KR100760588B1 - 수용성 중합체의 제조방법 - Google Patents
수용성 중합체의 제조방법 Download PDFInfo
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- KR100760588B1 KR100760588B1 KR1020027013829A KR20027013829A KR100760588B1 KR 100760588 B1 KR100760588 B1 KR 100760588B1 KR 1020027013829 A KR1020027013829 A KR 1020027013829A KR 20027013829 A KR20027013829 A KR 20027013829A KR 100760588 B1 KR100760588 B1 KR 100760588B1
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- Prior art keywords
- water
- soluble polymer
- light irradiation
- light
- monomer
- Prior art date
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- 229920003169 water-soluble polymer Polymers 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title abstract description 36
- 239000000178 monomer Substances 0.000 claims abstract description 129
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 49
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 49
- 239000007864 aqueous solution Substances 0.000 claims abstract description 46
- -1 azo compound Chemical class 0.000 claims abstract description 40
- 239000003999 initiator Substances 0.000 claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 claims abstract description 19
- 229920000642 polymer Polymers 0.000 claims description 32
- 150000003839 salts Chemical group 0.000 claims description 30
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 17
- 230000001678 irradiating effect Effects 0.000 claims description 13
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 8
- 125000002091 cationic group Chemical group 0.000 claims description 4
- 230000001186 cumulative effect Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 20
- 238000006116 polymerization reaction Methods 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 19
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 description 7
- 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 7
- ISAOCJYIOMOJEB-UHFFFAOYSA-N desyl alcohol Natural products C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 7
- 239000000017 hydrogel Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 125000002348 vinylic group Chemical group 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 244000028419 Styrax benzoin Species 0.000 description 5
- 235000000126 Styrax benzoin Nutrition 0.000 description 5
- 235000008411 Sumatra benzointree Nutrition 0.000 description 5
- 229960002130 benzoin Drugs 0.000 description 5
- 235000019382 gum benzoic Nutrition 0.000 description 5
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000003607 modifier Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- KMNCBSZOIQAUFX-UHFFFAOYSA-N 2-ethoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OCC)C(=O)C1=CC=CC=C1 KMNCBSZOIQAUFX-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
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 239000003623 enhancer Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- VFXXTYGQYWRHJP-UHFFFAOYSA-N 4,4'-azobis(4-cyanopentanoic acid) Chemical compound OC(=O)CCC(C)(C#N)N=NC(C)(CCC(O)=O)C#N VFXXTYGQYWRHJP-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 2
