CN109642389A - 层叠体的制造方法 - Google Patents
层叠体的制造方法 Download PDFInfo
- Publication number
- CN109642389A CN109642389A CN201780051746.7A CN201780051746A CN109642389A CN 109642389 A CN109642389 A CN 109642389A CN 201780051746 A CN201780051746 A CN 201780051746A CN 109642389 A CN109642389 A CN 109642389A
- Authority
- CN
- China
- Prior art keywords
- base material
- fiber base
- laminated body
- polymeric layer
- polymer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 43
- 229920000642 polymer Polymers 0.000 claims abstract description 142
- 239000000835 fiber Substances 0.000 claims abstract description 138
- 239000000463 material Substances 0.000 claims abstract description 126
- 239000013047 polymeric layer Substances 0.000 claims abstract description 90
- 239000000839 emulsion Substances 0.000 claims abstract description 81
- 239000000701 coagulant Substances 0.000 claims abstract description 76
- 238000000034 method Methods 0.000 claims abstract description 38
- 229910052751 metal Inorganic materials 0.000 claims abstract description 35
- 239000002184 metal Substances 0.000 claims abstract description 35
- 150000003839 salts Chemical class 0.000 claims abstract description 31
- 150000007524 organic acids Chemical class 0.000 claims abstract description 30
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 238000007711 solidification Methods 0.000 claims abstract description 15
- 230000008023 solidification Effects 0.000 claims abstract description 15
- 229920000459 Nitrile rubber Polymers 0.000 claims abstract description 12
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 6
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 claims abstract description 4
- 125000003396 thiol group Chemical class [H]S* 0.000 claims abstract 2
- 239000010410 layer Substances 0.000 claims description 35
- 230000004224 protection Effects 0.000 claims description 28
- 239000004908 Emulsion polymer Substances 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000002585 base Substances 0.000 description 118
- 239000000243 solution Substances 0.000 description 85
- 239000000178 monomer Substances 0.000 description 67
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 42
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 33
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- -1 hair Substances 0.000 description 25
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 24
- 239000003431 cross linking reagent Substances 0.000 description 23
- 239000000203 mixture Substances 0.000 description 23
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- 230000000052 comparative effect Effects 0.000 description 17
- 238000005299 abrasion Methods 0.000 description 16
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 14
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- 239000003795 chemical substances by application Substances 0.000 description 13
- 150000001993 dienes Chemical class 0.000 description 13
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 12
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- 238000006243 chemical reaction Methods 0.000 description 11
- 238000004132 cross linking Methods 0.000 description 11
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- 150000002825 nitriles Chemical class 0.000 description 10
- 239000007788 liquid Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 7
- 239000000654 additive Substances 0.000 description 7
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- 239000011787 zinc oxide Substances 0.000 description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
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- 238000010438 heat treatment Methods 0.000 description 5
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- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 5
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
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- 239000003995 emulsifying agent Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
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- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 239000005060 rubber Substances 0.000 description 4
- 239000004034 viscosity adjusting agent Substances 0.000 description 4
- 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 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- 229920006037 cross link polymer Polymers 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- 239000003505 polymerization initiator Substances 0.000 description 3
- 235000019260 propionic acid Nutrition 0.000 description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- SBYMUDUGTIKLCR-UHFFFAOYSA-N 2-chloroethenylbenzene Chemical compound ClC=CC1=CC=CC=C1 SBYMUDUGTIKLCR-UHFFFAOYSA-N 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
- 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 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
- GUUVPOWQJOLRAS-UHFFFAOYSA-N Diphenyl disulfide Chemical compound C=1C=CC=CC=1SSC1=CC=CC=C1 GUUVPOWQJOLRAS-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-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
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
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- 125000001931 aliphatic group Chemical group 0.000 description 2
- 150000004996 alkyl benzenes Chemical class 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
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- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 2
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- 239000002270 dispersing agent Substances 0.000 description 2
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- 239000011777 magnesium Substances 0.000 description 2
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- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
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- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 2
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- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 1
- RIVJYLGQARVCBI-UHFFFAOYSA-N 2-tert-butylperoxy-2-methylpropane;cumene Chemical compound CC(C)C1=CC=CC=C1.CC(C)(C)OOC(C)(C)C RIVJYLGQARVCBI-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供了一种层叠体的制造方法,具有以下工序:使凝固剂溶液附着于纤维基材的凝固剂附着工序;以及使附着了上述凝固剂溶液的上述纤维基材与聚合物胶乳接触而使聚合物凝固由此在上述纤维基材上形成聚合物层的凝固工序,作为上述凝固剂溶液,使用在溶剂中溶解或分散了0.2~7.0重量%的作为凝固剂的金属盐和0.1~7.0重量%的有机酸而成的凝固剂溶液。在本发明的层叠体的制造方法中,优选上述金属盐为多价金属盐。在本发明的层叠体的制造方法中,优选上述有机酸为具有羧基、磺基、羟基、硫醇基的至少一种基团的有机酸。在本发明的层叠体的制造方法中,优选构成上述聚合物胶乳的聚合物为腈橡胶。
Description
技术领域
本发明涉及在纤维基材上形成聚合物层而成的层叠体的制造方法。此外,本发明涉及使用上述层叠体的保护手套的制造方法。
背景技术
一直以来,在工厂的制造作业、轻工作业、施工作业、农业作业等各种用途中,通过用橡胶、树脂等覆盖纤维制手套,从而使得提高了耐溶剂性、抓握性、耐磨耗性等的保护手套用作作业用手套。
例如,专利文献1公开了至少在手腕部编入伸缩性丝线、在该伸缩性丝线上覆盖橡胶或树脂而形成的保护手套。然而,通过专利文献1的技术得到的保护手套由于伸缩性丝线上覆盖的橡胶或树脂的影响,存在在用作作业用手套的情况下的柔软性不充分这一问题。
现有技术文献
专利文献
专利文献1:日本特开2014-111853号公报。
发明内容
发明要解决的问题
本发明是鉴于这样的实际情况而完成的,目的在于提供一种柔软性和耐磨耗性优异的层叠体的制造方法。此外,本发明的目的在于提供使用通过这样的制造方法而得到的层叠体的保护手套的制造方法。
用于解决问题的方案
本发明人等为了实现上述目的而进行了深入研究,结果发现,在制造通过使纤维基材与聚合物胶乳接触而使聚合物凝固来形成聚合物层而成的层叠体时,作为用于使聚合物胶乳的聚合物凝固的凝固剂溶液,通过使用在溶剂中分别以规定的比例溶解或分散了作为凝固剂的金属盐和有机酸而成的凝固剂溶液,从而能够实现上述目的,以至完成了本发明。
即,根据本发明,可提供层叠体的制造方法,其具有以下工序:使凝固剂溶液附着于纤维基材的凝固剂溶液附着工序;以及使附着了上述凝固剂溶液的上述纤维基材与聚合物胶乳接触而使聚合物凝固由此在上述纤维基材上形成聚合物层的凝固工序,作为上述凝固剂溶液,使用在溶剂中溶解或分散了0.2~7.0重量%的作为凝固剂的金属盐和0.1~7.0重量%的有机酸而成的凝固剂溶液。
在本发明的层叠体的制造方法中,优选上述金属盐为多元金属盐。
在本发明的层叠体的制造方法中,优选上述有机酸为具有羧基、磺基、羟基、硫醇基的至少一种基团的有机酸。
在本发明的层叠体的制造方法中,优选构成上述聚合物胶乳的聚合物为腈橡胶。
此外,根据本发明可以提供使用通过上述的制造方法而得到的层叠体的保护手套的制造方法。
发明效果
根据本发明,能够提供柔软性和耐磨耗性优异的层叠体的制造方法。此外,根据本发明,能够提供使用通过这样的制造方法而得到的层叠体的保护手套的制造方法。
附图说明
图1为在纤维基材上形成聚合物层而得到的层叠体的剖面图。
具体实施方式
本发明的层叠体的制造方法的特征在于,具有以下工序:使凝固剂溶液附着于纤维基材的凝固剂溶液附着工序;以及使附着了上述凝固剂溶液的上述纤维基材与聚合物胶乳接触而使聚合物凝固由此在上述纤维基材上形成聚合物层的凝固工序,作为上述凝固剂溶液,使用在溶剂中溶解或分散了0.2~7.0重量%的作为凝固剂的金属盐和0.1~7.0重量%的有机酸而成的凝固剂溶液。
作为本发明所使用的纤维基材,只要是纤维制的基材即可,没有特别限定,能够使用棉、毛、麻、羊毛等天然纤维;聚酯、聚氨酯、腈纶、尼龙等合成纤维等作为材料,在这些中,优选使用尼龙。此外,纤维基材可以是编织的基材,也可以是缝制的基材,可以是纺织布,也可以是无纺布。
纤维基材的厚度没有特别限定,优选为0.1~2.0mm。纤维基材的线密度没有特别限定,优选为50~500旦尼尔。纤维基材的针数(gauge)没有特别限定,优选为7~18针。在此,针数是指在1英寸间的针织机的针的数量。
另外,纤维基材由于由多个纤维构成,因此特别是在纤维基材为纺织布的情况下,通常纤维折叠而存在厚度方向上的重叠度密集的部分(相互重叠的纤维的数量多的部分)和在厚度方向上的纤维的重叠度稀疏的部分(相互重叠的纤维的数量少的部分),纤维基材由包含这些部分的层(基材层)而构成。因此,纤维基材在其微观结构中,在纤维的重合度密集的部分和纤维的重合度稀疏的部分,有时其厚度会有所不同,上述纤维基材的厚度以如下方式而求出:对于纤维基材,将纤维的重叠度密集的部分的厚度作为纤维基材的厚度,求出此时厚度的平均值。
本发明所使用的凝固剂溶液是在溶剂中溶解或分散了0.2~7.0重量%的作为凝固剂的金属盐和0.1~7.0重量%的有机酸而成的凝固剂溶液。
作为用作构成凝固剂溶液的凝固剂的金属盐,只要是能够使聚合物胶乳中的聚合物凝固的金属盐即可,没有特别限定,作为金属种类,可举出锂、钠、钾等1价金属;镁、钙、锌、铁、钡、锆、铜等2价金属;铝等3价金属等。此外,作为盐种类,可举出硝酸、硫酸、盐酸等无机酸;醋酸等有机酸等。在这些中,作为金属种类优选多价金属,更优选2价金属,特别优选钙。此外,作为盐种类优选硝酸或盐酸,特别优选硝酸。即,作为金属盐优选多价金属盐,更优选2价金属的硝酸盐或者卤化盐。
作为这些金属盐的具体例子,可举出硝酸钙、硝酸钡、硝酸锌等硝酸盐;氯化钡、氯化钙、氯化镁、氯化锌、氯化铝等卤化金属盐;醋酸钡、醋酸钙、醋酸锌等醋酸盐;硫酸钙、硫酸镁、硫酸铝等硫酸盐等,在这些中,优选硝酸盐和卤化金属盐,更优选硝酸钙和氯化钙,特别优选硝酸钙。
这些金属盐能够单独使用,或组合2种以上使用。
作为构成凝固剂溶液的有机酸,没有特别限定,优选具有羧基、磺基、羟基、硫醇基的至少一种基团的有机酸。具体而言,可举出醋酸、蚁酸、丙酸、柠檬酸、草酸、抗坏血酸、苹果酸、酒石酸、丙酸、安息香酸、乳酸、葡萄糖酸、琥珀酸、富马酸、烷基苯磺酸、脂肪族磺酸、十二烷基二苯醚磺酸等,在这些中,优选醋酸、蚁酸、丙酸、柠檬酸、草酸等具有羧基的有机酸,更优选醋酸。
作为用于使作为凝固剂的金属盐和有机酸溶解或分散的溶剂,没有特别限定,能够使用水或甲醇、乙醇等醇,或者这些的混合物等,在这些中,优选醇,特别优选甲醇。
凝固剂溶液中的作为凝固剂的金属盐的浓度为0.1~7.0重量%,优选为0.1~6.0重量%,更优选为0.1~4.0重量%,进一步优选为0.1~2.0重量%。此外,凝固剂溶液中的有机酸的浓度为0.2~7.0重量%,优选为0.2~5.0重量%,更优选为0.2~3.0重量%。
而且,在本发明的制造方法中,使这样的凝固剂溶液附着于纤维基材,使附着了凝固剂溶液的纤维基材与聚合物胶乳接触而使聚合物凝固,由此在纤维基材上形成聚合物层。
具体而言,在本发明的制造方法中,使上述凝固剂溶液附着于纤维基材,使通过这样而得到的附着了凝固剂溶液的纤维基材与聚合物胶乳接触,由此聚合物胶乳的一部分浸透至纤维基材内部,并且通过聚合物胶乳中的聚合物进行凝固,从而形成聚合物层。因此,通过本发明的制造方法而得到的层叠体如图1所示,在纤维基材的表面上形成聚合物层,并且聚合物层的一部分浸透至构成纤维基材的纤维的间隙。另外,图1为表示通过本发明的制造方法而得到的层叠体的剖面图的图,在图1中,将聚合物层中浸透到纤维基材的间隙的部分示为浸透聚合物层,此外,将聚合物层中形成于纤维基材的表面上的部分示为表面聚合物层。此外,在图1中,对于纤维基材的剖面,为了容易理解而简略地表示,但实际的纤维基材的剖面并不限定于这样的形状。在图1中,构成纤维基材的纤维示例为朝向相对于纸面垂直的方向,以成为1层的方式进行排列的状态,但构成纤维基材的纤维也可以折叠而以成为2层以上的方式进行排列。构成纤维基材的纤维,可以是单纤维(从上述天然纤维、合成纤维等中取出的一根一根),也可以是由多个单纤维形成的捻线。另外,在本发明中,将聚合物层适当地作为由浸透聚合物层和表面聚合物层形成的层进行说明,但通常这些浸透聚合物层和表面聚合物层作为一体而形成。
而且,根据本发明,作为用于使聚合物胶乳的聚合物凝固的凝固剂溶液,如上所述,使用含有作为凝固剂的金属盐和有机酸且将这些作为凝固剂的金属盐和有机酸设为规定的含有比例的凝固剂溶液,由此能够在纤维基材的表面上形成某种程度的厚度的聚合物层,并且使该聚合物层的一部分适度地浸透至纤维基材,由此能够使得到的层叠体的柔软性和耐磨耗性高度平衡,从而能够优选作为例如作业用手套等保护手套。
即,在本发明中,在使附着了凝固剂溶液的纤维基材与聚合物胶乳接触时,能够通过凝固剂溶液中的有机酸的作用,从而适宜调节基于凝固剂溶液中的作为凝固剂的金属盐的作用的、聚合物胶乳中的聚合物的凝固速度,由此能够使聚合物胶乳适当地浸透到纤维基材中,且使聚合物进行凝固。而且,由此能够如图1所示在纤维基材的表面上形成某种程度的厚度的聚合物层,并且能够使该聚合物层的一部分浸透到纤维基材中,因此浸透聚合物层的厚度和表面聚合物层的厚度分别成为适度,由此,在将得到的层叠体用作作业用手套等保护手套的情况下,柔软性和耐磨耗性优异。
特别地,根据本发明,即使在增大凝固剂溶液中的作为凝固剂的金属盐的含有比例的情况下(例如,即使在将凝固剂溶液中的作为凝固剂的金属盐的含有比例设为超过0.5重量%的情况下),通过凝固剂溶液中的有机酸的作用,能够使聚合物层的一部分适宜地浸透到纤维基材中,结果通过在得到的层叠体中的聚合物层中浸透于纤维基材的部分的作用,能够有效地防止聚合物层的剥离,由此特别能够提高层叠体的耐磨耗性。
另外,当凝固剂溶液中的作为凝固剂的金属盐的含有比例过多时,聚合物胶乳中的聚合物的凝固速度上升,在聚合物胶乳充分浸透到纤维基材中之前聚合物的凝固就已进行,因此在形成的聚合物层中形成于纤维基材的表面上的表面聚合物层的厚度变得过厚,得到的层叠体的柔软性降低,并且在形成的聚合物层中浸透到纤维基材中而形成的浸透聚合物层的厚度变得过薄,聚合物层变得容易从纤维基材剥离,因此层叠体的耐磨耗性下降。另一方面,当凝固剂溶液中的作为凝固剂的金属盐的含有比例过少时,聚合物胶乳中的聚合物的凝固速度下降,聚合物胶乳过度浸透到纤维基材中,因此会发生聚合物层到达纤维基层的背面的穿透,由此层叠体的生产率下降,在将得到的层叠体用作保护手套的情况下的使用感变差。
当凝固剂溶液中的有机酸的含有比例过少时,聚合物胶乳中的聚合物的凝固速度下降,聚合物胶乳过度浸透到纤维基材中,因此会发生聚合物层到达纤维基材的背面的穿透,由此层叠体的生产率下降,在将得到的层叠体用作保护手套的情况下的使用感变差。另一方面,当在凝固剂溶液中的有机酸的含有比例过多时,聚合物胶乳中的聚合物的凝固速度上升,在聚合物胶乳充分浸透到纤维基材中之前聚合物的凝固就已进行,因此在形成的聚合物层中形成于纤维基材的表面上的表面聚合物层的厚度变得过厚,得到的层叠体的柔软性下降,并且在形成的聚合物层中浸透到纤维基材中而形成的浸透聚合物层的厚度变得过薄,聚合物层变得容易从纤维基材剥离,因此层叠体的耐磨耗性下降。
作为本发明的制造方法所使用的聚合物胶乳,没有特别限定,从能够使得到的层叠体的柔软性更优异的方面出发,优选使用含有橡胶状聚合物的聚合物作为聚合物,作为橡胶状聚合物,可举出天然橡胶;丁二烯、异戊二烯等将共轭二烯聚合或共聚而形成的共轭二烯系橡胶等,在这些中,优选共轭二烯系橡胶。作为共轭二烯系橡胶,可举出将腈基共聚而成的所谓腈橡胶、异戊二烯橡胶、苯乙烯-丁二烯橡胶、氯丁二烯橡胶等,在这些中,特别优选腈橡胶。
作为腈橡胶,没有特别限定,能够使用将α,β-烯属不饱和腈单体和根据需要而使用的能够共聚的其他单体进行共聚而成的腈橡胶。
作为α,β-烯属不饱和腈单体,没有特别限定,能够使用具有腈基且碳原子数优选为3~18的烯属不饱和化合物。作为这样的α,β-烯属不饱和腈单体,可举出例如丙烯腈、甲基丙烯腈、卤代丙烯腈等,在这些中,特别优选丙烯腈。另外,这些α,β-烯属不饱和腈单体可以单独使用1种,也可以组合2种以上使用。
腈橡胶中的α,β-烯属不饱和腈单体单元的含有比例相对于全部单体单元优选为10~45重量%,更优选为20~40重量%。通过将α,β-烯属不饱和腈单体单元的含有比例设为上述范围,从而能够使得到的层叠体的耐溶剂性提高,并且能够提高手感。
此外,作为腈橡胶,从对得到的聚合物层赋予橡胶弹性的观点出发,优选含有共轭二烯单体单元的腈橡胶。
作为形成共轭二烯单体单元的共轭二烯单体,优选1,3-丁二烯、异戊二烯、2,3-二甲基-1,3-丁二烯、1,3-戊二烯、氯丁二烯等碳原子数为4~6的共轭二烯单体,更优选1,3-丁二烯和异戊二烯,特别优选1,3-丁二烯。另外,这些共轭二烯单体可以单独使用1种,也可以组合2种以上使用。
共轭二烯单体单元的含有比例相对于构成腈橡胶的全部单体单元优选为40~80重量%,更优选为52~78重量%。通过将共轭二烯单体单元的含有比例设为上述范围,从而对于得到的层叠体,能够使其耐溶剂性提高,并且能够提高在用作保护手套的情况下的手感。
此外,腈橡胶可以包含能够与形成α,β-烯属不饱和腈单体单元的单体和形成共轭二烯单体单元的单体共聚的其他烯属不饱和酸单体。
作为这样的能够共聚的其他烯属不饱和酸单体,没有特别限定,可举出例如含羧基烯属不饱和单体、含磺酸基烯属不饱和单体、含磷酸基烯属不饱和单体等。
作为含羧基烯属不饱和单体,没有特别限定,可举出丙烯酸、甲基丙烯酸、巴豆酸等烯属不饱和单羧酸;富马酸、马来酸、衣康酸、马来酸酐、衣康酸酐等烯属不饱和多元羧酸及其酸酐;马来酸甲酯、衣康酸甲酯等烯属不饱和多元羧酸的部分酯化合物等。
作为含磺酸基烯属不饱和单体,没有特别限定,可举出乙烯基磺酸、甲基乙烯基磺酸、苯乙烯磺酸、(甲基)烯丙基磺酸、(甲基)丙烯酸-2-磺酸乙酯、2-丙烯酰胺-2-羟基丙磺酸等。
作为含磷酸基烯属不饱和单体,没有特别限定,可举出(甲基)丙烯酸-3-氯代-2-磷酸丙酯、(甲基)丙烯酸-2-磷酸乙酯、3-烯丙氧基-2-羟基丙烷磷酸等。
这些能够聚合的其他烯属不饱和酸单体也能够以碱金属盐或铵盐的形式使用,此外,可以单独使用1种,也可以组合2种以上使用。在上述能够共聚的其他烯属不饱和酸单体中,优选含羧基烯属不饱和单体,更优选烯属不饱和单羧酸,特别优选甲基丙烯酸。
在本发明所使用的构成聚合物胶乳的聚合物中的、能够共聚的其他烯属不饱和酸单体的含量相对于聚合物中的全部单体单元,优选为2~8重量%。通过将能够共聚的其他烯属不饱和酸单体单元的含量设为上述范围,从而能够使在纤维基材上形成的聚合物层的成型性优异,并且能够提高在将得到的层叠体用作保护手套的情况下的手感。
构成聚合物胶乳的聚合物除了上述的烯属不饱和腈单体单元、共轭二烯单体单元和能够共聚的其他烯属不饱和酸单体单元以外,还可以进一步含有其他单体单元。
作为形成其他单体单元的其他单体,只要是能够与共轭二烯单体、烯属不饱和腈单体单元及烯属不饱和酸单体共聚的单体即可,没有特别限定,可举出例如以下的单体。
即,作为其他单体,能够举出苯乙烯、α-甲基苯乙烯、单氯苯乙烯、二氯苯乙烯、三氯苯乙烯、单甲基苯乙烯、二甲基苯乙烯、三甲基苯乙烯、羟基甲基苯乙烯等芳香族乙烯基单体;丙烯酰胺、甲基丙烯酰胺、N,N-二甲基丙烯酰胺、N-羟甲基丙烯酰胺等烯属不饱和羧酸酰胺单体;(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸-2-乙基己酯等烯属不饱和羧酸烷基酯单体;乙酸乙烯酯、丙酸乙烯酯、叔碳酸乙烯酯等羧酸乙烯酯单体;氯乙烯、偏氯乙烯、氟乙烯、偏二氟乙烯等卤化乙烯基单体;乙烯、丙烯、1-丁烯、异丁烯等烯烃单体;甲基乙烯基醚、正丙基乙烯基醚、异丁基乙烯基醚、十二烷基乙烯基醚等乙烯基醚单体;乙酸烯丙酯、乙酸甲基烯丙酯、烯丙基氯、甲基烯丙基氯等(甲基)烯丙基化合物;乙烯基三甲氧基硅烷等乙烯基甲硅烷化合物;乙烯基吡啶、N-乙烯基吡咯烷酮等,在这些中,从能够进一步提高得到的层叠体的强度的观点出发,优选芳香族乙烯基单体。这些其他单体可以单独使用1种,也可以组合2种以上使用。
从防止聚合物层从纤维基材剥离的观点、从抑制在用作作业用手套的情况下的作业时的疲劳的观点以及从抑制在作为作业用手套而穿戴的情况下的溶剂气体透过的观点出发,构成聚合物胶乳的聚合物中的其他单体单元的含量相对于聚合物中的全部单体单元,优选为26重量%以下,更优选为10重量%以下,进一步优选为7重量%以下,特别优选为5重量%以下。
作为本发明所使用的聚合物胶乳,没有特别限定,可以是例如将含有上述单体的单体混合物进行聚合而得到的聚合物胶乳,能够使用将上述单体混合物进行乳液聚合而得到的胶乳、将对上述单体混合物进行溶液聚合而得到聚合物溶液进行转相乳化而得到的胶乳等。
在使用进行乳液聚合而得到的胶乳的情况下,能够通过调节用于乳液聚合的单体混合物的组成,从而容易地调节得到的共聚物的组成。作为乳液聚合的方法,能够采用一直以来公知的方法。
在将上述单体的混合物进行乳液聚合时,能够使用通常可使用的乳化剂、聚合引发剂、分子量调节剂等聚合辅助材料。这些聚合辅助材料的添加方法没有特别限定,可以是初期一次性添加法、分次添加法、连续添加法等任一种方法。
作为乳化剂,没有特别限定,可举出例如阴离子性表面活性剂、非离子性表面活性剂、阳离子性表面活性剂和两性表面活性剂等,在这些中,优选烷基苯磺酸盐、脂肪族磺酸盐、高级醇的硫酸酯盐、α-烯磺酸盐、烷基醚硫酸酯盐等阴离子性表面活性剂。
乳化剂的使用量相对于100重量份的所使用的全部单体,优选为0.5~10重量份,更优选为1~8重量份。
作为聚合引发剂,没有特别限定,优选自由基引发剂。作为自由基引发剂,没有特别限定,可举出例如:过硫酸钠、过硫酸钾、过硫酸铵、过磷酸钾、过氧化氢等无机过氧化物;叔丁基过氧化物、氢过氧化枯烯、对萜烷过氧化氢、二叔丁基过氧化物、过氧化叔丁基异丙苯、过氧化乙酰、过氧化异丁酰、过氧化辛酰、过氧化二苯甲酰、3,5,5-三甲基己酰基过氧化物、叔丁基过氧化异丁酸酯等有机过氧化物;偶氮双异丁腈、偶氮双-2,4-二甲基戊腈、偶氮双环己烷甲腈、偶氮双异丁酸甲酯等偶氮化合物等,在这些中,优选无机过氧化物或有机过氧化物,更优选无机过氧化物,特别优选过硫酸盐。这些聚合引发剂可以单独使用1种,也可以组合2种以上使用。
聚合引发剂的使用量相对于100重量份的所使用的全部单体,优选为0.01~2重量份,更优选为0.05~1.5重量份。
作为分子量调节剂,没有特别限定,可举出例如:α-甲基苯乙烯二聚体;叔十二烷基硫醇、正十二烷基硫醇、辛基硫醇等硫醇类;四氯化碳、二氯甲烷、二溴甲烷等卤化烃;二硫化四乙基秋兰姆、二硫化双五亚甲基秋兰姆、二硫化二异丙基黄原酸酯等含硫化合物等,在这些中,优选硫醇类、更优选叔十二烷基硫醇。这些分子量调节剂可以单独使用1种,也可以组合2种以上使用。
分子量调节剂的使用量根据其种类而不同,相对于100重量份的全部单体优选为0.1~1.5重量份,更优选为0.2~1.0重量份。
乳液聚合通常在水中进行。水的使用量相对于100重量份的所使用的全部单体,优选为80~500重量份,更优选为100~200重量份。
乳液聚合时,可以根据需要进一步使用除上述以外的聚合辅助材料。作为聚合辅助材料,可举出螯合剂、分散剂、pH调节剂、脱氧剂、粒径调节剂等,这些的种类、使用量没有特别限定。
作为单体的添加方法,可举出例如向反应容器中一次性添加使用的单体的方法、随着聚合的进行连续地或间断地添加的方法、添加单体的一部分反应至特定的转化率后将剩余的单体连续或间断地添加而聚合的方法等,可以采用任一种方法。在混合单体而连续或间断地添加的情况下,混合物的组成可以设为一定的,也可以使其变化。
此外,各单体可以在预先混合要使用的各种单体后向反应容器中添加,或者也可以分别向反应容器中添加。
进行乳液聚合时的聚合温度没有特别限定,通常为0~95℃、优选为5~70℃。聚合时间没有特别限定,通常为5~40小时左右。
按照以上的方式将单体进行乳液聚合,在达到规定的聚合转化率的时刻,冷却聚合体系,或添加聚合终止剂,终止聚合反应。终止聚合反应时的聚合转化率通常为80重量%以上,优选为90重量%以上。
聚合终止剂只要是通常在乳液聚合中所使用的聚合终止剂,则没有特别限定,作为其具体例子可举出羟胺、羟胺硫酸盐、二乙基羟胺、羟胺磺酸及其碱金属盐等羟胺化合物;二甲基二硫代氨基甲酸钠;氢醌衍生物;邻苯二酚衍生物;羟基二甲基苯硫代羧酸、羟基二乙基苯二硫代羧酸、羟基二丁基苯二硫代羧酸等芳香族羟基二硫代羧酸和它们的碱金属盐等芳香族羟基二硫代羧酸化合物等。
聚合终止剂的使用量没有特别限定,通常相对于100重量份的所使用的全部单体为0.05~2重量份。
可以在终止聚合反应后,根据期望而除去未反应的单体,调节固体成分浓度、pH。
构成聚合物胶乳的聚合物的粒子的重量平均粒径通常为30~1000nm,优选为50~500nm,更优选为70~200nm。通过将聚合物的粒子的重量平均粒径设为上述范围,从而聚合物胶乳的粘度变得适宜,聚合物胶乳的处理性提高,并且将聚合物层成型时的成型性提高,可得到具有均匀的聚合物层的层叠体。
聚合物胶乳的固体成分浓度通常为20~65重量%,优选为30~60重量%,更优选为35~55重量%。通过将该聚合物胶乳的固体成分浓度设为上述范围,从而能够提高胶乳的输送效率,并且聚合物胶乳的粘度变得适宜,聚合物胶乳的处理性提高。
聚合物胶乳的pH通常为5~13,优选为7~10,更优选为7.5~9。通过将聚合物胶乳的pH设为上述范围,从而机械稳定性提高,能够抑制聚合物胶乳在运送时的粗大凝聚物的产生,并且聚合物胶乳的粘度变得适宜,聚合物胶乳的处理性提高。
进而,本发明所使用的聚合物胶乳中能够添加交联剂、交联促进剂、氧化锌和粘度调节剂等。即,本发明所使用的聚合物胶乳可以是添加了这些的组合物(胶乳组合物)。对于以下的聚合物胶乳的说明,在使用胶乳组合物作为聚合物胶乳的情况下也相同。
作为交联剂优选使用硫系交联剂。作为硫系交联剂没有特别限定,可举出粉末硫、升华硫、沉淀硫、胶体硫、表面处理硫、不溶性硫等硫;氯化硫、二氯化硫、二硫化吗啉、二硫化烷基酚、二硫化二苯并噻唑、二硫化己内酰胺、含磷多硫化合物、高分子多硫化物等含硫化合物;二硫化四甲基秋兰姆、二甲基二硫代氨基甲酸硒、2-(4'-吗啉代二硫代)苯并噻唑等供硫性化合物等。这些交联剂可以单独使用1种,也可以组合2种以上使用。
硫系交联剂的添加量相对于100重量份的聚合物胶乳中的全部固体成分,优选为0.01~5重量份,更优选为0.05~3重量份,特别优选为0.1~2重量份。通过将硫系交联剂的添加量设为上述范围,从而对于得到的层叠体,能够使其耐溶剂性提高,并且能够提高在用作保护手套的情况下的手感。
硫系交联剂优选以使硫系交联剂分散于溶剂中的分散液的形式进行添加。通过作为分散液而添加于聚合物胶乳中,从而可得到在得到的聚合物层中的龟裂、小孔的产生和凝聚物的附着等缺陷少的层叠体。
作为硫系交联剂的分散液的制备方法没有特别限定,优选向硫系交联剂中添加溶剂,利用球磨机、珠磨机等湿式粉碎机进行粉碎搅拌的方法。
在使用硫作为硫系交联剂的情况下,优选并用交联促进剂(加硫促进剂)、氧化锌。
作为交联促进剂(加硫促进剂)没有特别限定,可举出例如:二乙基二硫代氨基甲酸、二丁基二硫代氨基甲酸、二-2-乙基己基二硫代氨基甲酸、二环己基二硫代氨基甲酸、二苯基二硫代氨基甲酸、二苄基二硫代氨基甲酸等二硫代氨基甲酸类及它们的锌盐;2-巯基苯并噻唑、2-巯基苯并噻唑锌、2-巯基噻唑啉、二苯并噻唑基·二硫化物、2-(2,4-二硝基苯基硫代)苯并噻唑、2-(N,N-二乙基硫代·氨基甲酰基硫代)苯并噻唑、2-(2,6-二甲基-4-吗啉代硫代)苯并噻唑、2-(4’-吗啉代·二硫代)苯并噻唑、4-吗啉基-2-苯并噻唑基·二硫化物、1,3-双(2-苯并噻唑基·巯基甲基)脲等,在这些中优选二乙基二硫代氨基甲酸锌、二丁基二硫代氨基甲酸锌、2-巯基苯并噻唑、2-巯基苯并噻唑锌。这些交联促进剂可以单独使用1种,也可以组合2种以上使用。
