CN111676700B - 碳纤维前体用处理剂以及碳纤维前体 - Google Patents
碳纤维前体用处理剂以及碳纤维前体 Download PDFInfo
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- CN111676700B CN111676700B CN202010609295.8A CN202010609295A CN111676700B CN 111676700 B CN111676700 B CN 111676700B CN 202010609295 A CN202010609295 A CN 202010609295A CN 111676700 B CN111676700 B CN 111676700B
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- Prior art keywords
- carbon fiber
- fiber precursor
- acid
- agent
- organic
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 109
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 89
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 89
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000002243 precursor Substances 0.000 title claims abstract description 66
- -1 phosphonium sulfonates Chemical class 0.000 claims abstract description 63
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 40
- 150000003839 salts Chemical class 0.000 claims abstract description 38
- 238000009499 grossing Methods 0.000 claims abstract description 35
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 27
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 26
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 23
- QTUOYBXDUHAXBB-UHFFFAOYSA-N diphosphanium sulfate Chemical class [PH4+].[PH4+].[O-]S([O-])(=O)=O QTUOYBXDUHAXBB-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 21
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 12
- 125000004437 phosphorous atom Chemical group 0.000 claims description 9
- 125000001424 substituent group Chemical group 0.000 claims description 9
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 31
- 150000003460 sulfonic acids Chemical class 0.000 abstract description 3
- 150000004028 organic sulfates Chemical class 0.000 abstract description 2
- 238000009987 spinning Methods 0.000 description 19
- 238000011156 evaluation Methods 0.000 description 17
- 238000000034 method Methods 0.000 description 16
- 230000000694 effects Effects 0.000 description 12
- 239000002253 acid Substances 0.000 description 10
- 239000002994 raw material Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- WNWHHMBRJJOGFJ-UHFFFAOYSA-N 16-methylheptadecan-1-ol Chemical compound CC(C)CCCCCCCCCCCCCCCO WNWHHMBRJJOGFJ-UHFFFAOYSA-N 0.000 description 6
- 229920002972 Acrylic fiber Polymers 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 235000019198 oils Nutrition 0.000 description 6
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 5
- 150000007513 acids Chemical class 0.000 description 5
- 125000001931 aliphatic group Chemical group 0.000 description 5
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 5
- PKBSGDQYUYBUDY-UHFFFAOYSA-N 1-nonacosanol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCO PKBSGDQYUYBUDY-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Natural products C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 4
- ULCZGKYHRYJXAU-UHFFFAOYSA-N heptacosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCO ULCZGKYHRYJXAU-UHFFFAOYSA-N 0.000 description 4
- IRHTZOCLLONTOC-UHFFFAOYSA-N hexacosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCO IRHTZOCLLONTOC-UHFFFAOYSA-N 0.000 description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 4
- REIUXOLGHVXAEO-UHFFFAOYSA-N pentadecan-1-ol Chemical compound CCCCCCCCCCCCCCCO REIUXOLGHVXAEO-UHFFFAOYSA-N 0.000 description 4
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 description 4
- LDMOEFOXLIZJOW-UHFFFAOYSA-N 1-dodecanesulfonic acid Chemical compound CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 description 3
- XUJLWPFSUCHPQL-UHFFFAOYSA-N 11-methyldodecan-1-ol Chemical compound CC(C)CCCCCCCCCCO XUJLWPFSUCHPQL-UHFFFAOYSA-N 0.000 description 3
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 3
- HVWGGPRWKSHASF-UHFFFAOYSA-N Sulfuric acid, monooctadecyl ester Chemical compound CCCCCCCCCCCCCCCCCCOS(O)(=O)=O HVWGGPRWKSHASF-UHFFFAOYSA-N 0.000 description 3
- 125000005233 alkylalcohol group Chemical group 0.000 description 3
- 125000002947 alkylene group Chemical group 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 3
- FYAQQULBLMNGAH-UHFFFAOYSA-N hexane-1-sulfonic acid Chemical compound CCCCCCS(O)(=O)=O FYAQQULBLMNGAH-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- YPDHMBTYUUZFOA-UHFFFAOYSA-N 1,4-dibutoxy-1,4-dioxobutane-2-sulfonic acid Chemical compound CCCCOC(=O)CC(S(O)(=O)=O)C(=O)OCCCC YPDHMBTYUUZFOA-UHFFFAOYSA-N 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- KVGOXGQSTGQXDD-UHFFFAOYSA-N 1-decane-sulfonic-acid Chemical compound CCCCCCCCCCS(O)(=O)=O KVGOXGQSTGQXDD-UHFFFAOYSA-N 0.000 description 2
- NQDZCRSUOVPTII-UHFFFAOYSA-N 10-methylundecan-1-ol Chemical compound CC(C)CCCCCCCCCO NQDZCRSUOVPTII-UHFFFAOYSA-N 0.000 description 2
- XDOFQFKRPWOURC-UHFFFAOYSA-N 16-methylheptadecanoic acid Chemical compound CC(C)CCCCCCCCCCCCCCC(O)=O XDOFQFKRPWOURC-UHFFFAOYSA-N 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- UAZLASMTBCLJKO-UHFFFAOYSA-N 2-decylbenzenesulfonic acid Chemical compound CCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O UAZLASMTBCLJKO-UHFFFAOYSA-N 0.000 description 2
- LBIZZGIYNNLXQN-UHFFFAOYSA-N 2-dodecoxy-2-oxoethanesulfonic acid Chemical compound CCCCCCCCCCCCOC(=O)CS(O)(=O)=O LBIZZGIYNNLXQN-UHFFFAOYSA-N 0.000 description 2
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 2
- DHIXFTVGHROZHD-UHFFFAOYSA-N 2-ethylhexane-1-sulfonic acid Chemical compound CCCCC(CC)CS(O)(=O)=O DHIXFTVGHROZHD-UHFFFAOYSA-N 0.000 description 2
- CTIFKKWVNGEOBU-UHFFFAOYSA-N 2-hexadecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O CTIFKKWVNGEOBU-UHFFFAOYSA-N 0.000 description 2
- QQBZFCFCMKHPPC-UHFFFAOYSA-N 2-pentadecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O QQBZFCFCMKHPPC-UHFFFAOYSA-N 0.000 description 2
