de) * | 2004-04-21 | 2008-04-10 | Stockhausen Gmbh | Verfahren zur Herstellung eines absorbierenden Polymers mittels Spreittrocknung |
JP5014607B2 (ja) * | 2004-09-24 | 2012-08-29 | 株式会社日本触媒 | 吸水性樹脂を主成分とする粒子状吸水剤 |
DE102005014291A1 (de) * | 2005-03-24 | 2006-09-28 | Basf Ag | Verfahren zur Herstellung wasserabsorbierender Polymere |
TWI353360B (en) | 2005-04-07 | 2011-12-01 | Nippon Catalytic Chem Ind | Production process of polyacrylic acid (salt) wate |
US8481664B2 (en) | 2005-04-12 | 2013-07-09 | Nippon Shokubai Co., Ltd. | Particulate water absorbing agent including polyacrylic acid (polyacrylate) based water absorbing resin as a principal component, method for production thereof, water-absorbent core and absorbing article in which the particulate water absorbing agent is used |
CN101501131B (zh) * | 2006-08-31 | 2012-06-13 | 株式会社日本触媒 | 颗粒吸水剂及其制备方法 |
-
2007
- 2007-09-17 JP JP2009528696A patent/JP5167263B2/ja active Active
- 2007-09-17 EP EP07820241.3A patent/EP2074153B1/de active Active
- 2007-09-17 WO PCT/EP2007/059759 patent/WO2008034786A1/de active Application Filing
- 2007-09-17 US US12/438,217 patent/US7960490B2/en active Active
- 2007-09-17 CN CN200780034597XA patent/CN101516925B/zh active Active
Also Published As
Publication number | Publication date |
---|---|
JP2010503758A (ja) | 2010-02-04 |
US20100001233A1 (en) | 2010-01-07 |
US7960490B2 (en) | 2011-06-14 |
CN101516925B (zh) | 2011-06-15 |
WO2008034786A1 (de) | 2008-03-27 |
EP2074153B1 (de) | 2015-09-09 |
CN101516925A (zh) | 2009-08-26 |
EP2074153A1 (de) | 2009-07-01 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5167263B2 (ja) | 中和度の低い、色安定性の吸水性ポリマー粒子の製造方法 | |
US9327270B2 (en) | Method for the continuous production of water absorbent polymer particles | |
US8080620B2 (en) | Process for continuously producing water-absorbing polymer particles | |
JP5322997B2 (ja) | 架橋した微粒子状のゲル状ポリマーの製造方法 | |
JP5992134B2 (ja) | 吸水性ポリマーの製造方法 | |
JP5610669B2 (ja) | 噴霧重合によりポリマーを製造する方法 | |
US8410222B2 (en) | Method for producing water-absorbing polymer particles | |
JP5610689B2 (ja) | 重合法 | |
US20110015362A1 (en) | Method for Manufacturing Water-Absorbing Polymer Particles with a Low Centrifuge Retention Capacity | |
US20080227933A1 (en) | Method For Producing Water-Absorbing Polymers | |
US20080161522A1 (en) | Production of Water-Absorbing Polymeric Particles | |
KR102563402B1 (ko) | 고흡수성 중합체 입자 제조 방법 | |
US20130058837A1 (en) | Process for producing water-absorbing polymer particles | |
US9833769B2 (en) | Process for producing water-absorbing polymer particles with high free swell rate | |
JP2011506695A (ja) | 吸水性ポリマー粒子の製造方法 | |
CN107406553B (zh) | 通过悬浮聚合制备吸水性聚合物颗粒的方法 | |
US9248429B2 (en) | Process for producing water-absorbing polymer particles in a polymerization reactor with at least two axially parallel rotating shafts | |
US20110112252A1 (en) | Method for Post-Crosslinking of the Surface of Water-Absorbing Polymer Particles | |
US10835634B2 (en) | Method for the agglomeration of superabsorber particles | |
EP2890411B1 (en) | Process for producing water-absorbing polymer particles | |
CN107257809B (zh) | 通过悬浮聚合制备吸水性聚合物颗粒的方法 | |
US9751958B2 (en) | Use of heating steam condensate for producing water-absorbent polymer particles | |
US8507645B2 (en) | Process for continuously producing water-absorbing polymer particles |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20100914 |
|
RD04 | Notification of resignation of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7424 Effective date: 20101228 |
|
A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20120803 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20120808 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20121025 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20121122 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20121221 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20151228 Year of fee payment: 3 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 5167263 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |