CN110964166A - 一种聚氨酯弹性体的制备方法 - Google Patents
一种聚氨酯弹性体的制备方法 Download PDFInfo
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- CN110964166A CN110964166A CN201811121628.1A CN201811121628A CN110964166A CN 110964166 A CN110964166 A CN 110964166A CN 201811121628 A CN201811121628 A CN 201811121628A CN 110964166 A CN110964166 A CN 110964166A
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- component
- polyurethane elastomer
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- chain extender
- dimethyltin
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- 229920003225 polyurethane elastomer Polymers 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000004970 Chain extender Substances 0.000 claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- 150000002009 diols Chemical class 0.000 claims abstract description 18
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 18
- 239000004417 polycarbonate Substances 0.000 claims abstract description 18
- 229920002635 polyurethane Polymers 0.000 claims abstract description 9
- 239000004814 polyurethane Substances 0.000 claims abstract description 9
- 239000012948 isocyanate Substances 0.000 claims abstract description 6
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 15
- 150000001412 amines Chemical group 0.000 claims description 14
- -1 carbon diol Chemical class 0.000 claims description 12
- 125000003158 alcohol group Chemical group 0.000 claims description 8
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 125000005442 diisocyanate group Chemical group 0.000 claims description 6
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 125000003944 tolyl group Chemical group 0.000 claims description 5
- PISLZQACAJMAIO-UHFFFAOYSA-N 2,4-diethyl-6-methylbenzene-1,3-diamine Chemical compound CCC1=CC(C)=C(N)C(CC)=C1N PISLZQACAJMAIO-UHFFFAOYSA-N 0.000 claims description 4
- BFSVOASYOCHEOV-UHFFFAOYSA-N 2-diethylaminoethanol Chemical compound CCN(CC)CCO BFSVOASYOCHEOV-UHFFFAOYSA-N 0.000 claims description 4
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 4
- CQQXCSFSYHAZOO-UHFFFAOYSA-L [acetyloxy(dioctyl)stannyl] acetate Chemical compound CCCCCCCC[Sn](OC(C)=O)(OC(C)=O)CCCCCCCC CQQXCSFSYHAZOO-UHFFFAOYSA-L 0.000 claims description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 4
- SDTDHTCWRNVNAJ-UHFFFAOYSA-L dimethyltin(2+);diacetate Chemical compound CC(=O)O[Sn](C)(C)OC(C)=O SDTDHTCWRNVNAJ-UHFFFAOYSA-L 0.000 claims description 4
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 4
- 239000012974 tin catalyst Substances 0.000 claims description 4
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 4
- CBEVWPCAHIAUOD-UHFFFAOYSA-N 4-[(4-amino-3-ethylphenyl)methyl]-2-ethylaniline Chemical compound C1=C(N)C(CC)=CC(CC=2C=C(CC)C(N)=CC=2)=C1 CBEVWPCAHIAUOD-UHFFFAOYSA-N 0.000 claims description 3
- HVCNXQOWACZAFN-UHFFFAOYSA-N 4-ethylmorpholine Chemical compound CCN1CCOCC1 HVCNXQOWACZAFN-UHFFFAOYSA-N 0.000 claims description 3
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- SNZAWIWMBQMVSB-BGSQTJHASA-L dioctyltin(2+);(z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)O[Sn](CCCCCCCC)(CCCCCCCC)OC(=O)CCCCCCC\C=C/CCCCCCCC SNZAWIWMBQMVSB-BGSQTJHASA-L 0.000 claims description 3
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 3
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 3
- ZBBLRPRYYSJUCZ-GRHBHMESSA-L (z)-but-2-enedioate;dibutyltin(2+) Chemical compound [O-]C(=O)\C=C/C([O-])=O.CCCC[Sn+2]CCCC ZBBLRPRYYSJUCZ-GRHBHMESSA-L 0.000 claims description 2
- PKZGKWFUCLURJO-GRHBHMESSA-L (z)-but-2-enedioate;dimethyltin(2+) Chemical compound C[Sn+2]C.[O-]C(=O)\C=C/C([O-])=O PKZGKWFUCLURJO-GRHBHMESSA-L 0.000 claims description 2
- OQBLGYCUQGDOOR-UHFFFAOYSA-L 1,3,2$l^{2}-dioxastannolane-4,5-dione Chemical compound O=C1O[Sn]OC1=O OQBLGYCUQGDOOR-UHFFFAOYSA-L 0.000 claims description 2
- DDPRYTUJYNYJKV-UHFFFAOYSA-N 1,4-diethylpiperazine Chemical compound CCN1CCN(CC)CC1 DDPRYTUJYNYJKV-UHFFFAOYSA-N 0.000 claims description 2
- JUXXCHAGQCBNTI-UHFFFAOYSA-N 1-n,1-n,2-n,2-n-tetramethylpropane-1,2-diamine Chemical compound CN(C)C(C)CN(C)C JUXXCHAGQCBNTI-UHFFFAOYSA-N 0.000 claims description 2
- GTEXIOINCJRBIO-UHFFFAOYSA-N 2-[2-(dimethylamino)ethoxy]-n,n-dimethylethanamine Chemical compound CN(C)CCOCCN(C)C GTEXIOINCJRBIO-UHFFFAOYSA-N 0.000 claims description 2
- IBOFVQJTBBUKMU-UHFFFAOYSA-N 4,4'-methylene-bis-(2-chloroaniline) Chemical compound C1=C(Cl)C(N)=CC=C1CC1=CC=C(N)C(Cl)=C1 IBOFVQJTBBUKMU-UHFFFAOYSA-N 0.000 claims description 2
- ZRWNRAJCPNLYAK-UHFFFAOYSA-N 4-bromobenzamide Chemical compound NC(=O)C1=CC=C(Br)C=C1 ZRWNRAJCPNLYAK-UHFFFAOYSA-N 0.000 claims description 2
- AOFIWCXMXPVSAZ-UHFFFAOYSA-N 4-methyl-2,6-bis(methylsulfanyl)benzene-1,3-diamine Chemical compound CSC1=CC(C)=C(N)C(SC)=C1N AOFIWCXMXPVSAZ-UHFFFAOYSA-N 0.000 claims description 2
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 2
- SVYKKECYCPFKGB-UHFFFAOYSA-N N,N-dimethylcyclohexylamine Chemical compound CN(C)C1CCCCC1 SVYKKECYCPFKGB-UHFFFAOYSA-N 0.000 claims description 2
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- DWRBCWYHLKHQAP-UHFFFAOYSA-L [butanoyloxy(dibutyl)stannyl] butanoate Chemical compound CCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCC DWRBCWYHLKHQAP-UHFFFAOYSA-L 0.000 claims description 2
- HAAANJSJNWKVMX-UHFFFAOYSA-L [butanoyloxy(dimethyl)stannyl] butanoate Chemical compound CCCC(=O)O[Sn](C)(C)OC(=O)CCC HAAANJSJNWKVMX-UHFFFAOYSA-L 0.000 claims description 2
- AWFFJJAOMMAGFE-BGSQTJHASA-L [dibutyl-[(z)-octadec-9-enoyl]oxystannyl] (z)-octadec-9-enoate Chemical compound CCCC[Sn+2]CCCC.CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O AWFFJJAOMMAGFE-BGSQTJHASA-L 0.000 claims description 2
- PGQPMLCDSAVZNJ-BGSQTJHASA-L [dimethyl-[(z)-octadec-9-enoyl]oxystannyl] (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)O[Sn](C)(C)OC(=O)CCCCCCC\C=C/CCCCCCCC PGQPMLCDSAVZNJ-BGSQTJHASA-L 0.000 claims description 2
- XQBCVRSTVUHIGH-UHFFFAOYSA-L [dodecanoyloxy(dioctyl)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCCCCCC)(CCCCCCCC)OC(=O)CCCCCCCCCCC XQBCVRSTVUHIGH-UHFFFAOYSA-L 0.000 claims description 2
- PZGVVCOOWYSSGB-UHFFFAOYSA-L but-2-enedioate;dioctyltin(2+) Chemical compound CCCCCCCC[Sn]1(CCCCCCCC)OC(=O)C=CC(=O)O1 PZGVVCOOWYSSGB-UHFFFAOYSA-L 0.000 claims description 2
- ODUCJAXGIAXRJA-UHFFFAOYSA-L butanoate;dioctyltin(2+) Chemical compound CCCCCCCC[Sn](OC(=O)CCC)(OC(=O)CCC)CCCCCCCC ODUCJAXGIAXRJA-UHFFFAOYSA-L 0.000 claims description 2
- 229960002887 deanol Drugs 0.000 claims description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 2
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 claims description 2
- 239000012972 dimethylethanolamine Substances 0.000 claims description 2
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 claims description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims 2
- 229910052799 carbon Inorganic materials 0.000 claims 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 claims 1
- PWEVMPIIOJUPRI-UHFFFAOYSA-N dimethyltin Chemical compound C[Sn]C PWEVMPIIOJUPRI-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000004073 vulcanization Methods 0.000 claims 1
- 229920001730 Moisture cure polyurethane Polymers 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229920001971 elastomer Polymers 0.000 description 6
- 239000000806 elastomer Substances 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 5
- 238000010926 purge Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- BXQLKGJCLJZZOP-UHFFFAOYSA-N methylsulfanylmethane;toluene Chemical compound CSC.CC1=CC=CC=C1 BXQLKGJCLJZZOP-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N urethane group Chemical group NC(=O)OCC JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G18/6651—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
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- Polyurethanes Or Polyureas (AREA)
Abstract
本发明涉及一种聚氨酯弹性体的制备方法，包括以下步骤：1)A组份：聚氨酯半预聚体制备，制备方法如下：聚碳酸酯二醇50‑100份、异氰酸酯40‑70份在60‑75℃环境下反应1.5‑3小时；2)B组分：聚碳酸酯二醇50‑100份、扩链剂0.5‑5份、催化剂0.01‑0.1份，混合均匀，浇筑到模具之中，在25‑30℃下进行固化，固化4‑6h后脱模，然后在80℃环境下后硫化8h，得到聚氨酯弹性体制品。本发明的聚氨酯弹性体制备方法，克服了聚氨酯预聚体的粘度高的弊端，制备的聚氨酯弹性体具有优越的力学性能，适合于应用在浇注快速固化的产品中。
Description
技术领域
本发明涉及具有良好的力学性能和优异的耐磨性以及耐油性的高性能聚氨酯弹性体。
背景技术
众所周知，聚氨酯弹性体是一种主链上含有较多的氨基甲酸酯基团的高分子嵌段聚合物，具有独特的聚氨酯结构，具有优良的综合力学性能尤其是耐磨性能和耐油性能。聚氨酯弹性体的一般制备方法为一步法，但一步法的制备不易控制，而预聚体法制备的聚氨酯预聚物粘度较大，不宜控制，故采用半预聚法制备聚氨酯半预聚物，不仅能够很好的控制预聚体的粘度，而且制备的预聚体更加稳定，弹性体的性能也更优异。
发明内容
本发明的目的是提供一种聚氨酯弹性体的制备方法，制备的弹性体具有优异的力学性能，耐磨和耐油性能优异。同时采用半预聚体的方法，使制备工艺更加稳定。扩链剂和催化剂的配合使用能够使聚氨酯弹性体的固化时间延长，适合制备大尺寸制品。
本发明所述的一种聚氨酯弹性体的制备方法，包括以下步骤：
1)A组分，聚氨酯半预聚物，制备方法如下：以质量份计，由聚碳酸酯二醇50-100份，聚二甲基甲基苯基硅氧烷碳二醇2-4份，二异氰酸酯40-70份在60-75℃环境下反应1.5-3小时，得到聚氨酯半预聚物；
2)B组分，制备方法：以质量份计，聚碳酸酯二醇50-100份、扩链剂0.5-5份、催化剂0.01-0.1份，混合均匀备用。