- PVXSFEGIHWMAOD-UHFFFAOYSA-N 2-tridecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O PVXSFEGIHWMAOD-UHFFFAOYSA-N 0.000 description 2
- ODJQKYXPKWQWNK-UHFFFAOYSA-L 3-(2-carboxylatoethylsulfanyl)propanoate Chemical compound [O-]C(=O)CCSCCC([O-])=O ODJQKYXPKWQWNK-UHFFFAOYSA-L 0.000 description 2
- UDTHXSLCACXSKA-UHFFFAOYSA-N 3-tetradecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCCCC1=CC=CC(S(O)(=O)=O)=C1 UDTHXSLCACXSKA-UHFFFAOYSA-N 0.000 description 2
- UCDCOJNNUVYFKJ-UHFFFAOYSA-N 4-undecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCC1=CC=C(S(O)(=O)=O)C=C1 UCDCOJNNUVYFKJ-UHFFFAOYSA-N 0.000 description 2
- KIWBPDUYBMNFTB-UHFFFAOYSA-N Ethyl hydrogen sulfate Chemical compound CCOS(O)(=O)=O KIWBPDUYBMNFTB-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- 150000005215 alkyl ethers Chemical class 0.000 description 2
- 125000005037 alkyl phenyl group Chemical group 0.000 description 2
- 150000008051 alkyl sulfates Chemical class 0.000 description 2
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 2
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
- NOPFSRXAKWQILS-UHFFFAOYSA-N docosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCO NOPFSRXAKWQILS-UHFFFAOYSA-N 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
- 229960000878 docusate sodium Drugs 0.000 description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- FIPPFBHCBUDBRR-UHFFFAOYSA-N henicosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCO FIPPFBHCBUDBRR-UHFFFAOYSA-N 0.000 description 2
- CKDDRHZIAZRDBW-UHFFFAOYSA-N henicosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCC(O)=O CKDDRHZIAZRDBW-UHFFFAOYSA-N 0.000 description 2
- GOQYKNQRPGWPLP-UHFFFAOYSA-N heptadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 2
- KEMQGTRYUADPNZ-UHFFFAOYSA-N heptadecanoic acid Chemical compound CCCCCCCCCCCCCCCCC(O)=O KEMQGTRYUADPNZ-UHFFFAOYSA-N 0.000 description 2
- AKRQHOWXVSDJEF-UHFFFAOYSA-N heptane-1-sulfonic acid Chemical compound CCCCCCCS(O)(=O)=O AKRQHOWXVSDJEF-UHFFFAOYSA-N 0.000 description 2
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- LPTIRUACFKQDHZ-UHFFFAOYSA-N hexadecyl sulfate;hydron Chemical compound CCCCCCCCCCCCCCCCOS(O)(=O)=O LPTIRUACFKQDHZ-UHFFFAOYSA-N 0.000 description 2
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- SIOLDWZBFABPJU-UHFFFAOYSA-N isotridecanoic acid Chemical compound CC(C)CCCCCCCCCC(O)=O SIOLDWZBFABPJU-UHFFFAOYSA-N 0.000 description 2
- ISYWECDDZWTKFF-UHFFFAOYSA-N nonadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCCC(O)=O ISYWECDDZWTKFF-UHFFFAOYSA-N 0.000 description 2
- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 description 2
- ZGAZPDWSRYNUSZ-UHFFFAOYSA-N nonane-1-sulfonic acid Chemical compound CCCCCCCCCS(O)(=O)=O ZGAZPDWSRYNUSZ-UHFFFAOYSA-N 0.000 description 2
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 description 2
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 2
- CNNRPFQICPFDPO-UHFFFAOYSA-N octacosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCO CNNRPFQICPFDPO-UHFFFAOYSA-N 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- WLGDAKIJYPIYLR-UHFFFAOYSA-N octane-1-sulfonic acid Chemical compound CCCCCCCCS(O)(=O)=O WLGDAKIJYPIYLR-UHFFFAOYSA-N 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- OQILCOQZDHPEAZ-UHFFFAOYSA-N octyl palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OCCCCCCCC OQILCOQZDHPEAZ-UHFFFAOYSA-N 0.000 description 2
- IACKKVBKKNJZGN-UHFFFAOYSA-N pentacosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCO IACKKVBKKNJZGN-UHFFFAOYSA-N 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 2
- URLJMZWTXZTZRR-UHFFFAOYSA-N sodium myristyl sulfate Chemical compound CCCCCCCCCCCCCCOS(O)(=O)=O URLJMZWTXZTZRR-UHFFFAOYSA-N 0.000 description 2
- 229960000776 sodium tetradecyl sulfate Drugs 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- AGGIJOLULBJGTQ-UHFFFAOYSA-N sulfoacetic acid Chemical compound OC(=O)CS(O)(=O)=O AGGIJOLULBJGTQ-UHFFFAOYSA-N 0.000 description 2
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 2
- BJQWBACJIAKDTJ-UHFFFAOYSA-N tetrabutylphosphanium Chemical compound CCCC[P+](CCCC)(CCCC)CCCC BJQWBACJIAKDTJ-UHFFFAOYSA-N 0.000 description 2
- TYWMIZZBOVGFOV-UHFFFAOYSA-N tetracosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCO TYWMIZZBOVGFOV-UHFFFAOYSA-N 0.000 description 2
- WFIYFFUAOQKJJS-UHFFFAOYSA-N tetraoctylphosphanium Chemical compound CCCCCCCC[P+](CCCCCCCC)(CCCCCCCC)CCCCCCCC WFIYFFUAOQKJJS-UHFFFAOYSA-N 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- REZQBEBOWJAQKS-UHFFFAOYSA-N triacontan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCO REZQBEBOWJAQKS-UHFFFAOYSA-N 0.000 description 2
- FPLNRAYTBIFSFW-UHFFFAOYSA-N tricosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCO FPLNRAYTBIFSFW-UHFFFAOYSA-N 0.000 description 2
- GTSMGKYOGFOSAR-UHFFFAOYSA-N tridecane-1-sulfonic acid Chemical compound CCCCCCCCCCCCCS(O)(=O)=O GTSMGKYOGFOSAR-UHFFFAOYSA-N 0.000 description 2
- SZHOJFHSIKHZHA-UHFFFAOYSA-N tridecanoic acid Chemical compound CCCCCCCCCCCCC(O)=O SZHOJFHSIKHZHA-UHFFFAOYSA-N 0.000 description 2
- QCLVFLIIJODTJU-UHFFFAOYSA-N triethyl(octyl)phosphanium Chemical compound CCCCCCCC[P+](CC)(CC)CC QCLVFLIIJODTJU-UHFFFAOYSA-N 0.000 description 2
- PYVOHVLEZJMINC-UHFFFAOYSA-N trihexyl(tetradecyl)phosphanium Chemical compound CCCCCCCCCCCCCC[P+](CCCCCC)(CCCCCC)CCCCCC PYVOHVLEZJMINC-UHFFFAOYSA-N 0.000 description 2
- SJEYEFOHSMBQIX-UHFFFAOYSA-N undecane-1-sulfonic acid Chemical compound CCCCCCCCCCCS(O)(=O)=O SJEYEFOHSMBQIX-UHFFFAOYSA-N 0.000 description 2
- ZDPHROOEEOARMN-UHFFFAOYSA-N undecanoic acid Chemical compound CCCCCCCCCCC(O)=O ZDPHROOEEOARMN-UHFFFAOYSA-N 0.000 description 2
- ADHNUPOJJCKWRT-JLXBFWJWSA-N (2e,4e)-octadeca-2,4-dienoic acid Chemical compound CCCCCCCCCCCCC\C=C\C=C\C(O)=O ADHNUPOJJCKWRT-JLXBFWJWSA-N 0.000 description 1
- ZUUFLXSNVWQOJW-MBIXAETLSA-N (2e,4e,6e)-octadeca-2,4,6-trienoic acid Chemical compound CCCCCCCCCCC\C=C\C=C\C=C\C(O)=O ZUUFLXSNVWQOJW-MBIXAETLSA-N 0.000 description 1
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 description 1
- GWSURTDMLUFMJH-FOCLMDBBSA-N (e)-hexadec-1-en-1-ol Chemical compound CCCCCCCCCCCCCC\C=C\O GWSURTDMLUFMJH-FOCLMDBBSA-N 0.000 description 1
- JEGNXMUWVCVSSQ-ISLYRVAYSA-N (e)-octadec-1-en-1-ol Chemical compound CCCCCCCCCCCCCCCC\C=C\O JEGNXMUWVCVSSQ-ISLYRVAYSA-N 0.000 description 1
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 description 1
- GYSCBCSGKXNZRH-UHFFFAOYSA-N 1-benzothiophene-2-carboxamide Chemical compound C1=CC=C2SC(C(=O)N)=CC2=C1 GYSCBCSGKXNZRH-UHFFFAOYSA-N 0.000 description 1
- FKKAGFLIPSSCHT-UHFFFAOYSA-N 1-dodecoxydodecane;sulfuric acid Chemical compound OS(O)(=O)=O.CCCCCCCCCCCCOCCCCCCCCCCCC FKKAGFLIPSSCHT-UHFFFAOYSA-N 0.000 description 1
- 229960002666 1-octacosanol Drugs 0.000 description 1
- QJRRBVNPIKYRQJ-UHFFFAOYSA-N 10-methylundecanoic acid Chemical compound CC(C)CCCCCCCCC(O)=O QJRRBVNPIKYRQJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
提供一种提高耐燃化处理工序中的耐燃化纤维的集束性的碳纤维前体用处理剂。碳纤维前体用处理剂含有:(A)包含氨基改性硅酮的平滑剂;(B)选自有机硫酸鏻盐、有机磺酸鏻盐、在分子中具有碳原子数为3以上的烷基的有机硫酸的季铵盐、在分子中具有碳原子数为3以上的烷基的有机磺酸的季铵盐中的至少一种鎓盐;以及(C)非离子表面活性剂。
Description
技术领域
本发明涉及碳纤维前体用处理剂以及附着有碳纤维前体用处理剂的碳纤维前体。
背景技术
碳纤维通常作为例如与环氧树脂等基体树脂组合而成的碳纤维复合材料而被广泛用于建材、传输设备等各领域中。碳纤维例如可如下进行制造:通过进行对丙烯酸纤维进行纺丝的纺丝工序、以及对纤维进行拉伸的拉伸工序来制造碳纤维前体,对于碳纤维前体进行耐燃化处理工序以及碳化处理工序,由此制造出碳纤维。在碳纤维前体中,为了抑制在碳纤维的制造工序中产生的纤维间的胶着或熔接,有时使用碳纤维前体用处理剂。
国际公开第2013-129115号中公开了一种技术,其中,通过使碳纤维前体用处理剂含有具有包含氮原子的改性基团的改性硅酮、以及酸性磷酸酯,可实现处理剂的溶液稳定性的提高、对碳纤维前体进行纺丝时的结胶的抑制以及烧制处理中的碳纤维的熔接的抑制。
发明内容
发明所要解决的课题
现有的碳纤维前体用处理剂中,对碳纤维前体赋予耐燃化处理工序中的集束性的效果不充分。
因此,本发明所要解决的课题在于提高耐燃化处理工序中的耐燃化纤维的集束性。
用于解决课题的手段
用于解决上述课题的碳纤维前体用处理剂含有:平滑剂;选自有机硫酸鏻盐、有机磺酸鏻盐、在分子中具有碳原子数为3以上的烷基的有机硫酸的季铵盐、在分子中具有碳原子数为3以上的烷基的有机磺酸的季铵盐中的至少一种鎓盐;以及非离子表面活性剂。
上述鎓盐优选包含选自有机硫酸鏻盐和有机磺酸鏻盐中的至少一者。
上述鎓盐优选包含选自与分子中的磷原子键结的取代基全部是碳原子数为3以上的烷基的有机硫酸鏻盐以及与分子中的磷原子键结的取代基全部是碳原子数为3以上的烷基的有机磺酸鏻盐中的至少一者。
上述平滑剂优选包含氨基改性硅酮。
上述平滑剂优选包含氨基改性硅酮和聚醚改性硅酮。
设上述平滑剂和上述鎓盐的合计含有比例为100质量份时,优选在碳纤维前体用处理剂中以0.01~20质量份的比例含有上述鎓盐。
上述非离子表面活性剂优选包含相对于1摩尔碳原子数为4~20的脂肪族饱和醇以1~20摩尔的比例加成环氧乙烷而成的物质。
用于解决上述课题的碳纤维前体附着有上述碳纤维前体用处理剂。
发明的效果
根据本发明,能够提高耐燃化处理工序中的耐燃化纤维的集束性。
具体实施方式
(第1实施方式)
下面对具体实现本发明的碳纤维前体用处理剂(下文中简称为处理剂)的第1实施方式进行说明。
本实施方式的处理剂含有(A)平滑剂、(B)特定的鎓盐、以及(C)非离子表面活性剂。下面对本实施方式的处理剂中含有的各成分的详细情况进行说明。
(A)平滑剂
作为本实施方式的处理剂中含有的平滑剂,例如可以举出硅酮、酯等。
关于作为平滑剂使用的硅酮没有特别限制,例如可以举出二甲基硅酮、苯基改性硅酮、氨基改性硅酮、酰胺改性硅酮、聚醚改性硅酮、氨基聚醚改性硅酮、烷基改性硅酮、烷基芳烷基改性硅酮、烷基聚醚改性硅酮、酯改性硅酮、环氧改性硅酮、甲醇改性硅酮、巯基改性硅酮等。
关于作为平滑剂使用的酯没有特别限制,例如可以举出:(1)棕榈酸辛酯、月桂酸油基酯、油酸油基酯、油酸异二十四烷基酯等脂肪族单醇与脂肪族单羧酸的酯化合物;(2)1,6-己二醇二癸酸酯、甘油三油酸酯、三羟甲基丙烷三月桂酸酯、季戊四醇四辛酸酯等脂肪族多元醇与脂肪族单羧酸的酯化合物;(3)壬二酸二油基酯、硫代二丙酸二油基酯、硫代二丙酸二异十六烷基酯、硫代二丙酸二异硬脂酯等脂肪族单醇与脂肪族多元羧酸的酯化合物;(4)油酸苄基酯、月桂酸苄基酯等芳香族单醇与脂肪族单羧酸的酯化合物;(5)双酚A二月桂酸酯、双酚A的环氧烷加成物的二月桂酸酯等芳香族多元醇与脂肪族单羧酸的完全酯化合物;(6)双(2-乙基己基)邻苯二甲酸酯、二异硬脂基间苯二甲酸酯、偏苯三酸三辛酯等脂肪族单醇与芳香族多元羧酸的完全酯化合物;(7)椰子油、菜籽油、葵花籽油、大豆油、蓖麻油、芝麻油、鱼油和牛脂等天然油脂;等等。此外还可以使用在合成纤维用处理剂中采用的公知的平滑剂等。
平滑剂可以单独使用1种,也可以组合使用2种以上。
平滑剂优选包含氨基改性硅酮。氨基改性硅酮的氨基当量例如优选为500~10000g/mol。平滑剂包含氨基改性硅酮的情况下,可提高由被赋予了处理剂的碳纤维前体得到的碳纤维的强度。另外,平滑剂更优选包含氨基改性硅酮和聚醚改性硅酮。这种情况下,可提高后述的纺丝工序中的集束性、同时进一步提高后述的耐燃化处理工序中的集束性。
平滑剂的运动粘度例如在25℃下优选为10mm2/s~100000mm2/s。
(B)特定的鎓盐
本实施方式的处理剂中含有的特定的鎓盐为选自有机硫酸鏻盐、有机磺酸鏻盐、在分子中具有碳原子数为3以上的烷基的有机硫酸的季铵盐、在分子中具有碳原子数为3以上的烷基的有机磺酸的季铵盐中的至少一者。
上述烷基的碳原子数优选为4以上、更优选为5以上。另外,上述烷基的碳原子数优选为20以下。上述烷基可以为直链状和支链状的任一者,优选为直链状。
作为构成有机硫酸鏻盐的有机硫酸,例如可以举出:(1)乙基硫酸、辛基硫酸、月桂基硫酸、十四烷基硫酸、十六烷基硫酸、十八烷基硫酸等烷基硫酸酯;(2)聚氧乙烯月桂基醚硫酸等聚氧化烯烷基醚硫酸(聚氧化烯的平均加成摩尔数例如为1~25)、聚氧乙烯壬基苯基醚硫酸等聚氧化烯烷基苯基醚硫酸(聚氧化烯的平均加成摩尔数例如为1~25)。
作为构成在分子中具有碳原子数为3以上的烷基的有机硫酸的季铵盐的有机硫酸,例如可以举出:(1)辛基硫酸、月桂基硫酸、十四烷基硫酸、十六烷基硫酸、十八烷基硫酸、异十八烷基硫酸等烷基硫酸酯;(2)聚氧乙烯月桂基醚硫酸、聚氧乙烯十四烷基醚硫酸、聚氧乙烯十六烷基醚硫酸、聚氧乙烯十八烷基醚硫酸、聚氧乙烯异十八烷基醚硫酸等聚氧化烯烷基醚硫酸(聚氧化烯的平均加成摩尔数例如为1~25)、聚氧乙烯壬基苯基醚硫酸等聚氧化烯烷基苯基醚硫酸(聚氧化烯的平均加成摩尔数例如为1~25)。
作为构成有机磺酸鏻盐的有机磺酸,例如可以举出:(1)甲磺酸、乙烷磺酸、己基磺酸、庚基磺酸、2-乙基己基磺酸、辛基磺酸、壬基磺酸、癸基磺酸、十一烷基磺酸、十二烷基磺酸、十三烷基磺酸等烷基磺酸;(2)对甲苯磺酸、乙基苯磺酸、癸基苯磺酸、十一烷基苯磺酸、十二烷基苯磺酸、十三烷基苯磺酸、十四烷基苯磺酸、十五烷基苯磺酸、十六烷基苯磺酸、二丁基萘磺酸等烷基芳基磺酸;(3)十六烷基二苯基醚二磺酸等二苯基醚磺酸;(4)二辛基磺基琥珀酸酯、二丁基磺基琥珀酸酯、十二烷基磺基乙酸酯、壬基苯氧基聚乙二醇磺基乙酸酯等酯磺酸;等等。
作为构成在分子中具有碳原子数为3以上的烷基的有机磺酸的季铵盐的有机磺酸,例如可以举出:(1)己基磺酸、庚基磺酸、2-乙基己基磺酸、辛基磺酸、壬基磺酸、癸基磺酸、十一烷基磺酸、十二烷基磺酸、十三烷基磺酸等烷基磺酸;(2)癸基苯磺酸、十一烷基苯磺酸、十二烷基苯磺酸、十三烷基苯磺酸、十四烷基苯磺酸、十五烷基苯磺酸、十六烷基苯磺酸、二丁基萘磺酸等烷基芳基磺酸;(3)十六烷基二苯基醚二磺酸等二苯基醚磺酸;(4)二辛基磺基琥珀酸酯、二丁基磺基琥珀酸酯、十二烷基磺基乙酸酯、壬基苯氧基聚乙二醇磺基乙酸酯等酯磺酸;等等。
作为构成有机硫酸鏻盐和有机磺酸鏻盐的磷鎓,例如可以举出四甲基磷鎓、四乙基磷鎓、四丁基磷鎓、四辛基磷鎓、二丁基二己基磷鎓三己基十四烷基磷鎓、三乙基辛基磷鎓、三苯基甲基磷鎓等季磷鎓。
作为构成在分子中具有碳原子数为3以上的烷基的有机硫酸的季铵盐和在分子中具有碳原子数为3以上的烷基的有机磺酸的季铵盐的季铵,例如可以举出四丁基铵、三己基十四烷基铵。
特定的鎓盐可以单独使用1种,也可以组合使用2种以上。
需要说明的是,特定的鎓盐优选包含选自有机硫酸鏻盐和有机磺酸鏻盐中的至少一者。另外,特定的鎓盐更优选包含选自与分子中的磷原子键结的取代基全部是碳原子数为3以上的烷基的有机硫酸鏻盐以及与分子中的磷原子键结的取代基全部是碳原子数为3以上的烷基的有机磺酸鏻盐中的至少一者。这种情况下,能够对附着有处理剂的碳纤维前体赋予抗静电性。
(C)非离子表面活性剂
作为本实施方式的处理剂中含有的非离子表面活性剂没有特别限制,例如可以举出使环氧烷加成至醇类或羧酸类而得到的物质。
关于作为非离子表面活性剂的原料使用的醇类的具体例,例如可以举出:(1)甲醇、乙醇、丙醇、丁醇、戊醇、己醇、辛醇、壬醇、癸醇、十一烷醇、十二烷醇、十三烷醇、十四烷醇、十五烷醇、十六烷醇、十七烷醇、十八烷醇、十九烷醇、二十烷醇、二十一烷醇、二十二烷醇、二十三烷醇、二十四烷醇、二十五烷醇、二十六烷醇、二十七烷醇、二十八烷醇、二十九烷醇、三十烷醇等直链烷基醇;(2)异丙醇、异丁醇、异己醇、2-乙基己醇、异壬醇、异癸醇、异十二烷醇、异十三烷醇、异十四烷醇、异三十烷醇、异十六烷醇、异十七烷醇、异十八烷醇、异十九烷醇、异二十烷醇、异二十一烷醇、异二十二烷醇、异二十三烷醇、异二十四烷醇、异二十烷五醇、异二十六烷醇、异二十七烷醇、异二十八烷醇、异二十九烷醇、异十五烷醇等支链烷基醇;(3)十四烯醇、十六烯醇、十七烯醇、十八烯醇、十九烯醇等直链烯基醇;(4)异十六烯醇、异十八烯醇等支链烯基醇;(5)环戊醇、环己醇等环状烷基醇;(6)苯酚、壬基苯酚、苯甲醇、单苯乙烯化苯酚、二苯乙烯化苯酚、三苯乙烯化苯酚等芳香族系醇;等等。
关于作为非离子表面活性剂的原料使用的羧酸类的具体例,例如可以举出:(1)辛酸、壬酸、癸酸、十一烷酸、十二烷酸、十三烷酸、十四烷酸、十五烷酸、十六烷酸、十七烷酸、十八烷酸、十九烷酸、二十烷酸、二十一烷酸、山嵛酸等直链烷基羧酸;(2)2-乙基己酸、异十二烷酸、异十三烷酸、异十四烷酸、异十六烷酸、异十八烷酸等支链烷基羧酸;(3)十八碳烯酸、十八碳二烯酸、十八碳三烯酸等直链烯基羧酸;(4)苯甲酸等芳香族系羧酸;等等。
关于作为非离子表面活性剂的原料使用的环氧烷的具体例,例如可以举出环氧乙烷、环氧丙烷等。
非离子表面活性剂可以单独使用1种,也可以将2种以上组合使用。
需要说明的是,非离子表面活性剂优选包含相对于1摩尔的直链烷基醇等碳原子数为4~20的脂肪族饱和醇以1~20摩尔的比例加成环氧乙烷而成的物质。这种情况下,处理剂的稳定性提高。
(D)其他成分
本实施方式的处理剂可以在不妨碍本发明的效果的范围内进一步含有通常用于处理剂中的其他成分。作为其他成分,例如可以举出增粘剂、抗氧化剂、紫外线吸收剂等用于保持处理剂的品质的稳定化剂、电荷控制剂。其他成分可以单独使用1种、也可以将2种以上组合使用。
接着对本实施方式的处理剂中的各成分的含有比例进行说明。本实施方式的处理剂中的各成分的含有比例没有特别限制,优选为下述含有比例。
设(A)平滑剂、(B)特定的鎓盐以及(C)非离子表面活性剂的合计含有比例(以下称为主成分合计)为100质量份时,(A)平滑剂的含有比例优选为29.9~95质量份、更优选为60~90质量份。
设主成分合计为100质量份时,(B)特定的鎓盐的含有比例优选为0.1~30质量份、更优选为0.5~25质量份。另外,设平滑剂和特定的鎓盐的合计含有比例为100质量份时,(B)特定的鎓盐的含有比例优选为0.01~20质量份。这种情况下,容易得到赋予抗静电性的效果以及提高碳纤维的强度的效果。
设主成分合计为100质量份时,(C)非离子表面活性剂优选为1~70质量份、更优选为5~30质量份。
另外,设本实施方式的处理剂中的不挥发成分的含有比例为100质量份时,(A)平滑剂、(B)特定的鎓盐以及(C)非离子表面活性剂的合计含有比例优选为50质量份以上、更优选为75质量份以上。
(第2实施方式)
接着对具体实现本发明的碳纤维前体的第2实施方式进行说明。
本实施方式的碳纤维前体具备将原料纤维纺丝而成的纤维部分、以及附着于纤维部分的第1实施方式的处理剂。通过对本实施方式的碳纤维前体进行在200~300℃、优选230~270℃的氧化性气氛中转换成耐燃化纤维的耐燃化处理工序以及将耐燃化纤维进一步在300~2000℃、优选300~1300℃的惰性气氛中进行碳化的碳化处理工序而制造出碳纤维。
作为原料纤维,例如可以举出丙烯酸纤维等。丙烯酸纤维优选由以聚丙烯腈作为主成分的纤维构成,该聚丙烯腈是使至少90摩尔%以上的丙烯腈与10摩尔%以下的耐燃化促进成分共聚而得到的。作为耐燃化促进成分,例如可以适当地使用对于丙烯腈具有共聚性的含乙烯基化合物。
碳纤维前体中的第1实施方式的处理剂的附着量没有特别限制,优选按照相对于碳纤维前体为0.1~2质量%的方式附着,更优选按照为0.3~1.2质量%的方式附着。需要说明的是,上述浓度为不含溶剂的固体成分浓度。
碳纤维前体的单纤维纤度没有特别限制,从性能和制造成本的平衡的方面出发优选为0.1~2.0dTex。另外,构成碳纤维前体的纤维束的单纤维的根数没有特别限制,从性能和制造成本的平衡的方面出发优选为1,000~96,000根。
碳纤维前体可以通过对原料纤维进行纺丝和拉伸的缫丝工序来制造。缫丝工序中例如依次进行对原料纤维进行纺丝的纺丝工序、使第1实施方式的处理剂附着于纺丝后的纤维的附着处理工序、以及对纺丝后的纤维进行拉伸的拉伸工序。需要说明的是,原料纤维在刚纺丝后即进行拉伸,但将附着处理工序后的高倍率拉伸特别称为“拉伸工序”。
附着处理工序是在对原料纤维进行纺丝后使第1实施方式的处理剂进行附着的工序。即,附着处理工序中,使第1实施方式的处理剂附着于原料纤维。
附着处理工序中的第1实施方式的处理剂的附着方法可以应用公知的方法。作为公知的附着方法,例如可以举出喷雾给油法、浸渍给油法、辊给油法、使用计量泵的引导给油法等。使第1实施方式的处理剂附着于纤维时的处理剂的形态例如可以为有机溶剂溶液或水性液等。
拉伸工序中的拉伸方法可以应用公知的方法。作为公知的拉伸方法,例如可以举出使用高温水蒸气的湿热拉伸法、使用热辊的干热拉伸法等。
在缫丝工序中,使第1实施方式的处理剂附着的时机和使第1实施方式的处理剂附着的次数没有特别限制。例如,可以附着于纺丝工序前的原料纤维,也可以在拉伸工序后附着。作为在拉伸工序后附着的时机,例如可以举出刚进行拉伸工序后、拉伸工序后的卷取阶段、即将进行耐燃化处理工序之前。需要说明的是,第1实施方式的处理剂优选在拉伸工序前进行一次附着,更优选在拉伸工序前进行一次附着、在拉伸工序后立即进行再次附着。
对第1实施方式和第2实施方式的效果进行说明。
(1)第1实施方式的处理剂含有(A)平滑剂、(B)特定的鎓盐、以及(C)非离子表面活性剂。第2实施方式的碳纤维前体附着有第1实施方式的处理剂。根据上述构成,由附着有处理剂的碳纤维前体制造碳纤维时的耐燃化处理工序中的耐燃化纤维的集束性提高。进而,根据上述构成,能够对附着有处理剂的碳纤维前体赋予抗静电性、提高由附着有处理剂的碳纤维前体得到的碳纤维的强度、以及提高制造碳纤维前体时的纺丝工序中的集束性。
(2)(B)特定的鎓盐可以包含选自有机硫酸鏻盐和有机磺酸鏻盐中的至少一者。根据上述构成,可更显著地得到上述(1)的效果。
(3)(B)特定的鎓盐可以包含选自与分子中的磷原子键结的取代基全部是碳原子数为3以上的烷基的有机硫酸鏻盐以及与分子中的磷原子键结的取代基全部是碳原子数为3以上的烷基的有机磺酸鏻盐中的至少一者。根据上述构成,可提高对附着有处理剂的碳纤维前体赋予抗静电性的效果。由此能够减少在使碳纤维前体移动时或卷取时所产生的电,碳纤维前体的处理变得容易。
(4)(A)平滑剂可以包含氨基改性硅酮。根据上述构成,可提高由附着有处理剂的碳纤维前体得到的碳纤维的强度。
(5)(A)平滑剂可以包含氨基改性硅酮和聚醚改性硅酮。根据上述构成,除了上述(4)的效果以外,还可提高制造碳纤维前体时的纺丝工序中的集束性,并且进一步提高耐燃化处理工序中的耐燃化纤维的集束性。
(6)碳纤维前体用处理剂中,设(A)平滑剂和(B)特定的鎓盐的合计含有比例为100质量份时,可以以0.01~20质量份的比例含有(B)特定的鎓盐。根据上述构成,容易得到上述(3)的效果和上述(4)的效果。
(7)(C)非离子表面活性剂可以包含相对于1摩尔的碳原子数为4~20的脂肪族饱和醇以1~20摩尔的比例加成环氧乙烷而成的物质。根据上述构成,可提高处理剂的稳定性。
[实施例]
以下为了更具体地说明本发明的构成和效果,举出实施例等,但本发明并不受这些实施例的限定。需要说明的是,以下的实施例和比较例的说明中,份是指质量份,并且%是指质量%。
试验分组1(碳纤维前体用处理剂的制造)
(实施例1)
使用表1所示的各成分,将平滑剂(A-1)120g、平滑剂(A-4)40g、特定的鎓盐(B-1)10g、非离子表面活性剂(C-1)20g、非离子表面活性剂(C-2)10g加入烧杯中,进行搅拌将其充分混合。一边继续进行搅拌一边缓慢地添加离子交换水使固体成分浓度达到25%,由此制备实施例1的碳纤维前体用处理剂的25%水性液。
(实施例2~13和比较例1~6)
使用表1中示出的各成分,利用与实施例1相同的方法制备实施例2~13和比较例1~6的各碳纤维前体用处理剂。
[表1]
表1的符号栏中记载的A-1~A-6、B-1~B-8、rb1~rb5以及C-1~C-5的各成分的详细内容如下所述。
(平滑剂)
A-1:25℃的运动粘度为650mm2/s、氨基当量为1800g/mol的氨基改性硅酮
A-2:25℃的运动粘度为90mm2/s、氨基当量为5000g/mol的氨基改性硅酮
A-3:25℃的运动粘度为1400mm2/s、氨基当量为2000g/mol的氨基改性硅酮
A-4:25℃的运动粘度为1700mm2/s、硅酮主链/聚醚侧链=20/80(质量比)、环氧乙烷/环氧丙烷=50/50(摩尔比)的聚醚改性硅酮