- 239000012965 benzophenone Substances 0.000 description 2
- LWMFAFLIWMPZSX-UHFFFAOYSA-N bis[2-(4,5-dihydro-1h-imidazol-2-yl)propan-2-yl]diazene Chemical compound N=1CCNC=1C(C)(C)N=NC(C)(C)C1=NCCN1 LWMFAFLIWMPZSX-UHFFFAOYSA-N 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 229940050176 methyl chloride Drugs 0.000 description 2
- QYZFTMMPKCOTAN-UHFFFAOYSA-N n-[2-(2-hydroxyethylamino)ethyl]-2-[[1-[2-(2-hydroxyethylamino)ethylamino]-2-methyl-1-oxopropan-2-yl]diazenyl]-2-methylpropanamide Chemical compound OCCNCCNC(=O)C(C)(C)N=NC(C)(C)C(=O)NCCNCCO QYZFTMMPKCOTAN-UHFFFAOYSA-N 0.000 description 2
- 239000000123 paper Substances 0.000 description 2
- 239000003504 photosensitizing agent Substances 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- AVTLBBWTUPQRAY-UHFFFAOYSA-N 2-(2-cyanobutan-2-yldiazenyl)-2-methylbutanenitrile Chemical compound CCC(C)(C#N)N=NC(C)(CC)C#N AVTLBBWTUPQRAY-UHFFFAOYSA-N 0.000 description 1
- DPBJAVGHACCNRL-UHFFFAOYSA-N 2-(dimethylamino)ethyl prop-2-enoate Chemical class CN(C)CCOC(=O)C=C DPBJAVGHACCNRL-UHFFFAOYSA-N 0.000 description 1
- WYGWHHGCAGTUCH-UHFFFAOYSA-N 2-[(2-cyano-4-methylpentan-2-yl)diazenyl]-2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)C WYGWHHGCAGTUCH-UHFFFAOYSA-N 0.000 description 1
- FLKBKUFGKQPPRY-UHFFFAOYSA-N 2-[2-[2-[2-[1-(2-hydroxyethyl)-4,5-dihydroimidazol-2-yl]propan-2-yldiazenyl]propan-2-yl]-4,5-dihydroimidazol-1-yl]ethanol;dihydrochloride Chemical compound Cl.Cl.N=1CCN(CCO)C=1C(C)(C)N=NC(C)(C)C1=NCCN1CCO FLKBKUFGKQPPRY-UHFFFAOYSA-N 0.000 description 1
- AUZRCMMVHXRSGT-UHFFFAOYSA-N 2-methylpropane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CC(C)CS(O)(=O)=O AUZRCMMVHXRSGT-UHFFFAOYSA-N 0.000 description 1
- MNULHGQAROOBFB-UHFFFAOYSA-N 3-[(1-amino-2-methylpropylidene)amino]propanoic acid Chemical compound CC(C)C(N)=NCCC(O)=O MNULHGQAROOBFB-UHFFFAOYSA-N 0.000 description 1
- NMZSJIQGMAGSSO-UHFFFAOYSA-N 3-[[1-amino-2-[[1-amino-1-(2-carboxyethylimino)-2-methylpropan-2-yl]diazenyl]-2-methylpropylidene]amino]propanoic acid Chemical compound OC(=O)CCNC(=N)C(C)(C)N=NC(C)(C)C(=N)NCCC(O)=O NMZSJIQGMAGSSO-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 1
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- KYIKRXIYLAGAKQ-UHFFFAOYSA-N abcn Chemical compound C1CCCCC1(C#N)N=NC1(C#N)CCCCC1 KYIKRXIYLAGAKQ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000003926 acrylamides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229940024874 benzophenone Drugs 0.000 description 1
- PASDCCFISLVPSO-UHFFFAOYSA-N benzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1 PASDCCFISLVPSO-UHFFFAOYSA-N 0.000 description 1
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 1
- 229940073608 benzyl chloride Drugs 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- NBXSIUSZCHNKCZ-UHFFFAOYSA-N bis[2-(1,4,5,6-tetrahydropyrimidin-2-yl)propan-2-yl]diazene;dihydrochloride Chemical compound Cl.Cl.N=1CCCNC=1C(C)(C)N=NC(C)(C)C1=NCCCN1 NBXSIUSZCHNKCZ-UHFFFAOYSA-N 0.000 description 1