3)聚氨酯弹性体的制备过程：将B组份和A组分进行混合反应，混合温度为60-75℃，立即浇筑到模具中，在25-30℃下进行固化，固化4-6h后脱模，然后在80℃环境下后硫化8h，得到聚氨酯弹性体制品。
其中，A组分中所述的聚碳酸酯二醇数均分子量为1500-4000。
其中，A组分中所述的聚二甲基甲基苯基硅氧烷碳二醇为羟乙氧基丙基封端聚二甲基甲基苯基硅氧烷，数均分子量为1000-4000。
其中，A组份中所述的二异氰酸酯为甲苯二异氰酸酯TDI-100，甲苯二异氰酸酯TDI-80、4，4′-二苯基甲烷二异氰酸酯MDI-100，4，4′-二苯基甲烷二异氰酸酯MDI-50，二异氰酸酯中的一种或两种的混合物。
其中，A组份中，聚氨酯半预聚物中的游离异氰酸根含量为4.0％-16.0％。
其中，B组份中所述的聚碳酸酯二醇数均分子量为1500-4000。
2.其中，B组份中所述的扩链剂为胺类扩链剂和醇类扩链剂，胺类扩链剂包括4，4′-二氨基-3，3′-二乙基-二苯基甲烷，3-氯-3’-乙基-4，4’-二氨基二苯甲烷，3，3’二氯-4，4’-二氨基二苯甲烷，二乙基甲苯二胺(DETDA)，二甲硫基甲苯二胺DMTDA，二乙氨基乙醇(DEAE)，醇类扩链剂包括1，4一丁二醇(BDO)、1，6一己二醇、三羟甲基丙烷、二甘醇(DEG)、三甘醇、新戊二醇(NPG)，B组份中所述的扩链剂为醇类扩链剂和胺类扩链剂中的一种或几种的混合物，扩链剂的用量为0.5-5份。
3.其中，B组份中所述的催化剂为锡类催化剂和胺类催化剂，锡类催化剂包括二丁酸二丁基锡、二丁酸二甲基锡、二丁酸二辛基锡、二乙酸二丁基锡、二乙酸二甲基锡、二乙酸二辛基锡、辛酸亚锡、二月桂酸二丁基锡、二月桂酸二甲基锡、二月桂酸二辛基锡、二油酸二丁基锡、二油酸二甲基锡、二油酸二辛基锡、醋酸锡、二醋酸二丁基锡、二醋酸二甲基锡、二醋酸二辛基锡、马来酸二甲基锡、马来酸二丁基锡、马来酸二辛基锡、双十二烷硫基二丁基锡、双十二烷硫基二甲基锡、双十二烷硫基二辛基锡、草酸亚锡等；胺类催化剂包括双(二甲氨基乙基)醚、五甲基二乙烯三胺、三乙烯二胺、二甲基乙醇胺、四甲基乙二胺、四甲基丙二胺、N，N-二甲基环己胺、N，N，N′，N′-四甲基亚烷基二胺、三乙胺、N，N-二甲基苄胺、三乙醇胺、N-乙基吗啉、N，N’-二乙基哌嗪、吡啶，N，N’-二甲基吡啶，B组份中所述的催化剂为锡类催化剂和胺类催化剂中的一种或几种的混合物，催化剂的用量为0.01-0.1份。
其中，所制备的聚氨酯弹性体制品的硬度为邵A硬度40A-85A之间。
本发明通过采用醇类扩链剂和胺类扩链剂两种的配合，以及催化剂配合的加入，制备了固化时间长，能够有充分时间大型制品的聚氨酯弹性体，适合于制备大尺寸的样品。
本发明为半预聚法配合合适的扩链剂和催化剂的新型组合来制备聚氨酯弹性体的方法。聚氨酯弹性体的制备方法克服了预聚体法中制备预聚物时的粘度过高和一步法的不稳定性的缺点，同时在半预聚体中使用胺类和醇类扩链剂的配合，制备的聚氨酯弹性体固化时间长，并且力学性能优越，耐磨性和耐油性优异。
具体实施方式
下面结合实施实例对本发明做进一步的说明。
实施例1
A组分：聚碳酸酯二醇PCL-1500(数均分子量1500)50份，聚二甲基甲基苯基硅氧烷碳二醇(数均分子量1000)2份，在120℃经氮气吹扫环境下除水2h，降至60℃时加入TDI-10040份，反应1.5h，得到游离异氰酸根含量为4％的半预聚体。
B组份：聚碳酸酯二醇PCL-1500(数均分子量1500)50份、BDO 0.5份、催化剂辛酸亚锡0.01份：
弹性体：A组分与B组份以1∶1的比例混合，在60℃下搅拌30秒后，浇注到模具中，25度下固化4h，然后80℃下后硫化8h，得到聚氨酯弹性体。
实施例2
A组分：聚碳酸酯二醇PCL-4000(数均分子量4000)100份，聚二甲基甲基苯基硅氧烷碳二醇(数均分子量4000)4份，在120℃经氮气吹扫环境下除水2h，降至75℃时加入MDI-100 70份，反应3h，得到游离异氰酸根含量为16％的半预聚体。
B组份：聚碳酸酯二醇PCL-1500(数均分子量1500)10份、二乙基甲苯二胺(DETDA)5份、催化剂N-乙基吗啉0.1份。
弹性体：A组分与B组份以1∶1的比例混合，在75℃下搅拌30秒后，浇注到模具中，30度下固化6h，然后80℃下后硫化8h，得到聚氨酯弹性体。
实施例3
A组分：聚碳酸酯二醇PCL-2000(数均分子量2000)75份，聚二甲基甲基苯基硅氧烷碳二醇(数均分子量3000)2份，在120℃经氮气吹扫环境下除水2h，降至70℃时加入MDI-5060份，反应2h，得到游离异氰酸根含量为10％的半预聚体。
B组份：聚碳酸酯二醇PCL-3000(数均分子量3000)80份、二甲硫基甲苯二胺DMTDA2份，1，6一己二醇2份、催化剂N，N，N′，N′-四甲基亚烷基二胺0.02份和二月桂酸二丁基锡0.01份。
弹性体：A组分与B组份以1∶1的比例混合，在75℃下搅拌30秒后，浇注到模具中，30度下固化5h，然后80℃下后硫化8h，得到聚氨酯弹性体。
实施例4
A组分：聚碳酸酯二醇PCL-3000(数均分子量2000)60份，聚二甲基甲基苯基硅氧烷碳二醇(数均分子量2000)3份，在120℃经氮气吹扫环境下除水2h，降至70℃时加入TDI-8065份，反应2.5h，得到游离异氰酸根含量为12％的半预聚体。
B组份：聚碳酸酯二醇PCL-2000(数均分子量2000)75份、4，4′-二氨基-3，3′-二乙基-二苯基甲烷1份，三羟甲基丙烷0.5份、催化剂N，N’-二甲基吡啶0.01份和二油酸二辛基锡0.01份；
弹性体：A组分与B组份以1∶1的比例混合，在75℃下搅拌30秒后，浇注到模具中，25度下固化5h，然后80℃下后硫化8h，得到聚氨酯弹性体。
以上实施例1-4的测试性能实验结果如表1：
表1实施例1-4的测试性能实验结果
| 项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 |
| 凝胶时间/min | 9 | 13 | 8 | 5 |
| 硬度/邵A | 72 | 40 | 61 | 85 |
| 拉伸强度/MPa | 38 | 30 | 34 | 42 |
| 撕裂强度/kN·m<sup>-1</sup> | 128 | 121 | 115 | 158 |
| 拉断伸长率/％ | 510 | 640 | 550 | 420 |
| DIN磨耗/mm<sup>3</sup> | 31 | 27 | 30 | 35 |
Claims (8)
1.一种聚氨酯弹性体的制备方法，其特征在于，包括以下步骤：
1)A组分，聚氨酯半预聚物制备方法如下：以质量份计，由聚碳酸酯二醇50-100份，聚二甲基甲基苯基硅氧烷碳二醇，2-4份，二异氰酸酯40-70份在60-75℃环境下反应1.5-3小时得到聚氨酯半预聚物；
2)B组分，制备方法：以质量份计，聚碳酸酯二醇50-100份、扩链剂0.5-5份、催化剂0.01-0.1份，混合均匀备用；
3)聚氨酯弹性体的制备过程：将B组份和A组分进行混合反应，混合温度为60-75℃，立即浇筑到模具中，在25-30℃下进行固化反应，固化4-6h后脱模，然后在80℃环境下后硫化8h，得到聚氨酯弹性体制品。
2.根据权利要求1所述的聚氨酯弹性体的制备方法，其特征在于，A组分中所述的聚碳酸酯二醇，数均分子量为1500-4000。
3.根据权利要求1所述的聚氨酯弹性体的制备方法，其特征在于，A组分中所述的聚二甲基甲基苯基硅氧烷碳二醇为羟乙氧基丙基封端聚二甲基甲基苯基硅氧烷，数均分子量为1000-4000；根据权利要求1所述的聚氨酯弹性体的制备方法，其特征在于，A组份中所述的二异氰酸酯为甲苯二异氰酸酯TDI-100，甲苯二异氰酸酯TDI-80、4，4′-二苯基甲烷二异氰酸酯MDI-100，4，4′-二苯基甲烷二异氰酸酯MDI-50，二异氰酸酯中的一种或两种的混合物。
4.根据权利要求1所述的聚氨酯弹性体的制备方法，其特征在于，A组份中，聚氨酯半预聚物中的游离异氰酸根含量为4.0％-16.0％。
5.根据权利要求1所述的聚氨酯弹性体的制备方法，其特征在于，B组份中所述的聚碳酸酯二醇数均分子量为1500-4000。
6.根据权利要求1所述的聚氨酯弹性体的制备方法，其特征在于，B组份中所述的扩链剂为胺类扩链剂和醇类扩链剂，胺类扩链剂包括4，4′-二氨基-3，3′-二乙基-二苯基甲烷，3-氯-3’-乙基-4，4’-二氨基二苯甲烷，3，3’二氯-4，4’-二氨基二苯甲烷，二乙基甲苯二胺(DETDA)，二甲硫基甲苯二胺DMTDA，二乙氨基乙醇(DEAE)，醇类扩链剂包括1，4一丁二醇(BDO)，1，6一己二醇，三羟甲基丙烷，二甘醇(DEG)，三甘醇，新戊二醇(NPG)，B组份中所述的扩链剂为醇类扩链剂和胺类扩链剂中的一种或几种的混合物，扩链剂的用量为0.5-5份。
7.根据权利要求1所述的聚氨酯弹性体的制备方法，其特征在于，B组份中所述的催化剂为锡类催化剂和胺类催化剂，锡类催化剂包括二丁酸二丁基锡、二丁酸二甲基锡、二丁酸二辛基锡、二乙酸二丁基锡、二乙酸二甲基锡、二乙酸二辛基锡、辛酸亚锡、二月桂酸二丁基锡、二月桂酸二甲基锡、二月桂酸二辛基锡、二油酸二丁基锡、二油酸二甲基锡、二油酸二辛基锡、醋酸锡、二醋酸二丁基锡、二醋酸二甲基锡、二醋酸二辛基锡、马来酸二甲基锡、马来酸二丁基锡、马来酸二辛基锡、双十二烷硫基二丁基锡、双十二烷硫基二甲基锡、双十二烷硫基二辛基锡、草酸亚锡等；胺类催化剂包括双(二甲氨基乙基)醚、五甲基二乙烯三胺、三乙烯二胺、二甲基乙醇胺、四甲基乙二胺、四甲基丙二胺、N，N-二甲基环己胺、N，N，N′，N′-四甲基亚烷基二胺、三乙胺、N，N-二甲基苄胺、三乙醇胺、N-乙基吗啉、N，N’-二乙基哌嗪、吡啶，N，N’-二甲基吡啶，B组份中所述的催化剂为锡类催化剂和胺类催化剂中的一种或几种的混合物，催化剂的用量为0.01-0.1份。
8.根据权利要求1所述的聚氨酯弹性体的制备方法，其特征在于，所制备的聚氨酯弹性体制品的硬度为邵A硬度40A-85A之间。
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