WO2018131687A1 - 積層体 - Google Patents
積層体 Download PDFInfo
- Publication number
- WO2018131687A1 WO2018131687A1 PCT/JP2018/000694 JP2018000694W WO2018131687A1 WO 2018131687 A1 WO2018131687 A1 WO 2018131687A1 JP 2018000694 W JP2018000694 W JP 2018000694W WO 2018131687 A1 WO2018131687 A1 WO 2018131687A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- polymer
- polymer layer
- base material
- latex
- polymer latex
- Prior art date
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- 229920000642 polymer Polymers 0.000 claims abstract description 319
- 239000000835 fiber Substances 0.000 claims abstract description 208
- 229920000126 latex Polymers 0.000 claims abstract description 176
- 239000004816 latex Substances 0.000 claims abstract description 176
- 239000000463 material Substances 0.000 claims abstract description 122
- 239000000178 monomer Substances 0.000 claims description 85
- 239000000758 substrate Substances 0.000 claims description 62
- 230000001681 protective effect Effects 0.000 claims description 47
- 239000000701 coagulant Substances 0.000 claims description 41
- 239000002562 thickening agent Substances 0.000 claims description 31
- 230000003204 osmotic effect Effects 0.000 claims description 25
- 238000004519 manufacturing process Methods 0.000 claims description 23
- 239000007787 solid Substances 0.000 claims description 23
- 229920000459 Nitrile rubber Polymers 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- 150000001993 dienes Chemical class 0.000 claims description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 13
- 150000002825 nitriles Chemical class 0.000 claims description 12
- 229920003169 water-soluble polymer Polymers 0.000 claims description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 238000005345 coagulation Methods 0.000 claims description 2
- 230000015271 coagulation Effects 0.000 claims description 2
- 238000010030 laminating Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 169
- 239000002585 base Substances 0.000 description 113
- 238000000034 method Methods 0.000 description 35
- 239000000203 mixture Substances 0.000 description 35
- 229910052751 metal Inorganic materials 0.000 description 22
- 239000002184 metal Substances 0.000 description 22
- 238000000465 moulding Methods 0.000 description 22
- 230000032683 aging Effects 0.000 description 20
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 19
- 239000003431 cross linking reagent Substances 0.000 description 19
- 229910052717 sulfur Inorganic materials 0.000 description 18
- 239000011593 sulfur Substances 0.000 description 18
- -1 wool Substances 0.000 description 17
- 238000006116 polymerization reaction Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- 239000002904 solvent Substances 0.000 description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 238000004132 cross linking Methods 0.000 description 12
- 150000003839 salts Chemical class 0.000 description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 10
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 9
- 229920001971 elastomer Polymers 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 8
- 238000007720 emulsion polymerization reaction Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000005060 rubber Substances 0.000 description 8
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 6
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 235000011054 acetic acid Nutrition 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 238000003795 desorption Methods 0.000 description 4
- 239000003995 emulsifying agent Substances 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- 230000000149 penetrating effect Effects 0.000 description 4
- 150000002978 peroxides Chemical class 0.000 description 4
- 239000003505 polymerization initiator Substances 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- 238000004073 vulcanization Methods 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229920003244 diene elastomer Polymers 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910001507 metal halide Inorganic materials 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 241000894007 species Species 0.000 description 3
- 229920003002 synthetic resin Polymers 0.000 description 3
- 239000000057 synthetic resin Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- YAJYJWXEWKRTPO-UHFFFAOYSA-N 2,3,3,4,4,5-hexamethylhexane-2-thiol Chemical compound CC(C)C(C)(C)C(C)(C)C(C)(C)S YAJYJWXEWKRTPO-UHFFFAOYSA-N 0.000 description 2
- SDJHPPZKZZWAKF-UHFFFAOYSA-N 2,3-dimethylbuta-1,3-diene Chemical compound CC(=C)C(C)=C SDJHPPZKZZWAKF-UHFFFAOYSA-N 0.000 description 2
- 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
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 2
- 229940054266 2-mercaptobenzothiazole Drugs 0.000 description 2
- GIUBHMDTOCBOPA-UHFFFAOYSA-N 3h-1,3-benzothiazole-2-thione;zinc Chemical compound [Zn].C1=CC=C2SC(S)=NC2=C1 GIUBHMDTOCBOPA-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 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
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 230000001112 coagulating effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 2
- ZQMIGQNCOMNODD-UHFFFAOYSA-N diacetyl peroxide Chemical compound CC(=O)OOC(C)=O ZQMIGQNCOMNODD-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- AUZONCFQVSMFAP-UHFFFAOYSA-N disulfiram Chemical compound CCN(CC)C(=S)SSC(=S)N(CC)CC AUZONCFQVSMFAP-UHFFFAOYSA-N 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000002431 foraging effect Effects 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000002763 monocarboxylic acids Chemical class 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 239000005077 polysulfide Substances 0.000 description 2
- 229920001021 polysulfide Polymers 0.000 description 2
- 150000008117 polysulfides Polymers 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 230000005070 ripening Effects 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 125000001273 sulfonato group Chemical class [O-]S(*)(=O)=O 0.000 description 2
- 125000000542 sulfonic acid group Chemical group 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- 229920002994 synthetic fiber Polymers 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
- 238000012546 transfer Methods 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical compound C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 description 1
- SVHAMPNLOLKSFU-UHFFFAOYSA-N 1,2,2-trichloroethenylbenzene Chemical compound ClC(Cl)=C(Cl)C1=CC=CC=C1 SVHAMPNLOLKSFU-UHFFFAOYSA-N 0.000 description 1
- 150000005206 1,2-dihydroxybenzenes Chemical class 0.000 description 1
- WGJCBBASTRWVJL-UHFFFAOYSA-N 1,3-thiazolidine-2-thione Chemical compound SC1=NCCS1 WGJCBBASTRWVJL-UHFFFAOYSA-N 0.000 description 1
- 150000005208 1,4-dihydroxybenzenes Chemical class 0.000 description 1
- AYMDJPGTQFHDSA-UHFFFAOYSA-N 1-(2-ethenoxyethoxy)-2-ethoxyethane Chemical compound CCOCCOCCOC=C AYMDJPGTQFHDSA-UHFFFAOYSA-N 0.000 description 1
- XSZYESUNPWGWFQ-UHFFFAOYSA-N 1-(2-hydroperoxypropan-2-yl)-4-methylcyclohexane Chemical compound CC1CCC(C(C)(C)OO)CC1 XSZYESUNPWGWFQ-UHFFFAOYSA-N 0.000 description 1
- LGBYJXBCVZKJBL-UHFFFAOYSA-N 1-[(2-oxoazepan-1-yl)disulfanyl]azepan-2-one Chemical compound O=C1CCCCCN1SSN1C(=O)CCCCC1 LGBYJXBCVZKJBL-UHFFFAOYSA-N 0.000 description 1
- OZCMOJQQLBXBKI-UHFFFAOYSA-N 1-ethenoxy-2-methylpropane Chemical compound CC(C)COC=C OZCMOJQQLBXBKI-UHFFFAOYSA-N 0.000 description 1
- LAYAKLSFVAPMEL-UHFFFAOYSA-N 1-ethenoxydodecane Chemical compound CCCCCCCCCCCCOC=C LAYAKLSFVAPMEL-UHFFFAOYSA-N 0.000 description 1
- OVGRCEFMXPHEBL-UHFFFAOYSA-N 1-ethenoxypropane Chemical compound CCCOC=C OVGRCEFMXPHEBL-UHFFFAOYSA-N 0.000 description 1
- CISIJYCKDJSTMX-UHFFFAOYSA-N 2,2-dichloroethenylbenzene Chemical compound ClC(Cl)=CC1=CC=CC=C1 CISIJYCKDJSTMX-UHFFFAOYSA-N 0.000 description 1
- WQMSFSSGCZUEPE-UHFFFAOYSA-N 2,3-dibutyl-4-hydroxybenzenecarbodithioic acid Chemical compound CCCCc1c(O)ccc(C(S)=S)c1CCCC WQMSFSSGCZUEPE-UHFFFAOYSA-N 0.000 description 1
- RWGJDHDOFUBENT-UHFFFAOYSA-N 2,3-diethyl-4-hydroxybenzenecarbodithioic acid Chemical compound CCc1c(O)ccc(C(S)=S)c1CC RWGJDHDOFUBENT-UHFFFAOYSA-N 0.000 description 1
- GSFSVEDCYBDIGW-UHFFFAOYSA-N 2-(1,3-benzothiazol-2-yl)-6-chlorophenol Chemical compound OC1=C(Cl)C=CC=C1C1=NC2=CC=CC=C2S1 GSFSVEDCYBDIGW-UHFFFAOYSA-N 0.000 description 1
- 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 1
- RCPUUVXIUIWMEE-UHFFFAOYSA-N 2-(2,4-dinitrophenyl)sulfanyl-1,3-benzothiazole Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC=C1SC1=NC2=CC=CC=C2S1 RCPUUVXIUIWMEE-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 1
- SBYMUDUGTIKLCR-UHFFFAOYSA-N 2-chloroethenylbenzene Chemical compound ClC=CC1=CC=CC=C1 SBYMUDUGTIKLCR-UHFFFAOYSA-N 0.000 description 1
- NRSMWHGLCNBZSO-UHFFFAOYSA-N 2-ethylidenebutanedioic acid Chemical compound CC=C(C(O)=O)CC(O)=O NRSMWHGLCNBZSO-UHFFFAOYSA-N 0.000 description 1
- NCNAZAGHUIATKV-UHFFFAOYSA-N 2-hydroxy-2-(prop-2-enoylamino)propane-1-sulfonic acid Chemical compound OS(=O)(=O)CC(O)(C)NC(=O)C=C NCNAZAGHUIATKV-UHFFFAOYSA-N 0.000 description 1
- BTOVVHWKPVSLBI-UHFFFAOYSA-N 2-methylprop-1-enylbenzene Chemical compound CC(C)=CC1=CC=CC=C1 BTOVVHWKPVSLBI-UHFFFAOYSA-N 0.000 description 1
- RPBWMJBZQXCSFW-UHFFFAOYSA-N 2-methylpropanoyl 2-methylpropaneperoxoate Chemical compound CC(C)C(=O)OOC(=O)C(C)C RPBWMJBZQXCSFW-UHFFFAOYSA-N 0.000 description 1
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- BIISIZOQPWZPPS-UHFFFAOYSA-N 2-tert-butylperoxypropan-2-ylbenzene Chemical compound CC(C)(C)OOC(C)(C)C1=CC=CC=C1 BIISIZOQPWZPPS-UHFFFAOYSA-N 0.000 description 1
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 description 1
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 description 1
- OHXAOPZTJOUYKM-UHFFFAOYSA-N 3-Chloro-2-methylpropene Chemical compound CC(=C)CCl OHXAOPZTJOUYKM-UHFFFAOYSA-N 0.000 description 1
- ZTHJQCDAHYOPIK-UHFFFAOYSA-N 3-methylbut-2-en-2-ylbenzene Chemical compound CC(C)=C(C)C1=CC=CC=C1 ZTHJQCDAHYOPIK-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- HLBZWYXLQJQBKU-UHFFFAOYSA-N 4-(morpholin-4-yldisulfanyl)morpholine Chemical compound C1COCCN1SSN1CCOCC1 HLBZWYXLQJQBKU-UHFFFAOYSA-N 0.000 description 1
- RJMXTPCJDQRHQG-UHFFFAOYSA-N 4-hydroxy-2,3-dimethylbenzenecarbothioic s-acid Chemical compound CC1=C(C)C(C(S)=O)=CC=C1O RJMXTPCJDQRHQG-UHFFFAOYSA-N 0.000 description 1
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- XWPGCGMKBKONAU-UHFFFAOYSA-N zirconium(4+);disulfide Chemical compound [S-2].[S-2].[Zr+4] XWPGCGMKBKONAU-UHFFFAOYSA-N 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Images
Classifications
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- D—TEXTILES; PAPER
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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Definitions
- the present invention relates to a laminate in which a fiber base composed of a plurality of fibers and a polymer layer formed from a polymer latex are laminated. Moreover, this invention relates to a protective glove provided with the said laminated body.