交联促进剂的使用量相对于100重量份的聚合物胶乳中的全部固体成分,优选为0.1~10重量份,更优选为0.5~5重量份。
此外,氧化锌的使用量相对于100重量份的聚合物胶乳中的全部固体成分,优选为5重量份以下,更优选为0.1~3重量份,进一步优选为0.5~2重量份。
此外,为了将聚合物胶乳的粘度设为所期望的范围,优选向聚合物胶乳中添加粘度调节剂。作为粘度调节剂没有特别限定,可举出羧甲基纤维素系增粘剂、聚羧酸系增粘剂和多糖类系增粘剂等。此外,聚合物胶乳的粘度优选为500~8000mPa·s,更优选为2500~7000mPa·s。特别地,在以胶乳组合物的状态(例如向聚合物胶乳中添加上述的交联剂、交联促进剂、氧化锌和粘度调节剂等的状态)使用聚合物胶乳的情况下,优选将这样的胶乳组合物的粘度设为上述范围。
聚合物胶乳中能够如上所述添加交联剂、交联促进剂、氧化锌和粘度调节剂等,进而能够根据需要以规定量添加抗老化剂、抗氧化剂、防腐剂、抗菌剂、湿润剂、增粘剂、分散剂、颜料、染料、填充材料、增强材料、pH调节剂等各种添加剂。
未添加交联剂的状态的聚合物胶乳的固体成分浓度优选控制在上述范围,添加了交联剂的聚合物胶乳(添加了交联剂而成的胶乳组合物)的固体成分浓度优选为5~40重量%,更优选为10~25重量%。此外,添加了交联剂的聚合物胶乳(添加了交联剂而成的胶乳组合物)的表面张力优选为25~40mN/m。
在本发明的制造方法中,首先使上述的凝固剂溶液附着于上述的纤维基材,接下来通过使附着了凝固剂溶液的纤维基材与聚合物胶乳接触而使聚合物凝固,从而在纤维基材上形成聚合物层,由此得到由纤维基材和聚合物层形成的层叠体。
作为使凝固剂溶液附着于纤维基材的方法,没有特别限定,可举出例如使纤维基材浸渍于凝固剂溶液的方法。
使纤维基材浸渍于凝固剂溶液的情况下的浸渍时间没有特别限定,优选为30~1秒,更优选为10~1秒。
此外,在使纤维基材附着凝固剂溶液时,优选使纤维基材以包覆于所期望的形状的成型用模具的状态浸渍于凝固剂溶液。
作为待包覆纤维基材的成型用模具没有特别限定,材质能够使用瓷器制、玻璃制、金属制、塑料制等各种材质。成型用模具的形状只要配合最终产品的形状设为所期望的形状即可。例如,在将层叠体用作保护手套的情况下,作为待包覆纤维基材的成型用模具,优选使用具有从手腕到指尖的形状的成形用模具等各种手套用的成型用模具。
此外,在本发明的制造方法中,优选在使凝固剂溶液附着于纤维基材后,进行干燥,由此除去凝固剂溶液中所包含的溶剂。此时的干燥温度没有特别限定,只要根据使用的溶剂进行选择即可,优选为10~80℃,更优选为15~70℃。此外,干燥时间没有特别限定,优选为600~1秒,更优选为300~5秒。
接下来,使像这样附着了凝固剂溶液的纤维基材与聚合物胶乳接触,由此使聚合物胶乳中的聚合物凝固,在纤维基材上形成聚合物层。
作为使附着了凝固剂溶液的纤维基材与聚合物胶乳接触的方法没有特别限定,可举出例如使附着了凝固剂溶液的纤维基材浸渍于聚合物胶乳的方法等。
此外,在使附着了凝固剂溶液的纤维基材浸渍于聚合物胶乳时,优选使附着了凝固剂溶液的纤维基材以包覆于所期望的形状的成型用模具的状态浸渍于聚合物胶乳。此时优选:预先将纤维基材以包覆于所期望的形状的成型用模具的状态如上述那样使纤维基材附着凝固剂溶液,然后,使附着了凝固剂溶液的纤维基材保持包覆于成型用模具的状态而浸渍于聚合物胶乳。
此外,在本发明的制造方法中,优选在使附着了凝固剂溶液的纤维基材浸渍于聚合物胶乳后,进行干燥。此时的干燥温度没有特别限定,优选10~80℃,更优选15~80℃。此外,干燥时间也没有特别限定,优选为120分钟~5秒,更优选为60分钟~10秒。
另外,在使用添加了交联剂的聚合物胶乳作为聚合物胶乳的情况下,作为聚合物胶乳可以使用预先熟成(也称为前加硫)了的聚合物胶乳。
熟成时的温度条件没有特别限定,优选为20~50℃。此外,从防止纤维基材和聚合物层的剥离的观点、从使得到的层叠体在用作保护手套的情况下的耐磨耗性提高的观点以及从抑制在将该保护手套用作作业用手套的情况下的溶剂气体透过的观点出发,熟成时的时间优选为4小时以上且120小时以下,更优选为24小时以上且72小时以下。通过将熟成时间设为上述范围,从而在得到的层叠体中,聚合物层适度地浸透到纤维基材中,由此防止纤维基材和聚合物层的剥离,得到的层叠体的耐磨耗性提高,并且能够有效地抑制在将层叠体用作保护手套的情况下的溶剂气体的透过。
进而,在使用添加了交联剂的聚合物胶乳作为聚合物胶乳的情况下,优选在使附着了凝固剂溶液的纤维基材浸渍于聚合物胶乳后,对附着了纤维基材的聚合物胶乳进行加热,由此使构成聚合物胶乳的聚合物交联。
用于交联的加热温度优选为60~160℃,更优选设为80~150℃。通过将加热温度设为上述范围,从而能够缩短交联反应所需要的时间而提高层叠体的生产率,并且能够抑制过度加热导致的聚合物的氧化劣化,提高得到的层叠体的物性。用于交联的加热时间只要根据加热温度适宜选择即可,通常为5~120分钟。
在本发明的制造方法中,如上所述那样通过使附着了凝固剂溶液的纤维基材与聚合物胶乳接触,从而聚合物胶乳的一部分浸透到纤维基材中,并且聚合物胶乳中的聚合物凝固,由此在纤维基材上形成聚合物层,得到层叠体。因此,得到的层叠体如图1所示以聚合物胶乳的聚合物的一部分浸透到纤维基材中的状态凝固而形成聚合物层,成为柔软性和耐磨耗性优异的层叠体。
另外,在本发明的制造方法中,优选在纤维基材上形成聚合物层后,将聚合物层在20~80℃的温水中浸渍0.5~60分钟左右,由此从聚合物层除去水溶性杂质(乳化剂、水溶性高分子、凝固剂等)。在使用添加了交联剂的聚合物胶乳(添加了交联剂而成的胶乳组合物)作为聚合物胶乳的情况下,使这样的聚合物层浸渍于温水的处理可以在使聚合物层的聚合物交联后进行,但从能够更高效地除去水溶性杂质的方面出发,优选在使聚合物层的聚合物交联前进行。
此外,在以纤维基材包覆于成型用模具的状态下形成聚合物层的情况下,能够通过将形成了聚合物层的纤维基材从成型用模具摘下而得到层叠体。作为从成型用模具摘下的方法,能够采用用手从成型用模具剥离,或通过水压、压缩空气的压力而剥离的方法。
将层叠体从成型用模具摘下后,也可以进一步在60~120℃的温度进行10~120分钟的加热处理(后交联工序)。此外,也可以在层叠体内侧和/或外侧的表面形成基于氯化处理、涂布处理等的表面处理层。
作为这样的通过本发明的制造方法而得到的层叠体,在构成层叠体的聚合物层中浸透到纤维基材中的部分的厚度、即在图1中所示的浸透聚合物层的厚度没有特别限定,优选为0.6~0.05mm,更优选为0.55~0.1mm,进一步优选为0.5~0.2mm。通过将浸透聚合物层的厚度设为上述范围,从而在将得到的层叠体用作保护手套的情况下的耐磨耗性更加提高。另外,由于浸透聚合物层为如图1所示那样表示的是浸透到纤维基材中的部分,因此厚度的上限为浸透到纤维基材整体中时的厚度,是与纤维基材本身的厚度相同的值。例如,在使用厚度为0.6mm的纤维基材作为纤维基材的情况下,浸透聚合物层的厚度的上限(在聚合物层浸透到纤维基材整体中的情况下的浸透聚合物层的厚度)为0.6mm。
此外,在通过本发明的制造方法而得到的层叠体中,聚合物层中未浸透纤维基材的部分的厚度、即在图1中所示的表面聚合物层的厚度没有特别限定,优选为0.6~0.05mm,更优选为0.5~0.1mm,进一步优选为0.45~0.12mm。通过将表面聚合物层的厚度设为上述范围,从而在将得到的层叠体用作保护手套的情况下的柔软性进一步提高。
在聚合物层中的浸透聚合物层和表面聚合物层的厚度的比率没有特别限定,以浸透聚合物层的厚度与表面聚合物层的厚度的比(浸透聚合物层的厚度/表面聚合物层的厚度)计,优选为5~0.2,更优选为2~0.3。通过将浸透聚合物层的厚度与表面聚合物层的厚度的比设为上述范围,从而在将得到的层叠体用作保护手套的情况下,能够使柔软性和耐磨耗性高度平衡。
此外,聚合物层整体的厚度、即浸透聚合物层和表面聚合物层的合计的厚度,没有特别限定,优选为1.0~0.05mm。
根据本发明,作为用于使聚合物胶乳的聚合物凝固的凝固剂溶液,通过如上述那样使用在溶剂中溶解或分散了0.2~7.0重量%的凝固剂和0.1~7.0重量%的有机酸而成的凝固剂溶液,从而可如图1所示那样得到在纤维基材的表面上形成某种程度的厚度的聚合物层、并且该聚合物层的一部分适度地浸透到纤维基材中的层叠体。因此,根据本发明,得到的层叠体柔软性和耐磨耗性优异,能够优选用作作业用手套,特别是优选用作家庭用、农业用、渔业用和工业用等的保护手套。
实施例
以下,举出实施例和比较例,对本发明进行更具体地说明,但本发明并不限定于该实施例。以下只要没有特别限定,“份”为重量基准。物性和特性的试验或评价方法如下所述。
表面聚合物层的厚度、浸透聚合物层的厚度和层叠体整体的厚度
对于在实施例和比较例中制造的层叠体,使用光学显微镜(KEYENCE公司制VHX-200)观察从中指指尖起12cm的手掌部分的层叠有聚合物层的剖面,测定了表面聚合物层的厚度、浸透聚合物层的厚度和层叠体整体的厚度。对于具体的测定方法,当参照图1说明时,表面聚合物层的厚度通过测定10处从纤维基材的表面至聚合物层的表面的距离、算出测定结果的数平均值而求出。此外,浸透聚合物层的厚度通过测定10处从纤维基材的表面至浸透了的聚合物的最深部分的距离、算出测定结果的数平均值而求出。进而,层叠体整体的厚度通过测定10处从聚合物层的表面至纤维基材的背面的距离、算出测定结果的数平均值而求出。
柔软性
请10个人分别穿戴在实施例和比较例中制造的手套,通过下述的评价标准进行评价。
5:非常柔软
4:柔软
3:稍微柔软
2:硬
1:非常硬
耐磨耗性
磨耗试验根据EN388所记载的方法,使用马丁代尔式磨耗试验机(STM633:SATRA公司制)而实施了评价。具体而言,对于在实施例和比较例中制造的层叠体,一边施加规定的重量,一边反复摩擦,得到了直到破损为止的摩擦次数。根据达到破损为止的摩擦次数,分为从0级到4级的级别,级别越高耐磨耗性越优异。
LEVEL 4:转速8000转
LEVEL 3:转速2000转以上且小于8000转
LEVEL 2:转速500转以上且小于2000转
LEVEL 1:转速100转以上且小于500转
LEVEL 0:转速小于100转
穿透
对于在实施例和比较例中制造的层叠体,目视确认浸透到纤维基材的聚合物层是否到达纤维基材的背面,通过以下的基准进行评价。
无:聚合物层未到达纤维基材的背面。
有:聚合物层到达了纤维基材的背面。
醋酸气味
让10个受验者穿戴在实施例和比较例中制造的层叠体,进行1小时的键盘输入操作的轻操作,计数1小时作业后感受到因醋酸的气味而导致不快的人的人数,通过以下的基准进行了评价。
无:感受到不快的人数为0人。
有:感受到不快感的人数为1人以上。
实施例1
配合剂的分散液的制备
将1.0份的胶体硫(细井化学工业公司制)、0.5份的分散剂(花王公司制,商品名“DEMOL N”)、0.0015份的5%氢氧化钾水溶液(和光纯药工业公司制)、1.0份的水在球磨机中粉碎搅拌48小时,得到固体成分浓度50重量%的分散液。
此外,对于代替上述胶体硫而使用二丁基二硫代氨基甲酸锌(大内新兴化学工业公司制,以下有时称为“ZnDBC”。)的分散液,也同样地进行了制备。进而,对于代替上述胶体硫而使用氧化锌(正同化学工业公司制)的分散液,也同样地进行了制备。
聚合物胶乳的制备
在聚合反应器中加入65份的作为共轭二烯单体的1,3-丁二烯(以下有时称为“BD”。)、30份的作为α,β-烯属不饱和腈单体的丙烯腈(以下有时称为“AN”。)、5份的作为烯属不饱和单羧酸系单体的甲基丙烯酸(以下有时称为“MAA”。)、0.4份的叔十二烷基硫醇、132份的离子交换水、3份的十二烷基苯磺酸钠、0.5份的β-萘磺酸甲醛缩合物钠盐、0.3份的过硫酸钾和0.05份的乙二胺四乙酸钠盐,将聚合温度保持在30~40℃进行聚合,使其反应直到聚合转化率到达94%为止,得到聚合物胶乳。
从得到的聚合物胶乳中除去未反应单体后,调节聚合物胶乳的pH及固体成分浓度,得到固体成分浓度40%、pH8的实施例1的浸渍成型用胶乳。
(浸渍成型用胶乳组合物的制备)
在上述的浸渍成型用胶乳中,添加10%氨水溶液,将pH调节到9.5,并且以相对于100份的浸渍成型用胶乳中的共聚物分别以固体成分换算成为1.0份的胶体硫(以上述硫分散液的形式添加)、0.5份的ZnDBC、2.0份的氧化锌的方式添加各配合剂的水分散液。另外,在添加各配合剂的水分散液时,以搅拌浸渍成型用胶乳的状态,缓慢地添加了规定的量。在添加物被均匀地混合后,添加作为粘度调节剂的Aron(东亚合成(株)制),将组合物的粘度调节至3000mPa·s,得到了浸渍成型用胶乳组合物。
凝固剂溶液的制备
将1.0重量%的作为凝固剂的硝酸钙和3.0重量%的作为有机酸的醋酸分别溶解于甲醇而形成甲醇溶液,将其作为凝固剂溶液而制备。
层叠体(保护手套)的制造
首先,对上述的浸渍成型用胶乳组合物,在温度30℃、48小时条件下实施熟成(也称为前加硫)。接下来,将手套形状的包覆了纤维基材(材质:尼龙,线密度:300旦尼尔,针数:13针,厚度:0.8mm)的陶瓷手套模具在上述的凝固剂溶液中浸渍5秒,从凝固剂溶液提起后,以温度30℃、1分钟的条件进行干燥。然后,将陶瓷手套模具在上述的浸渍成型用胶乳组合物中浸渍5秒,从浸渍成型用胶乳组合物提起后,以温度30℃、30分钟的条件进行干燥,接下来以温度70℃、10分钟的条件进行干燥,由此在纤维基材上形成聚合物层。然后,将形成了聚合物层的陶瓷手套模具在60℃的温水中浸渍90秒,从聚合物层中溶出水溶性杂质后,以温度30℃、10分钟的条件进行干燥,进而以温度125℃、30分钟的条件进行热处理,由此对聚合物层中的聚合物实施交联处理。接下来,将形成了聚合物层的纤维基材从陶瓷手套模具剥离,由此得到层叠体(保护手套)。对于得到的层叠体,按照上述的方法,进行了表面聚合物层的厚度、浸透聚合物层的厚度和层叠体整体的厚度、柔软性、耐磨耗性、穿透以及醋酸气味的评价。结果示于表1。另外,在表1中,将表面聚合物层的厚度和浸透聚合物层的厚度的合计值作为聚合物层整体的厚度而表示。
实施例2~5
代替实施例1所使用的凝固剂溶液,分别制备0.2重量%的硝酸钙和3.0重量%的醋酸的甲醇溶液(实施例2)、7.0重量%的硝酸钙和3.0重量%的醋酸的甲醇溶液(实施例3)、1.0重量%的硝酸钙和0.1重量%的醋酸的甲醇溶液(实施例4)以及1.0重量%的硝酸钙和7.0重量%的醋酸的甲醇溶液(实施例5)用作凝固剂溶液,除此以外,与实施例1同样地进行,得到层叠体(保护手套),同样地进行了评价。结果示于表1。
实施例6
代替实施例1所使用的凝固剂溶液,制备4.8重量%的硝酸钙和3.0重量%的醋酸的甲醇溶液用作凝固剂溶液,除此之外,与实施例1同样地进行,得到层叠体(保护手套),同样地进行了评价。结果示于表1。
比较例1~5
代替实施例1所使用的凝固剂溶液,分别制备仅溶解1.0重量%的硝酸钙的甲醇溶液(比较例1)、仅溶解3.0重量%的醋酸的甲醇溶液(比较例2)、仅溶解0.1重量%的硝酸钙的甲醇溶液(比较例3)、仅溶解10.0重量%的硝酸钙的甲醇溶液(比较例4)以及10.0重量%的硝酸钙和8.0重量%的醋酸的甲醇溶液(比较例5)用作凝固剂溶液,除此以外,与实施例1同样地进行,得到层叠体(保护手套),同样地进行了评价。结果示于表1。
[表1]
如表1所示,作为用于使聚合物胶乳(浸渍成型用胶乳组合物)中的聚合物凝固的凝固剂溶液,使用在溶剂中溶解或分散了0.2~7.0重量%的凝固剂和0.1~7.0重量%的有机酸而成的凝固剂溶液由此而得到的层叠体,其柔软性和耐磨耗性均优异,而且未确认出穿透和醋酸气味(实施例1~6)。
另一方面,使用即使凝固剂的含有比例为上述范围但不含有机酸的凝固剂溶液而得到的层叠体,其柔软性差(比较例1)。
使用即使有机酸的含有比例为上述范围但不含凝固剂的凝固剂溶液而得到的层叠体,其柔软性差且发生了穿透(比较例2)。
使用凝固剂的含有比例过小且不含有机酸的凝固剂溶液而得到的层叠体,其柔软性差,而且发生了穿透(比较例3)。
使用凝固剂的含有比例过大且不含有机酸的凝固剂溶液而得到的层叠体,其柔软性和耐磨耗性差(比较例4)。
使用凝固剂的含有比例和有机酸的含有比例都过大的凝固剂溶液而得到的层叠体,其耐磨耗性差,而且确认到了醋酸气味(比较例5)。
Claims (7)
1.一种层叠体的制造方法,具有以下工序:
使凝固剂溶液附着于纤维基材的凝固剂溶液附着工序;以及
使附着了所述凝固剂溶液的所述纤维基材与聚合物胶乳接触而使聚合物凝固,由此在所述纤维基材上形成聚合物层的凝固工序,
作为所述凝固剂溶液,使用在溶剂中溶解或分散了0.2~7.0重量%的作为凝固剂的金属盐和0.1~7.0重量%的有机酸而成的凝固剂溶液。
2.根据权利要求1所述的层叠体的制造方法,其中,所述金属盐为多价金属盐。
3.根据权利要求1或2所述的层叠体的制造方法,其中,所述有机酸为具有羧基、磺基、羟基、硫醇基的至少一种基团的有机酸。
4.根据权利要求1~3中任一项所述的层叠体的制造方法,其中,构成所述聚合物胶乳的聚合物为腈橡胶。
5.根据权利要求1~4中任一项所述的层叠体的制造方法,其中,在所述凝固工序中,以浸透聚合物层的厚度成为0.05~0.6mm的方式形成所述聚合物层,所述浸透聚合物层是所述聚合物层中浸透于所述纤维基材的部分。
6.根据权利要求1~5中任一项所述的层叠体的制造方法,其中,在所述凝固工序中,以表面聚合物层的厚度成为0.05~0.6mm的方式形成所述聚合物层,所述表面聚合物层是所述聚合物层中未浸透于所述纤维基材的部分。
7.一种保护手套的制造方法,使用通过权利要求1~6中的任一项所述的制造方法而得到的层叠体。
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JP2011001662A (ja) * | 2009-06-19 | 2011-01-06 | Towa Corp:Kk | 手袋及びその製造方法 |
US20150135403A1 (en) * | 2013-11-19 | 2015-05-21 | Ansell Limited | Polymer blends of nitrile rubber and polychloroprene |
US20160262469A1 (en) * | 2015-03-10 | 2016-09-15 | Ansell Limited | Supported glove having an abrasion resistant nitrile coating |
Family Cites Families (5)
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JPH105304A (ja) * | 1996-06-21 | 1998-01-13 | Koki Bussan Kk | 水不透過性手袋 |
US9061453B2 (en) * | 2009-11-02 | 2015-06-23 | Atg Ceylon (Private) Limited | Protective garments and materials therefor |
WO2013090888A1 (en) | 2011-12-16 | 2013-06-20 | Ansell Healthcare Products Llc | Latex coated high performance polyethylene fabrics |
JP6460363B2 (ja) * | 2012-10-31 | 2019-01-30 | ショーワグローブ株式会社 | 手袋 |
US10350848B2 (en) * | 2013-11-26 | 2019-07-16 | Ansell Limited | Nitrile/polyurethane polymer blends |
-
2017
- 2017-09-19 WO PCT/JP2017/033714 patent/WO2018061868A1/ja unknown
- 2017-09-19 US US16/337,104 patent/US11325356B2/en active Active
- 2017-09-19 JP JP2018542424A patent/JP6922923B2/ja active Active
- 2017-09-19 CN CN201780051746.7A patent/CN109642389B/zh active Active
- 2017-09-19 KR KR1020197012461A patent/KR20190053962A/ko not_active Application Discontinuation
- 2017-09-19 EP EP17855823.5A patent/EP3521506A4/en not_active Withdrawn
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2011001662A (ja) * | 2009-06-19 | 2011-01-06 | Towa Corp:Kk | 手袋及びその製造方法 |
US20150135403A1 (en) * | 2013-11-19 | 2015-05-21 | Ansell Limited | Polymer blends of nitrile rubber and polychloroprene |
US20160262469A1 (en) * | 2015-03-10 | 2016-09-15 | Ansell Limited | Supported glove having an abrasion resistant nitrile coating |
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KR20190053962A (ko) | 2019-05-20 |
EP3521506A4 (en) | 2020-05-13 |
US11325356B2 (en) | 2022-05-10 |
JPWO2018061868A1 (ja) | 2019-07-11 |
CN109642389B (zh) | 2021-07-09 |
JP6922923B2 (ja) | 2021-08-18 |
US20200031100A1 (en) | 2020-01-30 |
WO2018061868A1 (ja) | 2018-04-05 |
EP3521506A1 (en) | 2019-08-07 |
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