- SFBXYJXNDOJHLL-UHFFFAOYSA-N bis[2-(4,5-dihydro-1h-imidazol-2-yl)propan-2-yl]diazene;sulfo hydrogen sulfate Chemical compound OS(=O)(=O)OS(O)(=O)=O.N=1CCNC=1C(C)(C)N=NC(C)(C)C1=NCCN1 SFBXYJXNDOJHLL-UHFFFAOYSA-N 0.000 description 1
- PZXSLFQJOZPCJG-UHFFFAOYSA-N bis[2-(5-methyl-4,5-dihydro-1h-imidazol-2-yl)propan-2-yl]diazene;dihydrochloride Chemical compound Cl.Cl.N1C(C)CN=C1C(C)(C)N=NC(C)(C)C1=NCC(C)N1 PZXSLFQJOZPCJG-UHFFFAOYSA-N 0.000 description 1
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 description 1
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- WVFLGSMUPMVNTQ-UHFFFAOYSA-N n-(2-hydroxyethyl)-2-[[1-(2-hydroxyethylamino)-2-methyl-1-oxopropan-2-yl]diazenyl]-2-methylpropanamide Chemical compound OCCNC(=O)C(C)(C)N=NC(C)(C)C(=O)NCCO WVFLGSMUPMVNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- QLNJFJADRCOGBJ-UHFFFAOYSA-N propionamide Chemical compound CCC(N)=O QLNJFJADRCOGBJ-UHFFFAOYSA-N 0.000 description 1
- 229940080818 propionamide Drugs 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- C08F2/00—Processes of polymerisation
- C08F2/04—Polymerisation in solution
- C08F2/10—Aqueous solvent
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Abstract
Description
실시예 1 | 실시예 2 | 실시예 3 | 실시예 4 | ||
광중합 조건 광중합 개시제1) | a와 b | a와 b | a와 b | a | |
a의 10시간 반감기 온도 (℃) | 56 | 56 | 56 | 56 | |
제1 광조사단계: 조사강도(W/㎡) | 4.2 | 4.2 | 4.2 | 4.2 | |
조사시간(분) | 20 | 20 | 20 | 20 | |
제2 광조사단계: 조사강도(W/㎡) | 300 | 300 | 60 | 60 | |
조사시간(분) | 30 | 6 | 30 | 30 | |
적산광량(J/㎡) | 540,000 | 108,000 | 108,000 | 108,000 | |
중합체 온도 피크온도 도달시간(분) | 10 | 10 | 10 | 10 | |
피크온도(℃) | 95 | 95 | 95 | 95 | |
제2 광조사단계에서의 중합체온도(℃) | 90→75 | 90→86 | 90→75 | 90→75 | |
수용성 중합체 0.5% 염점도(mPaㆍs) | 132 | 133 | 127 | 124 | |
불용해분(ml) | 없음 | 없음 | 없음 | 없음 | |
미반응 단량체 함유량(중량%) | 0.05 | 0.09 | 0.09 | 0.10 |
비교예 1 | 비교예 2 | 비교예 3 | 비교예 4 | |
광중합 조건 광중합 개시제1) | a와 b | a와 b | b | c |
a의 10시간 반감기 분해 온도 (℃) | 56 | 56 | - | - |
제1 광조사단계: 조사강도(W/㎡) | 4.2 | 4.2 | 4.2 | 4.2 |
조사시간(분) | 20 | 20 | 20 | 20 |
제2 광조사단계: 조사강도(W/㎡) | - | 50 | 60 | 60 |
조사시간(분) | - | 5 | 30 | 30 |
적산광량(J/㎡) | - | 15,000 | 108,000 | 108,000 |
중합체 온도 피크온도 도달시간(분) | 10 | 10 | 9 | 9 |
피크온도(℃) | 95 | 95 | 95 | 95 |
제2 광조사단계에서의 중합체온도(℃) | - | 90→87 | 90→75 | 90→75 |
수용성 중합체 0.5% 염점도(mPaㆍs) | 128 | 124 | 138 | 62 |
불용해분(ml) | 없음 | 없음 | 없음 | 80 |
미반응 단량체 함유량(중량%) | 0.61 | 0.25 | 0.21 | 0.35 |
Claims (5)
- 광중합 개시제를 함유하는 비닐계 단량체의 수용액에 빛을 조사하는 단계를 포함하는 수용성 중합체의 제조방법으로서, 광중합 개시제로서 10시간 반감기 온도가 90℃ 이하인 아조화합물을 사용하고, 0.5∼7W/㎡의 조사강도로 광조사하는 제1 광조사단계, 및 1단계보다 높은 조사강도로, 또한 70,000J/㎡ 이상의 적산광량으로 광조사하는 1회 이상의 제2 광조사단계를 포함하는 것을 특징으로 하는 수용성 중합체의 제조방법.
- 제1항에 있어서, 상기 얻어진 중합체의 중앙부의 온도가 피크온도에 도달한 후, 제1 광조사단계를 종료하고, 제2 광조사단계로 이행하는 것을 특징으로 하는 수용성 중합체의 제조방법.
- 제1항 또는 제2항에 있어서, 상기 중합체의 온도를 상기 아조화합물의 10시간 반감기 온도보다 높게 유지하면서, 1회 이상의 제2 광조사단계를 행하는 것을 특징으로 하는 수용성 중합체의 제조방법.
- 제1항 또는 제2항에 있어서, 상기 비닐계 단량체는 아크릴아미드 단독이거나, 또는 아크릴아미드와 다른 공중합성 비닐계 단량체의 혼합물이고, 이 혼합물은 상기 아크릴아미드를 10몰% 이상 함유하는 것을 특징으로 하는 수용성 중합체의 제조방법.
- 제4항에 있어서, 상기 아크릴아미드와 다른 공중합성 비닐계 단량체의 혼합물은 아크릴아미드와 디메틸아미노에틸(메타)아크릴레이트의 제4급염 및 제3급염 중 1종 이상과의 양이온성 단량체 혼합물이고, 이 혼합물은 상기 염을 5몰% 이상 함유하는 것을 특징으로 하는 수용성 중합체의 제조방법.
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KR20160041994A (ko) * | 2013-09-10 | 2016-04-18 | 미쯔비시 레이온 가부시끼가이샤 | 분말상 n-비닐카르복실산아미드 중합체 조성물 및 폴리비닐아민 수용액의 제조 방법 |
CN107151289B (zh) * | 2017-05-26 | 2019-05-07 | 南京工程学院 | 一种光引发体系制备阳离子聚丙烯酰胺的方法 |
CN110606915B (zh) * | 2019-09-20 | 2021-01-29 | 江苏富淼科技股份有限公司 | 一种紫外光引发制备固体型水溶性高分子聚合物的方法 |
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US4024040A (en) * | 1974-02-26 | 1977-05-17 | Hercules Incorporated | Polymerization of unsaturated monomers with radiation in the presence of salts |
US4018953A (en) | 1976-08-12 | 1977-04-19 | Xerox Corporation | Coating method |
JPS6031323B2 (ja) * | 1980-03-28 | 1985-07-22 | 日本原子力研究所 | 水溶性ビニルポリマ−の製造方法 |
JPS5834213B2 (ja) | 1980-07-09 | 1983-07-25 | 三菱製鋼株式会社 | 据込み頭部を持つ製品の成型装置 |
FR2489336B1 (fr) | 1980-09-04 | 1985-09-13 | Rhone Poulenc Spec Chim | Procede de preparation de polymeres ou copolymeres hydrosolubles a poids moleculaire eleve et a faible teneur en monomere(s) residuel(s), a partir de monomeres olefiniquement insatures |
JPS62235305A (ja) * | 1986-04-04 | 1987-10-15 | Dai Ichi Kogyo Seiyaku Co Ltd | 高分子量アクリル系重合体の製法 |
JPH0710896B2 (ja) * | 1987-04-30 | 1995-02-08 | 第一工業製薬株式会社 | 高分子量カチオン性アクリル系重合体の製造方法 |
JPS63295604A (ja) | 1987-05-28 | 1988-12-02 | Mitsubishi Rayon Co Ltd | 水溶性重合体の製造法 |
JPS63309501A (ja) | 1987-06-11 | 1988-12-16 | Mitsubishi Rayon Co Ltd | 水溶性重合体の製造方法 |
JPH0457682A (ja) | 1990-06-25 | 1992-02-25 | Kaisei Kogyo Kk | 折畳式作業台 |
JPH0710895A (ja) | 1993-06-23 | 1995-01-13 | Sumitomo Pharmaceut Co Ltd | グリコシル化合物の製造方法 |
JP3621552B2 (ja) | 1997-04-03 | 2005-02-16 | ダイヤニトリックス株式会社 | 水溶性重合体の製造方法 |
JP3621554B2 (ja) | 1997-04-25 | 2005-02-16 | ダイヤニトリックス株式会社 | 水溶性重合体の製造方法 |
JP3693084B2 (ja) * | 1997-07-16 | 2005-09-07 | ダイヤニトリックス株式会社 | 水溶性重合体の製造方法 |
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WO2001081431A1 (fr) | 2001-11-01 |
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