- protective gloves for example, protective gloves obtained by forming a film by attaching rubber or resin to the outer surface of a fiber glove attached to a glove mold are known.
- the rubber or resin may penetrate from the outer surface to the inside of the fiber glove, which causes the rubber or resin to adhere to the glove mold and attach the protective glove to the glove.
- the productivity of the protective gloves is lowered, and the comfort when the obtained protective gloves are worn is lowered.
- Patent Document 1 a fiber glove is impregnated with a coagulant solution obtained by dissolving an acid or a polyvalent metal salt, and then the surface of the glove body is applied.
- a protective glove is disclosed in which a thin film is formed by contacting an emulsion of rubber or synthetic resin, and a coating film of a synthetic resin paste is formed on the thin film.
- the protective glove obtained by the technique of Patent Document 1 is such that the thickness and the amount of penetration into the fiber glove are not controlled with respect to the thin film formed using an emulsion of rubber or synthetic resin, and the protective glove obtained is obtained There was a problem that the flexibility of.
- the present invention has been made in view of such a situation, and an object of the present invention is to provide a laminate that is excellent in productivity, and also excellent in flexibility and comfort during wearing. Moreover, this invention also aims at providing a protective glove provided with such a laminated body.
- the present inventors have found a laminated body in which a fiber base composed of a plurality of fibers and a polymer layer formed from a polymer latex are laminated.
- the ratio of the thickness of the portion of the polymer layer that has penetrated between the fibers to the average thickness of the base material layer of the fiber base material is controlled within a predetermined range, and the surface of the fiber base material in the polymer layer.
- a laminate comprising a fiber substrate composed of a plurality of fibers and a polymer layer formed from a polymer latex, wherein the polymer layer is partially Is the surface of the fiber base material of the osmotic polymer layer that is a portion of the polymer layer that has permeated between the fibers.
- the thickness t 2 [ ⁇ m] of the surface polymer layer is 80 ⁇ m or more when the thickness of the surface polymer layer is t 2 [ ⁇ m].
- a laminate is provided.
- the polymer latex preferably contains a nonionic water-soluble polymer as a thickener.
- the content ratio of the nonionic water-soluble polymer in the polymer latex is preferably 0.1 to 5.0% by weight.
- the nonionic water-soluble polymer is preferably polyvinyl alcohol and / or polyvinyl pyrrolidone.
- the polymer constituting the polymer latex is preferably nitrile rubber.
- the nitrile rubber preferably contains an ethylenically unsaturated nitrile monomer unit, a conjugated diene monomer unit, and an ethylenically unsaturated acid monomer unit.
- a protective glove provided with the above laminate is provided.
- it is a manufacturing method of said laminated body, Comprising: Latex adhesion process which adheres the said polymer latex to the said fiber base material, and the said polymer latex adhered to the said fiber base material A coagulation step of bringing the polymer latex into contact with a coagulant solution to coagulate the polymer in the polymer latex, thereby forming the polymer layer, and attaching the polymer latex to the fiber substrate.
- the polymer latex In the state in which the viscosity of the polymer latex is controlled in the range of 600 to 25,000 mPa ⁇ s at a rotational speed of 10 rpm measured using a B-type viscometer, the polymer latex is A method for producing a laminate to be adhered to a fiber substrate is provided.
- the polymer latex when the polymer latex is adhered to the fiber substrate, the polymer latex has a temperature of 25 ° C., a solid content concentration of 45% by weight, and a B-type viscometer.
- the polymer latex is preferably adhered to the fiber base material in a state where the viscosity at a rotational speed of 10 rpm measured using is controlled to 600 to 25,000 mPa ⁇ s.
- a laminate that is excellent in productivity and also excellent in flexibility and comfort at the time of wearing.
- a protective glove provided with such a laminated body can be provided.
- FIG. 1 is a schematic view of a fiber substrate used in the present invention and a schematic view of a laminate of the present invention.
- the laminate of the present invention is a laminate in which a fiber base composed of a plurality of fibers and a polymer layer formed from a polymer latex are laminated, and the polymer layer is partially From the surface of the fiber base material of the permeation polymer layer that covers the fiber base material in a state of permeation between the fibers, and is a portion of the polymer layer permeated between the fibers.
- the fiber substrate used in the present invention is not particularly limited as long as it is made of fiber.
- fibers constituting the fiber base material natural fibers such as cotton, wool, hemp, and wool, synthetic fibers such as polyester, polyurethane, acrylic, and nylon can be used as materials. Among these, cotton is used. Is preferred.
- the fibers constituting the fiber base material used in the present invention may be single fibers (one by one extracted from the above-mentioned natural fibers or synthetic fibers), or may be twisted yarns composed of a plurality of single fibers. Although it is good, it is preferably a twisted yarn.
- the fiber substrate may be a knitted or woven fiber as described above, or a non-woven fabric.
- the fiber base material may be sewn.
- the ratio (t 1 / d) of the thickness t 1 of the polymer layer to the base layer average thickness d of the fiber substrate is within the above range.
- the substrate layer average thickness d of the fiber substrate is preferably 50 to 3,000 ⁇ m, more preferably 100 to 2,000 ⁇ m, and still more preferably 400 to 900 ⁇ m.
- the fiber base material is composed of a plurality of fibers, particularly when the fiber base material is a woven fabric, the portion in which the fibers are usually folded and the overlapping degree of the fibers in the thickness direction is dense. There is a portion (a portion where the number of overlapping fibers is large) and a portion where a degree of overlapping of the fibers in the thickness direction is sparse (a portion where the number of overlapping fibers is small), and a layer including these portions ( It is comprised by the base material layer). For this reason, in the microstructure of the fiber base material, the thickness may be different between the portion where the fiber overlap is dense and the portion where the fiber overlap is sparse.
- the base material layer average thickness d of the fiber base material is determined as an average value in which the thickness of the portion where the overlapping degree of the fibers is dense is the thickness of the fiber base material. That is, the average of the thicknesses of the portions where the overlapping degree of the fibers is dense is defined as the base layer average thickness d.
- the linear density of the fibers constituting the fiber substrate is not particularly limited, but is preferably 50 to 500 denier.
- the gauge number of the fiber base material is not particularly limited, but a part of the polymer layer can be appropriately permeated by the fiber base material (the weight formed when the polymer layer is formed on the fiber base material). From the viewpoint that the thickness t 1 of the osmotic polymer layer in the combined layer can be controlled in a more appropriate range), it is preferably 7 to 18 gauge.
- the number of gauges refers to the number of knitting machine needles between 1 inch.
- a polymer latex described later is attached to such a fiber base, and then a coagulant solution is brought into contact with the polymer latex attached to the fiber base. It can be obtained by forming a polymer layer by solidifying the polymer. In this case, the polymer layer is formed so as to cover the fiber base material in a state where a part of the polymer layer penetrates the fiber base material.
- the polymer latex used in the present invention is not particularly limited, but it is preferable to use a polymer containing a rubbery polymer as the polymer because the resulting laminate can be made more flexible.
- the rubber-like polymer include natural rubber; conjugated diene rubber obtained by polymerizing or copolymerizing conjugated dienes such as butadiene and isoprene; among these, conjugated diene rubber is preferable.
- conjugated diene rubber include so-called nitrile rubber, isoprene rubber, styrene-butadiene rubber, chloroprene rubber and the like obtained by copolymerizing nitrile, and among these, nitrile rubber is particularly preferable.
- the nitrile rubber is not particularly limited, and a nitrile rubber obtained by copolymerizing an ⁇ , ⁇ -ethylenically unsaturated nitrile monomer and other copolymerizable monomers used as necessary can be used.
- the ⁇ , ⁇ -ethylenically unsaturated nitrile monomer is not particularly limited, and an ethylenically unsaturated compound having a nitrile group and preferably having 3 to 18 carbon atoms can be used.
- Examples of such ⁇ , ⁇ -ethylenically unsaturated nitrile monomers include acrylonitrile, methacrylonitrile, halogen-substituted acrylonitrile and the like, and among these, acrylonitrile is particularly preferable.
- These ⁇ , ⁇ -ethylenically unsaturated nitrile monomers may be used alone or in combination of two or more.
- the content ratio of the ⁇ , ⁇ -ethylenically unsaturated nitrile monomer unit in the nitrile rubber is preferably 10 to 45% by weight, more preferably 20 to 40% by weight, based on the total monomer units.
- the nitrile rubber preferably contains a conjugated diene monomer unit from the viewpoint of imparting rubber elasticity to the resulting polymer layer.
- conjugated diene monomer forming the conjugated diene monomer unit examples include 1,3-butadiene, isoprene, 2,3-dimethyl-1,3-butadiene, 1,3-pentadiene, chloroprene and the like having 4 to 4 carbon atoms. 6 conjugated diene monomers are preferred, 1,3-butadiene and isoprene are more preferred, and 1,3-butadiene is particularly preferred. In addition, these conjugated diene monomers may be used individually by 1 type, and may be used in combination of 2 or more type.
- the content ratio of the conjugated diene monomer unit is preferably 40 to 80% by weight, more preferably 52 to 78% by weight, based on all monomer units constituting the nitrile rubber.
- Nitrile rubber is also a monomer that forms ⁇ , ⁇ -ethylenically unsaturated nitrile monomer units and other ethylenically unsaturated monomers that are copolymerizable with monomers that form conjugated diene monomer units.
- An acid monomer may be included.
- Such other copolymerizable ethylenically unsaturated acid monomer is not particularly limited, and examples thereof include a carboxyl group-containing ethylenically unsaturated monomer, a sulfonic acid group-containing ethylenically unsaturated monomer, Examples thereof include phosphoric acid group-containing ethylenically unsaturated monomers.
- the carboxyl group-containing ethylenically unsaturated monomer is not particularly limited, but ethylenically unsaturated monocarboxylic acids such as acrylic acid, methacrylic acid, and crotonic acid; fumaric acid, maleic acid, itaconic acid, maleic anhydride, anhydrous And ethylenically unsaturated polyvalent carboxylic acids such as itaconic acid and anhydrides thereof; partially esterified products of ethylenically unsaturated polyvalent carboxylic acids such as methyl maleate and methyl itaconic acid; and the like.
- monocarboxylic acids such as acrylic acid, methacrylic acid, and crotonic acid
- fumaric acid, maleic acid, itaconic acid, maleic anhydride anhydrous And ethylenically unsaturated polyvalent carboxylic acids such as itaconic acid and anhydrides thereof
- the sulfonic acid group-containing ethylenically unsaturated monomer is not particularly limited, but vinyl sulfonic acid, methyl vinyl sulfonic acid, styrene sulfonic acid, (meth) allyl sulfonic acid, (meth) acrylic acid-2-sulfonic acid ethyl And 2-acrylamido-2-hydroxypropanesulfonic acid.
- the phosphoric acid group-containing ethylenically unsaturated monomer is not particularly limited, but includes (meth) acrylic acid-3-chloro-2-propyl phosphate, (meth) acrylic acid-2-ethyl phosphate, 3-allyloxy. Examples include -2-hydroxypropane phosphoric acid.
- copolymerizable ethylenically unsaturated acid monomers can be used as alkali metal salts or ammonium salts, and can be used singly or in combination of two or more. Good.
- carboxyl group-containing ethylenically unsaturated monomers are preferable, ethylenically unsaturated monocarboxylic acids are more preferable, and methacrylic acid is particularly preferable.
- the content of the other copolymerizable ethylenically unsaturated acid monomer in the polymer constituting the polymer latex used in the present invention is preferably 2 with respect to all monomer units in the polymer. ⁇ 8% by weight.
- the polymer constituting the polymer latex may contain other monomer units.
- monomers that form other monomer units include conjugated diene monomers, ethylenically unsaturated nitrile monomer units, and monomers copolymerizable with ethylenically unsaturated acid monomers. There is no particular limitation, and examples thereof include the following monomers.
- aromatic vinyl monomers such as styrene, ⁇ -methyl styrene, monochloro styrene, dichloro styrene, trichloro styrene, monomethyl styrene, dimethyl styrene, trimethyl styrene, hydroxymethyl styrene; acrylamide, Ethylenically unsaturated carboxylic acid amide monomers such as methacrylamide, N, N-dimethylacrylamide, N-methylolacrylamide; methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, (meth ) Ethylenically unsaturated carboxylic acid alkyl ester monomers such as 2-ethylhexyl acrylate; vinyl acetate monomers such as vinyl acetate, vinyl propionate and vinyl versatate; vinyl chloride, vinylidene chloride
- the content of other monomer units in the polymer constituting the polymer latex is a point of view that prevents the polymer layer from peeling off from the fiber substrate, and when used as a work glove. From the viewpoint of suppressing fatigue, and from the viewpoint of suppressing permeation of solvent gas when worn as a work glove, it is preferably 26% by weight or less, more preferably 10% by weight, based on the total monomer units in the polymer. % Or less, more preferably 7% by weight or less, and particularly preferably 5% by weight or less.
- the polymer latex used in the present invention is not particularly limited, and may be, for example, a polymer latex obtained by polymerizing a monomer mixture containing the above monomer.
- a latex obtained by emulsion polymerization, a latex obtained by phase inversion emulsification of a polymer solution obtained by solution polymerization of the monomer mixture, and the like can be used.
- the composition of the resulting copolymer can be easily adjusted by adjusting the composition of the monomer mixture used for the emulsion polymerization.
- a method of emulsion polymerization a conventionally known method can be employed.
- polymerization auxiliary materials such as an emulsifier, a polymerization initiator, and a molecular weight modifier can be used.
- the method for adding these polymerization auxiliary materials is not particularly limited, and any method such as an initial batch addition method, a divided addition method, or a continuous addition method may be used.
- the emulsifier examples include, but are not limited to, anionic surfactants, nonionic surfactants, cationic surfactants, and amphoteric surfactants. Among these, alkylbenzene sulfonates, aliphatics Anionic surfactants such as sulfonates, sulfates of higher alcohols, ⁇ -olefin sulfonates, and alkyl ether sulfates are preferred.
- the amount of the emulsifier is preferably 0.5 to 10 parts by weight, more preferably 1 to 8 parts by weight with respect to 100 parts by weight of the total monomers used.
- a radical initiator is preferable.
- the radical initiator is not particularly limited, and examples thereof include inorganic peroxides such as sodium persulfate, potassium persulfate, ammonium persulfate, potassium perphosphate, and hydrogen peroxide; t-butyl peroxide, cumene hydroperoxide, p-menthane hydroperoxide, di-t-butyl peroxide, t-butylcumyl peroxide, acetyl peroxide, isobutyryl peroxide, octanoyl peroxide, dibenzoyl peroxide, 3,5,5-trimethylhexanoyl Organic peroxides such as peroxide and t-butylperoxyisobutyrate; azo compounds such as azobisisobutyronitrile, azobis-2,4-dimethylvaleronitrile, azobiscyclohexanecarbonitrile, methyl
- inorganic peroxides or organic peroxides are preferred, inorganic peroxides are more preferable, persulfate are particularly preferred.
- These polymerization initiators may be used individually by 1 type, and may be used in combination of 2 or more type. The amount of the polymerization initiator used is preferably 0.01 to 2 parts by weight, more preferably 0.05 to 1.5 parts by weight with respect to 100 parts by weight of the total monomers used.
- the molecular weight modifier is not particularly limited.
- ⁇ -methylstyrene dimer mercaptans such as t-dodecyl mercaptan, n-dodecyl mercaptan, octyl mercaptan; halogenated carbon tetrachloride, methylene chloride, methylene bromide, etc. Hydrocarbons; sulfur-containing compounds such as tetraethylthiuram disulfide, dipentamethylene thiuram disulfide, diisopropylxanthogen disulfide; and the like.
- molecular weight regulators may be used alone or in combination of two or more.
- the amount of the molecular weight modifier used varies depending on the type, but is preferably 0.1 to 1.5 parts by weight, more preferably 0.2 to 1.0 parts by weight, based on 100 parts by weight of all monomers used. Part.
- Emulsion polymerization is usually performed in water.
- the amount of water used is preferably 80 to 500 parts by weight, more preferably 100 to 200 parts by weight, based on 100 parts by weight of the total monomers used.
- polymerization auxiliary materials other than the above may be further used as necessary.
- the polymerization auxiliary material include a chelating agent, a dispersing agent, a pH adjusting agent, a deoxidizing agent, a particle size adjusting agent and the like, and the type and amount of use thereof are not particularly limited.
- Examples of the monomer addition method include a method of adding monomers to be used in a reaction vessel all at once, a method of adding continuously or intermittently as the polymerization proceeds, and a part of the monomer is added. And a method in which the remaining monomer is continuously or intermittently added and polymerized, and any method may be employed.
- the composition of the mixture may be constant or may be changed.
- Each monomer may be added to the reaction vessel after previously mixing various monomers to be used, or may be added separately to the reaction vessel.
- the polymerization temperature at the time of emulsion polymerization is not particularly limited, but is usually 0 to 95 ° C., preferably 5 to 70 ° C.
- the polymerization time is not particularly limited, but is usually about 5 to 40 hours.
- the monomer is emulsion-polymerized, and when the predetermined polymerization conversion rate is reached, the polymerization reaction is stopped by cooling the polymerization system or adding a polymerization terminator.
- the polymerization conversion rate when stopping the polymerization reaction is usually 80% by weight or more, preferably 90% by weight or more.
- the polymerization terminator is not particularly limited as long as it is usually used in emulsion polymerization. Specific examples thereof include hydroxylamine, hydroxyamine sulfate, diethylhydroxyamine, hydroxyaminesulfonic acid and alkali metals thereof.
- Hydroxyamine compounds such as salts; sodium dimethyldithiocarbamate; hydroquinone derivatives; catechol derivatives; aromatic hydroxydithiocarboxylic acids such as hydroxydimethylbenzenethiocarboxylic acid, hydroxydiethylbenzenedithiocarboxylic acid, hydroxydibutylbenzenedithiocarboxylic acid, and alkali metal salts thereof
- Aromatic hydroxydithiocarboxylic acid compounds such as;
- the amount of the polymerization terminator used is not particularly limited, but is usually 0.05 to 2 parts by weight with respect to 100 parts by weight of the total monomers used.
- unreacted monomers may be removed to adjust the solid content concentration and pH.
- the weight average particle diameter of the polymer particles constituting the polymer latex is usually 30 to 1000 nm, preferably 50 to 500 nm, more preferably 70 to 200 nm.
- the solid content concentration of the polymer latex is usually 20 to 65% by weight, preferably 30 to 60% by weight, more preferably 35 to 55% by weight.
- the pH of the polymer latex is usually 5 to 13, preferably 7 to 10, and more preferably 7.5 to 9.
- the polymer latex used in the present invention may be a polymer latex composition by adding a crosslinking agent, a crosslinking accelerator, zinc oxide, or the like.
- a crosslinking agent e.g., a crosslinking accelerator, zinc oxide, or the like.
- the crosslinking agent it is preferable to use a sulfur-based crosslinking agent.
- a sulfur type crosslinking agent Sulfur, such as powder sulfur, sulfur white, precipitation sulfur, colloidal sulfur, surface treatment sulfur, insoluble sulfur; sulfur chloride, sulfur dichloride, morpholine disulfide, alkylphenol disulfide, dibenzothia Sulfur-containing compounds such as zirconium disulfide, caprolactam disulfide (N, N′-dithio-bis (hexahydro-2H-azepinone-2)), phosphorus-containing polysulfide, polymer polysulfide; tetramethylthiuram disulfide, selenium dimethyldithiocarbamate, And sulfur-donating compounds such as 2- (4′-morpholinodithio) benzothiazole.
- These crosslinking agents may be used alone or in combination of two or more.
- the addition amount of the sulfur-based crosslinking agent is preferably 0.01 to 5 parts by weight, more preferably 0.05 to 3 parts by weight, particularly preferably 0. 0 part by weight with respect to 100 parts by weight of the total solid content in the polymer latex. 1 to 2 parts by weight.
- the sulfur-based crosslinking agent is preferably added as a dispersion in which the sulfur-based crosslinking agent is dispersed in a solvent.
- a dispersion By adding it to the polymer latex as a dispersion, a laminate having few defects such as cracks, pinholes, and adhesion of aggregates in the resulting polymer layer can be obtained.
- the method for preparing the dispersion of the sulfur-based crosslinking agent is not particularly limited, but a method of adding a solvent to the sulfur-based crosslinking agent and pulverizing and stirring with a wet pulverizer such as a ball mill or a bead mill is preferable.
- sulfur-based crosslinking agent When sulfur is used as the sulfur-based crosslinking agent, it is preferable to use a crosslinking accelerator (vulcanization accelerator) or zinc oxide in combination.
- vulcanization accelerator vulcanization accelerator
- zinc oxide zinc oxide
- the crosslinking accelerator is not particularly limited.
- dithiocarbamine such as diethyldithiocarbamic acid, dibutyldithiocarbamic acid, di-2-ethylhexyldithiocarbamic acid, dicyclohexyldithiocarbamic acid, diphenyldithiocarbamic acid, and dibenzyldithiocarbamic acid.
- crosslinking accelerators may be used alone or in combination of two or more.
- the amount of the crosslinking accelerator used is preferably 0.1 to 10 parts by weight, more preferably 0.5 to 5 parts by weight with respect to 100 parts by weight of the total solid content in the polymer latex.
- the amount of zinc oxide used is preferably 5 parts by weight or less, more preferably 0.1 to 3 parts by weight, and still more preferably 0.5 to 2 parts by weight with respect to 100 parts by weight of the total solid content in the polymer latex. Part.
- a polymer latex to which a crosslinking agent is added When a polymer latex to which a crosslinking agent is added is used, a polymer latex that has been aged in advance (also referred to as pre-vulcanization) may be used.
- the viscosity of the polymer latex is a viscosity measured at a rotational speed of 10 rpm using a B-type viscometer at a temperature of 25 ° C. and a solid content concentration of 45% by weight, preferably 600 to 25,000 mPa ⁇ s. More preferably 800 to 20,000 mPa ⁇ s, still more preferably 900 to 15,000 mPa ⁇ s, and particularly preferably 1,000 to 12,000 mPa ⁇ s.
- the method for setting the viscosity of the polymer latex in the above range is not particularly limited, but for example, a method of adding a thickener to the polymer latex is preferably used.
- a thickener for example, Vinyl compounds, such as polyvinyl alcohol and polyvinyl pyrrolidone; Cellulose derivatives, such as hydroxyethyl cellulose, hydroxypropyl cellulose, carboxymethylcellulose salt; Polycarboxylic acid compound and its sodium salt; Polyethylene And polyoxyethylene derivatives such as glycol ethers.
- nonionic water-soluble polymers are preferable, and polyvinyl alcohol and polyvinyl pyrrolidone are particularly preferable.
- the content of the nonionic water-soluble polymer in the polymer latex is preferably 0.1 to 5.0% by weight. .
- the viscosity of the polymer latex can be made more appropriate.
- the method of adding a thickener to the polymer latex is not particularly limited, but when using a polymer latex with a cross-linking agent added, the generation of aggregates in the polymer latex is prevented. From the viewpoint that the polymer latex can be transferred better, after adding a part of the thickener before aging the polymer latex, add the remaining thickener after the aging. It is preferable to use a method of adding a thickener after ripening the polymer latex, or a method of adding a thickener after aging the polymer latex.
- a filler such as carbon black, silica, calcium carbonate, aluminum silicate, magnesium silicate, calcium silicate, magnesium oxide, zinc (meth) acrylate, magnesium (meth) acrylate may be added to the polymer latex. Although it is good, it is preferable not to add these fillers to the polymer latex from the viewpoint that the cut resistance when the obtained laminate is used as protective gloves can be further improved.
- additives such as anti-aging agents, antioxidants, preservatives, antibacterial agents, wetting agents, dispersing agents, pigments, dyes, fillers, reinforcing agents, and pH adjusters are added to the polymer latex as necessary. A predetermined amount can also be added.
- the solid content concentration of the polymer latex to which the crosslinking agent is added is preferably 25 to 55% by weight, more preferably 35 to 55% by weight.
- the surface tension of the polymer latex to which a crosslinking agent is added is preferably 25 to 40 mN / m.
- the coagulant solution used in the present invention is obtained by dissolving or dispersing a coagulant in a solvent.
- the coagulant is not particularly limited as long as it can coagulate the polymer in the polymer latex, and a metal salt or the like can be used.
- species which comprises a metal salt For example, Divalent metals, such as lithium, sodium, and potassium; Divalent metals, such as magnesium, calcium, zinc, iron, barium, zirconium, copper; Aluminum And trivalent metals such as
- the salt species constituting the metal salt is not particularly limited, and examples thereof include organic acids such as nitric acid, sulfuric acid, and acetic acid.
- the metal species is preferably a polyvalent metal, more preferably a divalent metal, and particularly preferably calcium.
- the metal salt is preferably a polyvalent metal salt, more preferably a divalent metal nitrate or halide.
- these metal salts include nitrates such as calcium nitrate, barium nitrate and zinc nitrate; metal halide salts such as barium chloride, calcium chloride, magnesium chloride, zinc chloride and aluminum chloride; barium acetate, calcium acetate and acetic acid Acetates such as zinc; sulfates such as calcium sulfate, magnesium sulfate, and aluminum sulfate; among these, nitrates and metal halides are preferable, calcium nitrate and calcium chloride are more preferable, and calcium nitrate is particularly preferable preferable.
- These metal salts can be used alone or in combination of two or more.
- the coagulant solution may further contain an organic acid in addition to the above-described coagulant.
- an organic acid which has at least 1 type of group of a carboxyl group, a sulfo group, a hydroxy group, and a thiol group is preferable.
- Specific examples include acetic acid, formic acid, propionic acid, citric acid, and oxalic acid. Among these, acetic acid is preferable.
- the solvent for dissolving or dispersing the coagulant is not particularly limited, but water, alcohol such as methanol or ethanol, or a mixture thereof can be used, and among these, water is particularly preferable.
- the concentration of the coagulant in the coagulant solution is usually 5 to 50% by weight, preferably 10 to 30% by weight.
- the laminate of the present invention allows a polymer latex to adhere to a fiber substrate, and then contacts such a coagulant solution with the polymer latex adhered to the fiber substrate. It can be obtained by forming a polymer layer by coagulating the polymer in the polymer latex. At this time, a part of the polymer latex adhering to the fiber base material penetrates between the fibers constituting the fiber base material, and in this state, when the coagulant solution is brought into contact with the polymer latex, FIG. As shown in (A) and FIG. 1 (B), a polymer layer is formed on the surface of the fiber base material, and part of the polymer layer penetrates to the gaps of the fibers constituting the fiber base material. It becomes.
- FIG. 1A and 1B are schematic views of a fiber base material and a laminate, respectively.
- FIG. 1A shows a cross-sectional view of the fiber base material
- FIG. 1 is a cross-sectional view of a laminate in which a polymer layer is laminated on the fiber base shown in FIG.
- the polymer layer covers the fiber base material in a state where part of the polymer layer penetrates between the fibers constituting the fiber base material.
- a portion that penetrates into the gaps between the fibers from the surface of the fiber base material is used as the permeation polymer layer, and among the polymer layers, the fiber base material is used.
- the part which covers a fiber base material from the surface of is shown as a surface polymer layer.
- the polymer layer is described as appropriately composed of a osmotic polymer layer and a surface polymer layer.
- the osmotic polymer layer and the surface polymer layer are integrally formed. It will be.
- the laminated body of this invention is not specifically limited, For example, it can be used as a protective glove.
- the fiber substrate is not particularly limited.
- a single fiber twisted yarn is used as the fiber, and a glove-shaped one is used by weaving this twisted yarn. be able to.
- a protective glove can be obtained by forming a polymer layer on a glove-shaped fiber substrate.
- the thickness of the penetrated portion in the fiber i.e., the thickness from the surface of the fiber substrate osmopolymers layer shown in FIG. 1 t 1 ( The unit is ⁇ m)
- the ratio of the thickness t 1 of the osmotic polymer layer to the average thickness d of the base material layer (t 1 / d), where d is the average thickness of the base material layer of the fiber base material (unit is ⁇ m) Is 0.1 to 0.95, preferably 0.1 to 0.9, more preferably 0.15 to 0.8, still more preferably 0.15 to 0.4, and particularly preferably 0.15. ⁇ 0.35.
- the ratio (t 1 / d) of the thickness t 1 of the osmotic polymer layer to the base layer average thickness d is in the above range, when the obtained laminate is used as a protective glove, It is possible to prevent the occurrence of a strike through in which the coalesced layer reaches the back surface of the fiber base material, thereby reducing the productivity of protective gloves caused by the back through (for example, a glove-shaped fiber base material)
- a polymer layer is formed by adhering a polymer latex to a fiber base material in a state where it is attached to a glove mold, the polymer latex adheres to the glove mold due to a back-through, resulting in a protective glove obtained.
- the ratio (t 1 / d) of the thickness t 1 of the osmotic polymer layer to the average thickness d of the base material layer may be in the above range, but the thickness t 1 of the osmotic polymer layer.
- the thickness itself is preferably 50 to 600 ⁇ m, more preferably 100 to 550 ⁇ m, still more preferably 120 to 500 ⁇ m, and particularly preferably 120 to 250 ⁇ m.
- the thickness of the portion of the polymer layer that covers the surface of the fiber substrate is 80 ⁇ m or more, preferably 100 ⁇ m. As mentioned above, More preferably, it is 180 micrometers or more.
- the thickness t 2 of the surface polymer layer is in the above range, the durability is improved in the case of using the obtained laminate as a protective glove.
- the upper limit of the thickness t 2 of the surface polymer layer is not particularly limited, preferably 1,000 ⁇ m less, more preferably 800 ⁇ m or less, more preferably 600 ⁇ m or less.
- the ratio of the thickness of the osmotic polymer layer to the surface polymer layer in the polymer layer is not particularly limited, but the ratio of the thickness t 2 of the surface polymer layer to the thickness t 1 of the osmotic polymer layer (t 2 / t 1 ) is preferably 0.2 to 5, more preferably 0.3 to 4, further preferably 0.8 to 4, and particularly preferably 1 to 2.
- the total thickness of the polymer layer that is, the sum of the thickness t 1 of the penetrating polymer layer and the thickness t 2 of the surface polymer layer is not particularly limited, but is preferably 150 ⁇ m or more.
- the laminate of the present invention has a ratio (t 1 / d) of the thickness t 1 of the osmotic polymer layer to the average thickness d of the base material layer and a thickness t 2 [ ⁇ m] of the surface polymer layer.
- t 1 / d the thickness of the osmotic polymer layer to the average thickness d of the base material layer
- t 2 [ ⁇ m] the thickness of the surface polymer layer.
- the production method of the present invention comprises a latex adhesion step for adhering the above polymer latex to a fiber substrate, and a polymer in the polymer latex by bringing a coagulant solution into contact with the polymer latex adhered to the fiber substrate. Coagulating step to form a polymer layer.
- the viscosity of the polymer latex is the viscosity at a rotational speed of 10 rpm measured using a B-type viscometer.
- the polymer latex is adhered to the fiber substrate in a state controlled in the range of 600 to 25,000 mPa ⁇ s.
- the viscosity of the polymer latex is more preferably 800 to 20,000 mPa ⁇ s, still more preferably 900 to 15,000 mPa ⁇ s, and particularly preferably 1,000 to 12,000 mPa ⁇ s.
- the temperature and solid content concentration of the polymer latex when the polymer latex is adhered to the fiber substrate are not particularly limited, and the viscosity under the condition of the rotation speed of 10 rpm measured using a B-type viscometer is the above.
- the temperature may be controlled to be within a range, but preferably in a state where the temperature is controlled to 20 to 40 ° C. and the solid content concentration is 30 to 50% by weight, particularly in a state where the temperature is controlled to 25 ° C. and the solid content concentration is 45% by weight. It is preferable to attach the polymer latex to the fiber substrate.
- the polymer latex when the polymer latex is adhered to the fiber substrate by adhering the polymer latex to the fiber substrate with the viscosity of the polymer latex adjusted to the above range, the polymer latex is The rate of permeation between the fibers of the fiber base material can be made moderate, thereby allowing the polymer latex to permeate appropriately between the fibers of the fiber base material without passing through. Can do. Therefore, the coagulant solution can be brought into contact with the polymer latex adhering to the fiber base material while the polymer latex is appropriately infiltrated into the fiber base material. As a result, a part of the polymer latex is made into the fiber base material.
- the polymer in the polymer latex coagulates while being appropriately permeated into the polymer layer to form a polymer layer, and the obtained laminate has a thickness t 1 of the osmotic polymer layer with respect to the substrate layer average thickness d of the fiber substrate.
- the ratio (t 1 / d) can be controlled within the above range.
- a method of adding a thickener to the polymer latex can be used.
- a method for adding a thickener when using a polymer latex to which a crosslinking agent is added, it is possible to prevent agglomerates from being generated in the polymer latex and to transfer the polymer latex. From the viewpoint of being able to perform better, a method of adding a thickener before and after aging the polymer latex or a method of adding a thickener after aging the polymer latex is used. It is preferable.
- the temperature condition for aging the polymer latex is not particularly limited, but is preferably 20 to 50 ° C.
- the time for aging is the viewpoint of preventing peeling between the fiber substrate and the polymer layer, the viewpoint of improving the durability when the obtained laminate is used as a protective glove, and the protective glove for working. From the viewpoint of suppressing the permeation of solvent gas when used as a glove, it is preferably 4 hours or longer and 120 hours or shorter, more preferably 24 hours or longer and 72 hours or shorter.
- the method for attaching the polymer latex to the fiber substrate is not particularly limited, and examples thereof include a method of immersing the fiber substrate in the polymer latex.
- the molding die for covering the fiber substrate is not particularly limited, but various materials such as porcelain, glass, metal, and plastic can be used.
- the shape of the molding die may be a desired shape according to the shape of the final product.
- various molds for gloves such as a mold having a shape from the wrist to the fingertip as the mold for covering the fiber base material. .
- the drying temperature at this time is not particularly limited, but is preferably 180 ° C. or lower, more preferably 10 to 170 ° C.
- the drying time is not particularly limited, but is preferably 1 second to 60 minutes, more preferably 3 seconds to 30 minutes.
- the polymer latex adhered to the fiber substrate in this manner is brought into contact with a coagulant solution, so that the polymer in the polymer latex is coagulated to form a polymer layer.
- the method of bringing the coagulant solution into contact with the polymer latex adhered to the fiber substrate is not particularly limited, and examples thereof include a method of immersing the fiber substrate to which the polymer latex is adhered in the coagulant solution.
- the fiber base material to which the polymer latex is adhered is immersed in the coagulant solution
- the fiber base material to which the polymer latex is adhered is placed on a molding die having a desired shape and the coagulant solution. It is preferable to immerse.
- the fiber base material is attached to the fiber base material as described above in a state where the fiber base material is previously covered with a molding die of a desired shape, and then the fiber base material to which the polymer latex is attached. Is preferably immersed in a coagulant solution while being covered with a molding die.
- the immersion time when the fiber base material is immersed in the coagulant solution is not particularly limited, but is preferably 30 to 1 second, more preferably 10 to 1 second.
- the solvent contained in the coagulant solution is dried by bringing the coagulant solution into contact with the polymer latex adhered to the fiber base material and then drying. It is preferable to remove.
- the drying temperature at this time is not particularly limited and may be selected according to the solvent to be used, but is preferably 10 to 80 ° C., more preferably 15 to 70 ° C.
- the drying time is not particularly limited, but is preferably 600 to 1 second, more preferably 300 to 5 seconds.
- the crosslinking agent as polymer latex
- the polymer latex adhering to the fiber base material is heated.
- the heating temperature for crosslinking is preferably 60 to 160 ° C, more preferably 80 to 150 ° C. By setting the heating temperature within the above range, the time required for the crosslinking reaction can be shortened to improve the productivity of the laminate, and the obtained laminate can suppress the oxidative degradation of the polymer due to excessive heating. The physical properties of can be improved.
- the heating time for crosslinking may be appropriately selected according to the heating temperature, but is usually 5 to 120 minutes.
- a laminate in which a polymer layer is formed on a fiber substrate is obtained as described above.
- the polymer layer is immersed in warm water at 20 to 80 ° C. for about 0.5 to 60 minutes to remove the polymer layer from the polymer layer. It is preferable to remove water-soluble impurities (emulsifier, water-soluble polymer, coagulant, etc.).
- water-soluble impurities emulsifier, water-soluble polymer, coagulant, etc.
- a laminate is obtained by detaching the fiber base material on which the polymer layer is formed from the molding die. Can do.
- the desorption method it is possible to adopt a method of peeling from the mold by hand, or peeling by water pressure or compressed air pressure.
- a heat treatment for 10 to 120 minutes may be performed at a temperature of 60 to 120 ° C. Further, a surface treatment layer by chlorination treatment or coating treatment may be formed on the inner and / or outer surface of the laminate.
- the polymer latex is brought into contact with the polymer latex adhered to the fiber base material.
- the polymer in the polymer latex coagulates without penetrating through the fibers of the fiber base material, and the polymer layer is formed on the fiber base material. Is obtained. Therefore, according to the production method of the present invention, it is possible to more effectively prevent the polymer layer from being broken through during the production of the laminate, and the occurrence of defects due to the breakthrough is suppressed, producing a laminate.
- the sex can be further improved.
- the comfort when the obtained protective gloves are actually worn is further improved.
- a method for producing a laminate a method of obtaining a laminate by first immersing a fiber substrate in a coagulant solution and then attaching a polymer latex to the fiber substrate is known.
- the fiber base material since the fiber base material is excessively contacted with the coagulant solution by immersing the fiber base material in the coagulant solution, the fiber base material may be deteriorated.
- the types of fiber base materials that can be used and the types of coagulants have been limited.
- the polymer latex is first attached to the fiber substrate, and then the coagulant solution is brought into contact with the polymer latex attached to the fiber substrate. Without excessive contact with the coagulant solution, which allows more types of fiber substrates and coagulants to be applied.
- the laminate obtained by the production method of the present invention is in a state in which a part of the polymer layer has moderately penetrated into the fiber base material, thereby improving durability and flexibility.
- the thickness t 1 of the osmotic polymer layer and the thickness t 2 of the surface polymer layer For the laminates produced in the examples and comparative examples, the cross section in which the polymer layer of the palm portion of 12 cm from the tip of the middle finger was laminated was observed using an optical microscope (VHX-200, manufactured by Keyence Corporation). The thickness t 1 of the osmotic polymer layer and the thickness t 2 of the surface polymer layer were measured. A specific measurement method will be described with reference to FIG. 1.
- the thickness t 1 of the osmotic polymer layer is measured by measuring the distance from the surface of the fiber substrate to the deepest portion of the osmotic polymer at 10 points. It calculated
- the laminates produced in the demolding examples and comparative examples were evaluated according to the following criteria as to whether or not they could be easily detached when peeled from the metal glove mold during the production of the laminate. 3: Desorption was possible within 10 seconds. 2: Desorption was possible within 5 minutes. 1: Desorption was not possible.
- the area of the polymer layer reaching the back surface is 5% or less of the entire back surface.
- the area of the polymer layer reaching the back surface is more than 5% and less than 20% of the entire back surface.
- the area of the polymer layer reaching the back surface is 20% or more of the entire back surface.
- the gloves manufactured in the flexible example and the comparative example were each worn by 10 people and evaluated according to the following evaluation criteria. 3: Soft 2: Hard 1: Very hard
- Example 1 Preparation of latex composition for dip molding
- latex of nitrile rubber (a1) (trade name “Nipol LX550L”, manufactured by Nippon Zeon Co., Ltd., acrylonitrile unit, 1,3-butadiene unit, and ethylenically unsaturated acid monomer Nitrile rubber latex containing monomer units) is prepared, and colloidal sulfur (manufactured by Hosoi Chemical Co., Ltd.) 1.0 in terms of solid content with respect to 100 parts of nitrile rubber in the latex of nitrile rubber (a1).
- colloidal sulfur manufactured by Hosoi Chemical Co., Ltd.
- the viscosity measured under a condition of a temperature of 25 ° C. and a solid content concentration of 45% by weight and a rotational speed of 10 rpm by a B-type viscometer was 10,000 mPa ⁇ s. .
- coagulant solution A coagulant solution was obtained by mixing 20 parts of calcium nitrate and 80 parts of water.
- the latex composition for dip molding obtained above was adjusted to 25 ° C., and then a glove-shaped fiber substrate (material: cotton, substrate layer average thickness d of fiber substrate) : 650 ⁇ m, linear density: 300 denier) was immersed in a latex composition for dip molding adjusted to 25 ° C. for 5 seconds, pulled up from the latex composition for dip molding, and then at a temperature of 30 ° C. Dried for 30 minutes. Thereafter, the metal glove mold was immersed in the above-mentioned coagulant solution for 5 seconds, pulled up from the coagulant solution, and then dried at a temperature of 30 ° C. for 1 minute to form a polymer layer on the fiber substrate. .
- the nitrile rubber in the polymer layer was subjected to a crosslinking treatment by performing a heat treatment at a temperature of 125 ° C. for 60 minutes.
- the laminated body (protective glove) was obtained by peeling the fiber base material in which the polymer layer was formed from metal glove molds.
- the thickness t 1 of osmopolymers layer, and the thickness was measured t 2 of the surface polymer layer, demolding property, strike through, durability (peeling resistance), durability
- the properties (cutting resistance) and flexibility were evaluated. The results are shown in Table 1.
- the thickness t 1 of the resultant osmopolymers layer based on the value of the thickness t 2 of the surface polymer layer, (the thickness t 1 / substrate layer average thickness of osmopolymer layer d) And the result of calculating the ratio of (the thickness t 2 of the surface polymer layer / the thickness t 1 of the osmotic polymer layer) was also shown (the same applies to Examples 2 to 7 and Comparative Examples 1 to 4 described later). .
- Example 2 The viscosity of the latex composition for dip molding was changed by changing the addition ratio of the thickener added before the aging of the latex composition to 0.2% by weight and the addition ratio of the thickener added after the aging to 0.1% by weight.
- a laminate (protective glove) was obtained and evaluated in the same manner as in Example 1 except that (viscosity at 25 ° C. and solid content concentration of 45% by weight) was adjusted to 5,400 mPa ⁇ s. The results are shown in Table 1.
- Example 3 The viscosity of the latex composition for dip molding was changed by changing the addition ratio of the thickener added before aging of the latex composition to 0.15 wt% and the addition ratio of the thickener added after aging to 0.05 wt%.
- a laminate (protective glove) was obtained and evaluated in the same manner as in Example 2 except that (viscosity at 25 ° C. and a solid content concentration of 45% by weight) was adjusted to 1,200 mPa ⁇ s. The results are shown in Table 1.
- Example 4 As a thickener, polyvinyl pyrrolidone (PVP) is used instead of polyvinyl alcohol (PVA), and the addition ratio of the thickener added before aging the latex composition is 0.2% by weight and added after aging. Except for changing the addition ratio of the thickener to 0.5% by weight and adjusting the viscosity of the dip molding latex composition (25 ° C., viscosity of 45% by weight of solid content) to 2,500 mPa ⁇ s. In the same manner as in Example 2, a laminate (protective glove) was obtained and evaluated in the same manner. The results are shown in Table 1.
- PVP polyvinyl pyrrolidone
- PVA polyvinyl alcohol
- Comparative Example 1 As a thickener, carboxymethylcellulose (CMC) is used instead of polyvinyl alcohol (PVA), and the addition ratio of the thickener added before aging of the latex composition is 0.2% by weight and added after aging. Implemented except that the addition ratio of the thickener was changed to 0.4% by weight, and the viscosity of the dip-molding latex composition (25 ° C., viscosity of 45% solids concentration) was adjusted to 5,500 mPa ⁇ s. In the same manner as in Example 1, a laminate (protective glove) was obtained and evaluated in the same manner. The results are shown in Table 1.
- CMC carboxymethylcellulose
- PVA polyvinyl alcohol
- Comparative Example 2 As the thickener, sodium polyacrylate (PAA) is used instead of polyvinyl alcohol (PVA), and the addition ratio of the thickener added before aging the latex composition is 0.05% by weight after aging. Except for changing the addition ratio of the thickener to be added to 0.1% by weight and adjusting the viscosity of the dip molding latex composition (25 ° C., viscosity of 45% by weight of solid content) to 5,800 mPa ⁇ s. In the same manner as in Example 1, a laminate (protective glove) was obtained and evaluated in the same manner. The results are shown in Table 1.
- Comparative Example 3 A fiber base material similar to that used in Example 1 was prepared, and a metal glove mold covered with the prepared fiber base material was immersed in the above-mentioned coagulant solution for 5 seconds and pulled up from the coagulant solution. Drying was performed at a temperature of 30 ° C. for 1 minute. Thereafter, the metal glove mold was immersed in the same dip-forming latex composition as used in Example 1 for 5 seconds, pulled up from the dip-forming latex composition, and then at a temperature of 30 ° C. for 30 minutes. It was made to dry and the polymer layer was formed on the fiber base material. Thereafter, the nitrile rubber in the polymer layer was subjected to a crosslinking treatment by performing a heat treatment at a temperature of 125 ° C. for 60 minutes. Subsequently, the laminated body (protective glove) was obtained by peeling the fiber base material in which the polymer layer was formed from metal glove molds. The obtained laminate was evaluated in the same manner as in Example 1. The results are shown in Table 1.
- Viscosity of the latex composition for dip molding was changed by changing the addition ratio of the thickener added before the aging of the latex composition to 0.05 wt% and the addition ratio of the thickener added after the aging to 0.02 wt%.
- a laminate (protective glove) was obtained and evaluated in the same manner as in Example 2 except that (viscosity at 25 ° C. and a solid content concentration of 45% by weight) was adjusted to 500 mPa ⁇ s. The results are shown in Table 1.
- the laminate in which the ratio of (thickness t 1 of the penetrating polymer layer / average thickness d of the base material layer) and the thickness t 2 of the surface polymer layer were controlled within the predetermined range of the present invention Both have excellent productivity due to good demolding results, and also have excellent comfort during wearing due to good results of back-through, as well as durability and flexibility. Excellent (Examples 1 to 4).
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Gloves (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Laminated Bodies (AREA)
Abstract
Description
本発明の積層体において、前記重合体ラテックス中における、前記ノニオン性水溶性高分子の含有割合が、0.1~5.0重量%であることが好ましい。
本発明の積層体において、前記ノニオン性水溶性高分子が、ポリビニルアルコールおよび/またはポリビニルピロリドンであることが好ましい。
本発明の積層体において、前記重合体ラテックスを構成する重合体がニトリルゴムであることが好ましい。
本発明の積層体において、前記ニトリルゴムが、エチレン性不飽和ニトリル単量体単位、共役ジエン単量体単位、およびエチレン性不飽和酸単量体単位を含有するものであることが好ましい。
本発明の積層体の製造方法において、前記重合体ラテックスを前記繊維基材に付着させる際に、前記重合体ラテックスを、温度が25℃、固形分濃度が45重量%、および、B型粘度計を用いて測定される回転速度10rpmの条件における粘度が600~25,000mPa・sに制御された状態にて、前記重合体ラテックスを前記繊維基材に付着させることが好ましい。
乳化重合して得られるラテックスを用いる場合には、乳化重合に用いる単量体混合物の組成を調節することにより、得られる共重合体の組成を容易に調節することができるようになる。乳化重合の方法としては、従来公知の方法を採用することができる。
乳化剤の使用量は、使用する全単量体100重量部に対して、好ましくは0.5~10重量部、より好ましくは1~8重量部である。
重合開始剤の使用量は、使用する全単量体100重量部に対して、好ましくは0.01~2重量部、より好ましくは0.05~1.5重量部である。
分子量調整剤の使用量は、その種類によって異なるが、使用する全単量体100重量部に対して、好ましくは0.1~1.5重量部、より好ましくは0.2~1.0重量部である。
また、各単量体は、使用する各種単量体を予め混合してから反応容器に添加しても、あるいは別々に反応容器に添加してもよい。
重合停止剤の使用量は、特に限定されないが、通常、使用する全単量体100重量部に対して、0.05~2重量部である。
架橋促進剤の使用量は、重合体ラテックス中の全固形分100重量部に対して、好ましくは0.1~10重量部、より好ましくは0.5~5重量部である。
本発明で用いる凝固剤溶液は、溶媒中に凝固剤を溶解または分散させてなるものである。
これらの金属塩の具体例としては、硝酸カルシウム、硝酸バリウム、硝酸亜鉛等の硝酸塩;塩化バリウム、塩化カルシウム、塩化マグネシウム、塩化亜鉛、塩化アルミニウム等のハロゲン化金属塩;酢酸バリウム、酢酸カルシウム、酢酸亜鉛等の酢酸塩;硫酸カルシウム、硫酸マグネシウム、硫酸アルミニウム等の硫酸塩;等が挙げられ、これらの中でも、硝酸塩およびハロゲン化金属塩が好ましく、硝酸カルシウムおよび塩化カルシウムがより好ましく、硝酸カルシウムが特に好ましい。
これらの金属塩は、単独または2種以上組み合わせて用いることができる。
本発明の製造方法は、上記した重合体ラテックスを繊維基材に付着させるラテックス付着工程と、繊維基材に付着させた重合体ラテックスに、凝固剤溶液を接触させて重合体ラテックス中の重合体を凝固させることで、重合体層を形成する凝固工程と、を備える。この際に、本発明の製造方法においては、重合体ラテックスを繊維基材に付着させる際に、重合体ラテックスの粘度を、B型粘度計を用いて測定される回転速度10rpmの条件における粘度で、600~25,000mPa・sの範囲に制御した状態にて、重合体ラテックスを繊維基材に付着させるものである。この際における、重合体ラテックスの粘度は、より好ましくは800~20,000mPa・s、さらに好ましくは900~15,000mPa・s、特に好ましくは1,000~12,000mPa・sである。なお、重合体ラテックスを、繊維基材に付着させる際における、重合体ラテックスの温度および固形分濃度は特に限定されず、B型粘度計を用いて測定される回転速度10rpmの条件における粘度が上記範囲となるように制御すればよいが、好ましくは温度20~40℃、固形分濃度30~50重量%に制御した状態、特に、温度25℃、固形分濃度45重量%に制御した状態にて、重合体ラテックスを繊維基材に付着させることが好ましい。
実施例および比較例で製造した積層体について、中指の先から12cmの掌部分の重合体層が積層された断面を、光学顕微鏡(キーエンス社製、VHX-200)を用いて観察することで、浸透重合体層の厚みt1、および表面重合体層の厚みt2を測定した。具体的な測定方法について図1を参照して説明すると、浸透重合体層の厚みt1は、繊維基材の表面から、浸透した重合体の最深部までの距離を、10カ所測定し、測定結果の数平均値を算出することにより求めた。また、表面重合体層の厚みt2は、繊維基材の表面から、重合体層の表面までの距離を、10カ所測定し、測定結果の数平均値を算出することにより求めた。
実施例および比較例で製造した積層体について、積層体の製造中に、金属製手袋型から剥がす際に、容易に脱着することができたか否かを、以下の基準で評価した。
3:10秒以内に脱着できた。
2:5分以内に脱着できた。
1:脱着できなかった。
実施例および比較例で製造した積層体について、繊維基材に浸透した重合体層が繊維基材の裏面まで到達しているか否かを目視にて確認し、以下の基準で評価した。
3:裏面に到達している重合体層の面積が裏面全体の5%以下。
2:裏面に到達している重合体層の面積が裏面全体の5%超、20%未満。
1:裏面に到達している重合体層の面積が裏面全体の20%以上。
実施例および比較例で製造した積層体について、重合体層と繊維基材との剥離を意図的に試み、以下の基準で評価した。
2:重合体層と繊維基材とを人力では容易に剥離できなかった。もしくは剥離できても重合体層と繊維基材とを分離させることができなかった。
1:重合体層と繊維基材とを人力で容易に剥離でき、重合体層と繊維基材とを分離させることができた。
実施例および比較例で製造した積層体について、長さ3cmの未使用カッター刃を積層体の重合体層側に水平に2.5kgfの力で3秒間押し当てた後、カッター刃が当たっていた部分の積層体を目視観察し、以下の基準で評価した。
2:重合体層の一部が切れずに残った。
1:重合体層がすべて切れた。
実施例および比較例で製造した手袋を10人にそれぞれ着用してもらい下記の評価基準で評価した。
3:柔らかい
2:硬い
1:非常に硬い
ディップ成形用ラテックス組成物の調製
重合体ラテックスとして、ニトリルゴム(a1)のラテックス(商品名「Nipol LX550L」、日本ゼオン社製、アクリロニトリル単位、1,3-ブタジエン単位、およびエチレン性不飽和酸単量体単位を含有するニトリルゴムのラテックス)を準備し、ニトリルゴム(a1)のラテックス中のニトリルゴム100部に対して、それぞれ固形分換算で、コロイド硫黄(細井化学工業社製)1.0部、ジブチルジチオカルバミン酸亜鉛(大内新興化学工業社製)0.5部、酸化亜鉛2.0部となるように、各配合剤の水分散液を調製し、調製した水分散液を添加し、ラテックス組成物を得た。なお、添加の際には、ラテックスを撹拌した状態で、各配合剤の水分散液を所定の量ゆっくり添加した。その後、ラテックス組成物の固形分濃度を調整し、ラテックス組成物に対して、増粘剤としてポリビニルアルコール(PVA)0.2重量%を添加し、次いで、温度30℃、48時間の条件で、熟成(前加硫ともいう。)を施した。そして、熟成後のラテックス組成物に対して、増粘剤としてポリビニルアルコール0.18重量%をさらに添加し、固形分濃度が45重量%であるディップ成形用ラテックス組成物を得た。得られたディップ成形用ラテックス組成物における、温度25℃かつ固形分濃度45重量%の条件下、B型粘度計による回転数10rpmの条件で測定される粘度は、10,000mPa・sであった。
硝酸カルシウム20部、および水80部を混合することで、凝固剤溶液を得た。
上記にて得られたディップ成形用ラテックス組成物を25℃に調整し、次いで、手袋形状の繊維基材(材質:綿、繊維基材の基材層平均厚みd:650μm、線密度:300デニール)を被せた金属製手袋型を、25℃に調整したディップ成形用ラテックス組成物に5秒間浸漬し、ディップ成形用ラテックス組成物から引き上げた後、温度30℃、30分間の条件で乾燥させた。その後、金属製手袋型を、上記の凝固剤溶液に5秒間浸漬し、凝固剤溶液から引き上げた後、温度30℃、1分間の条件で乾燥させ、繊維基材上に重合体層を形成した。その後、温度125℃、60分間の条件で熱処理を行う事で、重合体層中のニトリルゴムに架橋処理を施した。次いで、重合体層が形成された繊維基材を金属製手袋型から剥がすことで、積層体(保護手袋)を得た。得られた積層体について、上述した方法に従い、浸透重合体層の厚みt1、および表面重合体層の厚みt2を測定し、脱型性、裏抜け、耐久性(耐剥離性)、耐久性(耐切創性)および柔軟性の評価を行った。結果を表1に示す。なお、表1においては、得られた浸透重合体層の厚みt1、表面重合体層の厚みt2の値に基づいて、(浸透重合体層の厚みt1/基材層平均厚みd)の比、および(表面重合体層の厚みt2/浸透重合体層の厚みt1)の比を計算した結果も示した(後述する実施例2~7および比較例1~4についても同様)。
ラテックス組成物の熟成前に添加する増粘剤の添加割合を0.2重量%、熟成後に添加する増粘剤の添加割合を0.1重量%に変更し、ディップ成形用ラテックス組成物の粘度(25℃、固形分濃度45重量%の粘度)を5,400mPa・sに調整した以外は、実施例1と同様にして、積層体(保護手袋)を得て、同様に評価を行った。結果を表1に示す。
ラテックス組成物の熟成前に添加する増粘剤の添加割合を0.15重量%、熟成後に添加する増粘剤の添加割合を0.05重量%に変更し、ディップ成形用ラテックス組成物の粘度(25℃、固形分濃度45重量%の粘度)を1,200mPa・sに調整した以外は、実施例2と同様にして、積層体(保護手袋)を得て、同様に評価を行った。結果を表1に示す。
増粘剤として、ポリビニルアルコール(PVA)に代えてポリビニルピロリドン(PVP)を使用し、かつ、ラテックス組成物の熟成前に添加する増粘剤の添加割合を0.2重量%、熟成後に添加する増粘剤の添加割合を0.5重量%に変更し、ディップ成形用ラテックス組成物の粘度(25℃、固形分濃度45重量%の粘度)を2,500mPa・sに調整した以外は、実施例2と同様にして、積層体(保護手袋)を得て、同様に評価を行った。結果を表1に示す。
増粘剤として、ポリビニルアルコール(PVA)に代えてカルボキシメチルセルロース(CMC)を使用し、かつ、ラテックス組成物の熟成前に添加する増粘剤の添加割合を0.2重量%、熟成後に添加する増粘剤の添加割合を0.4重量%に変更し、ディップ成形用ラテックス組成物の粘度(25℃、固形分濃度45重量%の粘度)を5,500mPa・sに調整した以外は、実施例1と同様にして、積層体(保護手袋)を得て、同様に評価を行った。結果を表1に示す。
増粘剤として、ポリビニルアルコール(PVA)に代えてポリアクリル酸ナトリウム(PAA)を使用し、かつ、ラテックス組成物の熟成前に添加する増粘剤の添加割合を0.05重量%、熟成後に添加する増粘剤の添加割合を0.1重量%に変更し、ディップ成形用ラテックス組成物の粘度(25℃、固形分濃度45重量%の粘度)を5,800mPa・sに調整した以外は、実施例1と同様にして、積層体(保護手袋)を得て、同様に評価を行った。結果を表1に示す。
実施例1で用いたものと同様の繊維基材を準備し、準備した繊維基材を被せた金属製手袋型を、上記の凝固剤溶液に5秒間浸漬し、凝固剤溶液から引き上げた後、温度30℃、1分間の条件で乾燥させた。その後、金属製手袋型を、実施例1で用いたものと同様のディップ成形用ラテックス組成物に5秒間浸漬し、ディップ成形用ラテックス組成物から引き上げた後、温度30℃、30分間の条件で乾燥させ、繊維基材上に重合体層を形成した。その後、温度125℃、60分間の条件で熱処理を行う事で、重合体層中のニトリルゴムに架橋処理を施した。次いで、重合体層が形成された繊維基材を金属製手袋型から剥がすことで、積層体(保護手袋)を得た。得られた積層体について、実施例1と同様に評価した。結果を表1に示す。
ラテックス組成物の熟成前に添加する増粘剤の添加割合を0.05重量%、熟成後に添加する増粘剤の添加割合を0.02重量%に変更し、ディップ成形用ラテックス組成物の粘度(25℃、固形分濃度45重量%の粘度)を500mPa・sに調整した以外は、実施例2と同様にして、積層体(保護手袋)を得て、同様に評価を行った。結果を表1に示す。
また、(浸透重合体層の厚みt1/基材層平均厚みd)の比が小さすぎる場合には、得られる積層体は、耐久性に劣るものであった(比較例3)。
さらに、表面重合体層の厚みt2が薄すぎる場合には、得られる積層体は、脱型性の結果が不良であることから生産性に劣り、また、裏抜けの結果が不良であることから装着時の快適性にも劣り、しかも、耐久性にも劣るものであった(比較例4)。
Claims (9)
- 複数の繊維から構成される繊維基材と、重合体ラテックスから形成される重合体層とが積層されてなる積層体であって、
前記重合体層は、一部が、前記繊維の間に浸透した状態で前記繊維基材を被覆しており、
前記重合体層のうち、前記繊維の間に浸透した部分である浸透重合体層の、前記繊維基材の表面からの厚みをt1[μm]とし、前記繊維基材の基材層平均厚みをd[μm]とした場合に、前記基材層平均厚みdに対する前記浸透重合体層の厚みt1の比(t1/d)が、0.1~0.95であり、
前記重合体層のうち、前記繊維基材の表面を被覆する部分である表面重合体層の、前記繊維基材の表面からの厚みをt2[μm]とした場合に、前記表面重合体層の厚みt2[μm]が、80μm以上である積層体。 - 前記重合体ラテックスが、増粘剤としてノニオン性水溶性高分子を含有する請求項1に記載の積層体。
- 前記重合体ラテックス中における、前記ノニオン性水溶性高分子の含有割合が、0.1~5.0重量%である請求項2に記載の積層体。
- 前記ノニオン性水溶性高分子が、ポリビニルアルコールおよび/またはポリビニルピロリドンである請求項2または3に記載の積層体。
- 前記重合体ラテックスを構成する重合体がニトリルゴムである請求項1~4のいずれかに記載の積層体。
- 前記ニトリルゴムが、エチレン性不飽和ニトリル単量体単位、共役ジエン単量体単位、およびエチレン性不飽和酸単量体単位を含有する請求項5に記載の積層体。
- 請求項1~6のいずれかに記載の積層体を備える保護手袋。
- 請求項1~6のいずれかに記載の積層体の製造方法であって、
前記重合体ラテックスを、前記繊維基材に付着させるラテックス付着工程と、
前記繊維基材に付着させた前記重合体ラテックスに、凝固剤溶液を接触させて前記重合体ラテックス中の重合体を凝固させることで、前記重合体層を形成する凝固工程と、を備え、
前記重合体ラテックスを前記繊維基材に付着させる際に、前記重合体ラテックスの粘度を、B型粘度計を用いて測定される回転速度10rpmの条件における粘度で、600~25,000mPa・sの範囲に制御した状態にて、前記重合体ラテックスを前記繊維基材に付着させる積層体の製造方法。 - 前記重合体ラテックスを前記繊維基材に付着させる際に、前記重合体ラテックスを、温度が25℃、固形分濃度が45重量%、および、B型粘度計を用いて測定される回転速度10rpmの条件における粘度が600~25,000mPa・sに制御された状態にて、前記重合体ラテックスを前記繊維基材に付着させる請求項8に記載の積層体の製造方法。
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US16/476,795 US11305518B2 (en) | 2017-01-13 | 2018-01-12 | Laminate |
KR1020197020262A KR20190105009A (ko) | 2017-01-13 | 2018-01-12 | 적층체 |
EP18738939.0A EP3575083A4 (en) | 2017-01-13 | 2018-01-12 | LAMINATE |
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US20190375199A1 (en) | 2019-12-12 |
JP7095601B2 (ja) | 2022-07-05 |
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