CN1152009A - 可压缩硅橡胶 - Google Patents
可压缩硅橡胶 Download PDFInfo
- Publication number
- CN1152009A CN1152009A CN96120114A CN96120114A CN1152009A CN 1152009 A CN1152009 A CN 1152009A CN 96120114 A CN96120114 A CN 96120114A CN 96120114 A CN96120114 A CN 96120114A CN 1152009 A CN1152009 A CN 1152009A
- Authority
- CN
- China
- Prior art keywords
- composition
- group
- organopolysiloxane
- preparation
- weight
- 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
- 229920002379 silicone rubber Polymers 0.000 title description 19
- 239000004945 silicone rubber Substances 0.000 title description 4
- 239000000203 mixture Substances 0.000 claims abstract description 63
- 229920001971 elastomer Polymers 0.000 claims abstract description 35
- 239000000806 elastomer Substances 0.000 claims abstract description 5
- 229920001296 polysiloxane Polymers 0.000 claims description 45
- 150000001875 compounds Chemical class 0.000 claims description 29
- 238000002360 preparation method Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 15
- 238000007789 sealing Methods 0.000 claims description 13
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- 239000002245 particle Substances 0.000 claims 1
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- 239000004033 plastic Substances 0.000 abstract description 8
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- 239000003054 catalyst Substances 0.000 description 14
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- 150000001721 carbon Chemical group 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 11
- 230000006835 compression Effects 0.000 description 10
- 238000007906 compression Methods 0.000 description 10
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- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 10
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- 238000009833 condensation Methods 0.000 description 9
- 230000005494 condensation Effects 0.000 description 9
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- 125000000753 cycloalkyl group Chemical group 0.000 description 3
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- 238000005187 foaming Methods 0.000 description 3
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- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
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- 125000002769 thiazolinyl group Chemical group 0.000 description 3
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- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 2
- RJWUMFHQJJBBOD-UHFFFAOYSA-N 2-methylheptadecane Chemical compound CCCCCCCCCCCCCCCC(C)C RJWUMFHQJJBBOD-UHFFFAOYSA-N 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- GTJVPLGQFHDOAC-UHFFFAOYSA-N C(C(=O)O)(=O)O.C(CCCCCCC)[Sn]CCCCCCCC Chemical compound C(C(=O)O)(=O)O.C(CCCCCCC)[Sn]CCCCCCCC GTJVPLGQFHDOAC-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- 239000004902 Softening Agent Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 description 2
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
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- 125000005428 anthryl group Chemical group [H]C1=C([H])C([H])=C2C([H])=C3C(*)=C([H])C([H])=C([H])C3=C([H])C2=C1[H] 0.000 description 2
- 125000003710 aryl alkyl group Chemical group 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 125000004093 cyano group Chemical group *C#N 0.000 description 2
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- 239000000975 dye Substances 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N ethyl acetate Substances CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 125000005843 halogen group Chemical group 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 2
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 2
- REOJLIXKJWXUGB-UHFFFAOYSA-N mofebutazone Chemical group O=C1C(CCCC)C(=O)NN1C1=CC=CC=C1 REOJLIXKJWXUGB-UHFFFAOYSA-N 0.000 description 2
- 125000003136 n-heptyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 2
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
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- 125000000043 benzamido group Chemical group [H]N([*])C(=O)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
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- ZPOLOEWJWXZUSP-AATRIKPKSA-N bis(prop-2-enyl) (e)-but-2-enedioate Chemical compound C=CCOC(=O)\C=C\C(=O)OCC=C ZPOLOEWJWXZUSP-AATRIKPKSA-N 0.000 description 1
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- 230000002950 deficient Effects 0.000 description 1
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- QPJORFLSOJAUNL-UHFFFAOYSA-N dibenzo[a,d][7]annulene Chemical compound C1=CC2=CC=CC=C2CC2=CC=CC=C21 QPJORFLSOJAUNL-UHFFFAOYSA-N 0.000 description 1
- QSHZUFRQHSINTB-UHFFFAOYSA-L dibutyltin(2+);dibromide Chemical compound CCCC[Sn](Br)(Br)CCCC QSHZUFRQHSINTB-UHFFFAOYSA-L 0.000 description 1
- IEPRKVQEAMIZSS-AATRIKPKSA-N diethyl fumarate Chemical compound CCOC(=O)\C=C\C(=O)OCC IEPRKVQEAMIZSS-AATRIKPKSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
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- 239000012716 precipitator Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
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- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 125000004354 sulfur functional group Chemical group 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 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 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- BYQADQLDVPAGSR-UHFFFAOYSA-N toluene;hydrobromide Chemical compound Br.CC1=CC=CC=C1 BYQADQLDVPAGSR-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
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- 239000010457 zeolite Substances 0.000 description 1
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- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种粘度为1,000-100,000mPa·s的可交联制备弹性体的组合物,该组合物基于:(A)塑料空心体;和(B)可交联的有机硅化合物。
Description
该发明是关于交联产生弹性体的组合物,其制备方法,以及由这些组合物制备的成型体和密封体以及这些成型体和密封体的制备方法。
美国专利US-A5,258,212中描述了可压缩硅橡胶。该专利中描述的可压缩硅橡胶包括空心塑料珠、玻璃或硅玻璃。这种硅橡胶用于采用一种缎带式特殊密封装置密封固定的盘槽。
美国专利US-A5,580,794中描述硅弹性体,其包括环氧树脂制备的空心珠、玻璃、金属、陶瓷及类似物质。这些弹性体用做密封材料时,据说可增强抗油和抗压性能。
美国专利US-A5,246,973描述了发泡硅弹性体。这种发泡弹性体由可热膨胀的硅弹性体和可热膨胀的空心珠的混合物制备,这些空心珠的内部含有可挥发性物质,如丁烷或异丁烷等。加热该混合物,以使挥发性物质从可膨胀的空心珠中逸出并使硅弹性体发泡。
本发明的目的是克服现有技术中的缺陷,特别是提供一种以简便、经济的方式制备和处理可压缩硅弹性体的方法。
本发明是关于有机硅组合物,这种组合物的粘度为100-100,000mPa·s,其可交联得到可压缩弹性体。该组合物基于
(A)空心塑料体和
(B)可交联的有机硅化合物
根据本发明的组合物的粘度范围是100-100,000·mPa.s,优选是1,000-60,000mPa·s,特别优选是5,000-20,000mPa·s。
作为组分I的空心塑料体(A)优选是有机聚合物,如聚丙烯腈、聚氯乙烯、聚乙酸乙烯酯、聚酯、聚碳酸酯、聚乙烯、聚苯乙烯、聚甲基丙烯酸甲酯、聚乙烯醇、乙基纤维素、硝化纤维素、苄基纤维素、环氧树脂、羟基丙基甲基纤维素邻苯二甲酸酯、氯乙烯和乙酸乙烯酯的共聚物、乙酸乙烯酯和乙酸丁酸纤维素的共聚物、马来酸和苯乙烯的共聚物、丙烯腈和苯乙烯的共聚物、偏二氯乙烯和丙烯腈及同类物的共聚物。制备这些塑料空心体的方法是已知的,如在EP-B348,272(HCASCO NOBEL AG)、US-A3,615,972,US-A4,397,799和EP-A-112807中均有描述。
塑料空心体优选是可膨胀塑料空心体,直径为1-800μm,优选是5-100μm,特别优选是10-80μm。塑料空心体在空气中的密度范围是10-100kg/m3,优选是20-80kg/m3,特别优选是20-60kg/m3。Expancel Nobel Industries公司生产的商标为Expancel 091 DE的塑料空心体是特别优选的。这些塑料空心体的用量为0.1-30%(重量),优选为0.2-10%(重量),特别优选为0.5-3%(重量)。
本发明的组合物可以是硅橡胶组合物,该组合物通过公知的加合、缩合或自由基引发交联。
本发明的通过加合交联的硅橡胶组合物包括以下组分:
(A)组分I,如上定义的塑料空心体:
(B)可交联的有机硅化合物,该化合物是以下组分的混合物:
(IIa)每分子至少有两个链烯基的聚有机硅氧烷;
(IIb)有两个Si-H端基的聚有机硅氧烷;
(III)每分子至少有两个SiH基团的作为交联剂的聚有机硅氧烷;和
(IV)作为交联剂的氢化硅烷化催化剂。
优选将是至少有两个链烯基端基的聚二甲基硅氧烷(IIa)与至少有两个Si-H端基的聚二甲基硅氧烷的混合物作为聚有机硅氢烷(II)。
本发明的硅橡胶组合物的组分(IIa)是一种每个分子至少含有两个链烯基的聚有机硅氧烷,该聚有机硅氧烷在25℃时的粘度在100-100,000mPa.s之间,优选在200-20,000mPa.s之间,特别优选是在500-5,000mPa.s之间。组分(IIa)的用量在10-98%(重量)之间,优选在20-80%(重量)之间,特别优选在50-70%(重量)之间。
本发明的硅橡胶组合物的组分(IIb)是一种每分子至少含有两个Si-H端基团的聚有机硅氧烷,这种聚有机硅氧烷在25℃时的粘度优选在100-100,000mPa.s,更优选为200-20,000mPa.s,特别优选为500-5,000mPa.s。组分(IIb)的用量优选为0-98%(重量),更优选为5-70%(重量),特别优选为20-40%(重量)。
聚有机硅氧烷(II)是由下式所示的单元所构成:
RaRb 1SiO(4-a-b)/2
其中,a是0,1或2;b是0,1,2或3,条件是每个分子中至少有两个R基团,且(a+b)<4。
R为链烯基或氢原子。所有可与具有SiH官能团的交联剂进行氢化硅烷化反应的链烯基都可选为链烯基。具有2-6个碳原子的链烯基,如:乙烯基、烯丙基、甲代烯丙基、1-丙烯基、5-己烯基、乙炔基、丁间二烯基、己二烯基、环戊烯基、环戊二烯基和环己烯基,是优选的,特别优选乙烯基和烯丙基。
R1是一个取代或非取代、具有1-10个碳原子,优选1-6个碳原子的一价脂族饱和烃基团,例如烷基,如,甲基、乙基、丙基、丁基、己基;环烷基,如,环戊基、环己基、环庚基;芳基和烷芳基,如,苯基、甲苯基、二甲苯基、米基、苄基、β-苯乙基和萘基;卤代基,如3,3,3-三氟代丙基、间-、邻-、对-氯苯基、溴甲苯基和β-氰乙基。
链烯基可以连接在聚合物链的任何位置,但优选连接在末端的硅原子上。
组分(IIa)也可以是不同的含有链烯基的聚有机硅氧烷的混合物,这些聚有机硅氧烷的不同处在于烯基团,烯基团的性质和结构。
含有链烯基的聚有机硅氧烷的结构可以是线性的、环状的和支链的。除了单官能单元,例如RR1 2SiO1/2和R1 3SiO1/2和双官能单元,如R1 2SiO2/2和RR1SiO2/2,支链的聚有机硅氧烷同样也含有三官能单元,如R1SiO3/2和RSiO3/2,和/或分子式为
SiO4/2的四官能单元,其中R和R1基团的定义已前述。三官能和四官能单元可生成支链的聚有机硅氧烷,但量非常少,如少于0.1%(摩尔),不应多于20%(摩尔)。含有链烯基的聚有机硅氧烷可以含有为通式为
-OSi(R2R3)R4Si(R2R3)O-
的单元,其中R2和R3的定义与上面给出的R和R1的定义相同,并且R4是一个双价的有机基团,如亚乙基、亚丙基、亚苯基、二亚苯基或聚氧化亚甲基。组分(II)可含有这样的单元的量最高达50%(摩尔)。
特别优选使用含有乙烯基的聚二甲基硅氧烷,其分子式相应于以下通式:
(ViMe2SiO1/2)2(ViMeSiO)a(Me2SiO)b
其中a和b为非负数,并符合下列关系:a+1>0,50<(a+b)<2200,
优选200<(a+b)<1000,
和0<(a+1)/(a+b)<0.2。
本发明的硅橡胶组合物的加合交联过程中,组分(III)作为交联剂(c),且优选是一个具有SiH官能的聚有机硅氧烷,其是由下述通式的单元构成:
HcRd 1SiO(4-c-d)/2,
其中,c是0,1,2;d是0,1,2,3,条件是(c+d)<4,且每个分子中至少有两个硅键合的氢原子。R1基团的定义和上面给出的一样。
本发明所使用的聚有机硅氧烷优选是每分子中含有三个以上的SiH键。如果所使用的组分(III)分子中仅含有两个SiH键,则聚有机硅氧烷(II)优选是每分子中至少含有三个链烯基。
聚有机硅氧烷(III)作为交联剂。除去直接连到硅原子上的氢原子,交联剂中的氢含量为0.002-1.7%(重量),优选为0.1-1.7%(重量)。
聚有机硅氧烷(III)优选是每分子中至少含有3个,不多于60个硅原子。每分子中含有4-200个硅原子的SiH交联剂是特别优选的。
聚有机硅氧烷(III)的结构可以是线性、支链、环状或网状的。线性和环状的聚有机硅氧烷(III)是由具有以下通式的单元构成的:HR1 2SiO1/2,R1 3SiO1/2,HR1SiO2/2和R1 2SiO2/2,其中R1的定义上面已给出。支链和网状结构的聚有机硅氧烷(III)还含有三官能团单元,如HSiO3/2和R1SiO3/2,和/或四官能团单元,SiO4/2。随着三官能团和/或四官能团单元量的增加,交联剂呈现出网状的树脂结构。聚有机硅氧烷的有机基团R1通常选取可与组分(II)中的有机基团相容的基团,以使组分(II)和组分(III)是可相容的。
这里描述的聚有机硅烷的组合物和混合物也可以作为交联剂。
具有下列通式的聚有机硅氧烷(III)是特别优选的:
(HR1 2SiO1/2)e(R1 3SiO1/2)f(HR1SiO2/2)g(R1 2SiO2/2)h,
其中,e、f,g和h为非负数,并遵循下列关系:(e+f)=2,(e+g)>2,5<(g+h)<200和0.12g/(g+h)≤1并且R1的定义上面已给出。
可固化的硅橡胶组合物中含有的聚有机硅氧烷的量优选是使得SiH基团与烯基团的摩尔比在0.5-5之间,更优选为1.0-3.0。
组分(III)的用量为0.1-15%(重量),优选为2-8%(重量),特别优选为3-6%(重量)。
组分(IV)作为组分(II)的链烯基和组分(III)的硅键合的氢原子的加成反应(氢化硅烷化)的催化剂。其他文献中已介绍了许多种合适的氢化硅烷化反应催化剂。原则上,所有用作硅橡胶组合物的加成交联的氢化硅烷化催化剂都可以使用。
将金属,如铂、铑、钥、钌、铱、优选铂恰当地加载到很细的载体材料(如活性碳、氧化铝或二氧化硅)上可作为氢化硅烷化的催化剂。
优选使用铂和铂化合物。可溶于聚有机硅氧烷的铂化合物是特别优选的。可使用的可溶性铂化合物有铂-烯烃配合物,分子式为(PtCl2·烯烃)2和H(PtCl3·烯烃)2,具有2-8个碳原子的烯烃,如乙烯、丙烯、丁烯和辛烯的异构体或具有5-7个碳原子的环烯烃,如环戊烯、环己烯和环庚烯是优选使用的。其他的可溶性铂催化剂是分子式(PtCl2·C3H6)2的铂-环丙烷配合物,六氯铂酸与醇、醚和醛或其混合物的反应生成物;或者是在含有碳酸氢钠的乙醇溶液中,六氯铂酸与甲基乙烯基环四硅烷的反应产物。乙烯基硅氧烷和铂的配合物,如均-二乙烯基甲基二硅氧烷是特别优选的。
氢化硅烷化烷化催化剂可采用微囊的形式,含有催化剂的细粉碎的固体不溶于聚有机硅氧烷,如热塑性塑料(聚酯树脂和硅树脂)。所使用的氢化硅烷化催化剂也可以是包含化合物,如包含在环糊精中。
氢化硅烷化催化剂的用量取决于所希望的交联速度和经济性。如果使用通常的铂催化剂,其用量以铂金属计,为可固化化硅橡胶的0.1-500ppm(重量),优选为10-100ppm(重量)。如果合适,当催化剂与阻聚剂合用时其用量优选为0.01-5%(重量)。
本发明的缩合交联的硅橡胶组合物包括以下组分:
(A)空心塑料体,即优为上述已定义的组分I;
(B)可交联的有机硅化合物,该化合物是以下组分的混合物:
(V)含有可缩合基团的聚有机硅氧烷;
(VI)作为交联剂的有机硅化合物,该化合物可与空气中的水分反应,或与聚有机硅氧烷中的OH基团反应,或填料中的OH基团反应,以及
(VII)缩合催化剂。
所述的含有可缩合基团、并按照本发明使用的有机硅化合物优选是以下通式所示的那些化合物:
R5O-[SiR6O]n-R (V)
其中,R5可以相同或不同,为氢原子或含有1-6个碳原子的烷基。R6是相同或不同的含有1-18个碳原子的烃基团,其可以选择性地被以下基团取代:卤素原子、氨基、醚基、酯基、环氧基、巯基、氰基或聚乙二醇基,后者由氧乙烯基和/或氧丙烯基构成,n是至少为30的整数。
烃基团R6的例子为烷基,如甲基、乙基、正丙基、异丙基、1-正一丁基、2-正一丁基、异丁基、叔丁基、正戊基、异戊基、新戊基、叔戊基;己基,如正己基;庚基,如正庚基;辛基,如正辛基和异辛基,如2,2,4-三甲基戊基;壬基,如正壬基;癸基,如正癸基;十二烷基,如正十二烷基;十八烷基,如正十八烷基;链烯基,如乙烯基和丙烯基;环烷基,如环戊基、环己基、环庚基和甲基环己基;芳基,如苯基、萘基、蒽基和菲基;烷芳基,如间、邻,对甲苯基,二甲苯基和乙苯基;芳烷基,如苯甲基和α-、β-代基苯乙基。