A-5:25℃的运动粘度为17000mm2/s、环氧当量:3800g/mol的环氧改性硅酮
A-6:硫代二丙酸二(正十二烷基)酯
(特定的鎓盐)
B-1:十二烷基苯磺酸的四丁基鏻盐
B-2:环氧乙烷5摩尔加成的月桂基醚硫酸的四辛基鏻盐
B-3:乙烷磺酸的二丁基二己基鏻盐
B-4:十八烷基硫酸的三己基十四烷基鏻盐
B-5:十二烷基磺酸的三乙基辛基鏻盐
B-6:己基磺酸的三苯基甲基鏻盐
B-7:十二烷基苯磺酸的四丁基铵盐
B-8:辛基硫酸的三己基十四烷基铵盐
(其他离子性成分)
rb-1:十二烷基苯磺酸
rb-2:乙基硫酸的四乙基铵盐
rb-3:2-乙基己基磷酸酯
rb-4:硫酸钠
rb-5:十二烷基苯磺酸钠
(非离子表面活性剂)
C-1:异十二烷基醇的环氧乙烷10摩尔加成物
C-2:异十八烷醇的环氧乙烷5摩尔加成物
C-3:己醇的环氧乙烷5摩尔加成物
C-4:十四烷基醇的环氧乙烷18摩尔加成物
C-5:壬基苯酚的环氧乙烷7摩尔加成物
试验分组2(碳纤维前体和碳纤维的制造)
使用试验分组1中制备的碳纤维前体用处理剂,制造碳纤维前体和碳纤维。
将由丙烯腈95质量%、丙烯酸甲酯3.5质量%、甲基丙烯酸1.5质量%形成的特性粘度1.80的共聚物溶解在二甲基乙酰胺(DMAC)中,制作聚合物浓度为21.0质量%、60℃时的粘度为500泊的纺丝原液。将纺丝原液在保持于纺浴温度35℃的DMAC的70质量%水溶液的凝固浴中利用孔径(内径)0.075mm、孔数12,000的纺丝喷头以牵伸比0.8排出。
将凝固丝在水洗槽中脱溶剂并同时拉伸至5倍,制作水溶胀状态的丙烯酸纤维线料(原料纤维)。按照固体成分附着量为1质量%(不包含溶剂)的方式将试验分组1中制备的碳纤维前体用处理剂对于该丙烯酸纤维线料进行给油。碳纤维前体用处理剂的给油通过使用碳纤维前体用处理剂的4%离子交换水溶液的浸渍法来实施。
其后,利用130℃的加热辊对于丙烯酸纤维线料进行干燥致密化处理,进一步在170℃的加热辊间实施1.7倍的拉伸,然后卷取在丝管上,由此得到碳纤维前体。
由卷取的碳纤维前体进行丝的解舒,在具有230~270℃的温度梯度的耐燃化炉中在空气气氛下进行1小时耐燃化处理,然后卷取在丝管上,由此得到耐燃化丝(耐燃化纤维)。进一步由卷取的耐燃化丝进行丝的解舒,在氮气气氛下在具有300~1,300℃的温度梯度的碳化炉中进行烧制,转换成碳纤维,然后卷取在丝管上,由此得到碳纤维。
试验分组3(评价)
·耐燃化集束性的评价
在试验分组2的碳纤维的制造过程中,目视观察耐燃化处理后、卷取前的耐燃化丝的集束状态,按下述基准评价耐燃化集束性。将结果示于表1的“耐燃化集束性”栏中。
◎(优):产生集束,丝束宽度固定。
○(良):产生集束,但丝束宽度不固定。
×(不良):纤维束中存在空间,未产生集束。
·电阻的评价
将试验分组2中得到的碳纤维前体在20℃×65%RH的气氛下放置24小时,在该条件下将评价试样10g装入电阻测定用盒(40ml容量)中,使用东亚电波工业公司制造的商品名SM-5E型绝缘计测定电阻值(logΩ),按下述基准评价电阻。将结果示于表1的“电阻”栏中。
◎(优):小于9
○(良):9以上且小于10
×(不良):10以上
·碳纤维强度的评价
依据JIS R 7606对试验分组2中得到的碳纤维的强度进行测定,按下述基准进行评价。将结果示于表1的“碳纤维强度”栏中。
◎(优):4.0GPa以上
○(良):3.5GPa以上且小于4.0GPa
×(不良):小于3.5GPa
·纺丝集束性的评价
在试验分组2的碳纤维前体的制造过程中,目视观察即将卷曲至丝管之前的最终辊上的碳纤维前体的集束状态,按下述基准进行纺丝集束性的评价。将结果示于表1的“纺丝集束性”栏中。
◎(优):产生集束,丝束宽度固定。
○(良):产生集束,但丝束宽度不固定。
×(不良):纤维束中存在空间,未产生集束。
如表1所示,与使用不含有(B)特定的鎓盐的比较例1~6的处理剂的情况相比,在使用含有(A)平滑剂、(B)特定的鎓盐以及(C)非离子表面活性剂的实施例1~13的处理剂的情况下,耐燃化集束性的评价提高。另外,使用实施例1~13的处理剂的情况下,除了耐燃化集束性的评价以外,电阻的评价、碳纤维强度的评价以及纺丝集束性的评价均得到了优异的结果。
在使用了包含与分子中的磷原子键结的取代基全部是碳原子数为3以上的烷基的有机硫酸鏻盐或有机磺酸鏻盐作为(B)特定的鎓盐的实施例1~8的处理剂的情况下,与使用了(B)特定的鎓盐为其他特定的鎓盐的实施例9~10、12~13的处理剂的情况相比,电阻的评价显著提高。
作为(A)平滑剂使用包含氨基改性硅酮的实施例1~5的处理剂的情况下,与使用不含氨基改性硅酮的实施例6~8的处理剂的情况相比,碳纤维强度的评价显著提高。特别是作为(A)平滑剂使用包含氨基改性硅酮和聚醚改性硅酮的实施例1~3的处理剂的情况下,除了碳纤维强度的评价以外,耐燃化集束性的评价和纺丝集束性的评价也显著提高。
根据使用(A)平滑剂、(B)特定的鎓盐以及(C)非离子表面活性剂的各成分相同但(A)平滑剂和(B)特定的鎓盐的含有比例不同的实施例5和实施例11的处理剂时的结果的比较确认到,通过降低(B)特定的鎓盐相对于(A)平滑剂的含有比例的质量比例,具有容易提高电阻的评价和碳纤维强度的评价的倾向。
Claims (7)
1.一种碳纤维前体用处理剂,其含有:
包含氨基改性硅酮的平滑剂;
选自有机硫酸鏻盐、有机磺酸鏻盐、有机硫酸的季铵盐、有机磺酸的季铵盐中的至少一种鎓盐,所述季铵盐中的有机硫酸在分子中具有碳原子数为3以上的烷基,所述季铵盐中的有机磺酸在分子中具有碳原子数为3以上的烷基;以及
非离子表面活性剂。
2.如权利要求1所述的碳纤维前体用处理剂,其中,所述鎓盐包含选自有机硫酸鏻盐和有机磺酸鏻盐中的至少一者。
3.如权利要求2所述的碳纤维前体用处理剂,其中,所述鎓盐包含选自与分子中的磷原子键结的取代基全部是碳原子数为3以上的烷基的有机硫酸鏻盐以及与分子中的磷原子键结的取代基全部是碳原子数为3以上的烷基的有机磺酸鏻盐中的至少一者。
4.如权利要求1所述的碳纤维前体用处理剂,其中,所述平滑剂包含氨基改性硅酮和聚醚改性硅酮。
5.如权利要求3所述的碳纤维前体用处理剂,其中,设所述平滑剂和所述鎓盐的合计含有比例为100质量份时,以0.01质量份~20质量份的比例含有所述鎓盐。
6.如权利要求1~5中任一项所述的碳纤维前体用处理剂,其中,所述非离子表面活性剂包含相对于1摩尔碳原子数为4~20的脂肪族饱和醇以1摩尔~20摩尔的比例加成环氧乙烷而成的物质。
7.一种碳纤维前体,其附着有权利要求1~6中任一项所述的碳纤维前体用处理剂。
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