取代的烃基团R6的例子为卤代基团,如3-氯丙基,3,3,3-氟丙基,氯苯基和六氟丙基,如1-三氟甲基-2,2,2-三氟乙基;2-(全氟己基)乙基,1,1,2,2,-四氟乙氧基丙基,1-三氟甲基-2,2,2-三氟乙氧基丙基,全氟异丙氧基乙基,全氟异丙氧基丙基;氨取代基团,如N-(2-乙胺基)-3-氨丙基,3-氨丙基,3-(环己基胺基)-丙基;醚-官能基,如3-甲氧基丙基,3-乙氧基丙基;氰基-官能基,如2-氰乙基;酯-官能基,如甲基丙烯酰氧基丙基;环氧官能基,如缩水甘油氧基丙基;硫-官能基,如3-巯基丙基。
优选的R6是具有1-10碳原子的烃基团,更优选的是至少80%的R6是甲基,特别优选是至少90%的R6是甲基。
R基团优选是氢原子和具有1-4碳原子的烷基,氢原子、甲基和乙基是特别优选的。
优选如此选择分子式(V)中n的平均值以使得由分子式(V)代表的聚有机硅氧烷多分子硅醚在25℃的粘度大于30mPa.s,优选大于1000mPa.s。
虽然分子式(V)中没有表明,其中最多约有10%(摩尔)的二有机硅氧烷单元被其它的硅氧烷单元代替,这种情况经常发生,但仅以或多或少的难以避免的杂质的形式存在。这些可替代的硅氧烷单元是R6 3·SiO1/2,
R6SiO3/2和SiO4/2单元,其中R6在前面已定义过。
分子式为(V)的聚二有机硅氧烷的制备可按已知的方法进行,如由低分子量的环状或线性的由羟基和/或封端的聚有机硅氧烷聚合或缩聚制备。
有关这方面可参见学术出版公司(Academic Press Inc.)出版的作者为W.No11的“硅化学和技术”(1968)一书的第218页。
按照本发明使用的含有可缩合基团的聚有机硅氧烷,可以是单一类型的,也可以是至少有二种以上含有这种可缩合基团的聚有机硅氧烷的混合物。
聚有机硅氧烷的用量优选为10-98%(重量),更优选60-95%(重量),特别优选为80-95%(重量)。
交联剂也可以使用符合以下通式的硅氧烷:
Rb 7SiX4-b (VI)
该硅氧烷可以与空气中的水份反应,或与聚有机硅氧烷基团上的OH或填料上的OH反应。
其中,R7是单价的有机基团;
X是肟基、乙酸基、氨基、烷氧基或苯甲酰氨基;和
b是0,1,2或3。
R7基团的例子优选是选择性取代的、含有1-18个碳原子的烃基团,特别优选烷基,如甲基、乙基、正丙基、异丙基、正丁基、异丁基、叔丁基、正戊基、异戊基、新戊基和叔戊基;己基,如正己基和异己基;庚基,如正庚基和异庚基;辛基,如正辛基和异辛基,如2,2,4-三甲基戊基;壬基,如正壬基和异壬基;癸基,如正癸基和异癸基;十二烷基,如正十二烷基和异十二烷基;十八烷基,如正十八烷基和异十八烷基;链烯基,如乙烯基和烯丙基;环烷基,如环戊基,环己基、环庚基和甲基环己基;芳基,如苯基、萘基、蒽基,菲基;烷芳基,如对,邻,间甲苯基,二甲苯基,乙苯基,对-,邻-,间-乙烯基苯基、壬基苯基;芳烷基,如苄基,α-,β-苯乙基;如异氰基烷基,如异氰基丙基、异氰基乙基、异氰基己基、异氰基辛基,优选异氰基丙基;(甲基)丙烯酰氧基,如(甲基)丙烯酰氧基丙基,丙烯酰氧基丙基,优选(甲基)丙烯酰氧基丙基。
本发明所采用的催化剂是缩合催化剂,其优选是(有机)金属化合物,如金属羧酸盐、乙醇化物和卤化物,所述的金属为,例如铅、锌、锆、钛、锑、铁、镉、锡、钡、钙和锰。含有1-18个碳原子的羧酸的(有机)锡化合物和有机锡氯代物是特别优选的,特别是辛酸有机锡、环氧酸有机锡、己酸有机锡、月桂酸有机锡、乙酸有机锡、溴和氯的有机锡化合物。
此类(有机)锡化合物的例子是辛酸锡(II)、二月桂酸二丁基锡、三乙酸辛基锡、二辛酸二辛基锡、二乙酸二辛基锡、二乙酸二癸基锡、二乙酸二丁基锡、二溴二丁基锡、二月桂酸二辛基锡、乙酸三辛基锡。二羧酸二有机锡,特别是二月桂酸二丁基锡、二月桂酸二辛基锡、二乙酸二丁基锡、二乙酸二辛基锡是特别优选的。
组分(VI)的用量是0.1-15%(重量),优选1-10%(重量),优选优选2-5%(重量)。
本发明所使用的缩聚催化剂(VII)可以是一种类型或者含有至少两种此类缩聚催化剂的混合物。
为了制备本发明的组合物,缩聚催化剂(VII)的用量优选为0.01-4%(重量),更优选为0.1-3%(重量),特别优选为0.5-1.5%(重量)。
本发明的组合物也可含有其它的添加剂,因此,所述的硅橡胶组合物也可以选择性地含有其它添加剂,其用量可高达85%(重量),优选0.5-20%(重量)。这些添加剂可以是填充剂、分散辅剂、增粘剂、阻聚剂、颜料、染料、阻燃剂、增塑剂等。这些添加剂也包括石英粉、硅藻土、白土、白垩、锌钡白、炭黑、石墨、金属氧化物、碳酸盐、硫酸盐、金属粉、纤维、染料、颜料等。
填料的例子是填强型填料,如BET比表面积至少为50m2/g,优选为50-500m2/g的填料,例如热解法硅酸,其结构是脱水硅酸水凝胶,也就是所谓的“气凝胶”,该气凝胶也可以是用沉淀法得到的二氧化硅。非填强型填料,其BET比表面积小于50m2/g,例如石英粉、硅藻土、硅酸钙、硅酸锆、沸石、氧化铁、氧化锌、二氧化钛、氧化铝、碳酸钙、碳酸镁、碳酸锌、碳黑、云母和、白垩。所述填料可用上面提到的疏水剂进行疏水处理。
增塑剂的例子是二聚有机硅氧烷,该化合物在室温下是液体,如被三甲基甲硅氧端基封端的二甲基聚硅氧烷,其在25℃时的粘度为10-10,000mPa·s。
特别地,组合物可包括树脂状的聚有机硅氧烷,该聚有机硅氧烷主要是由分子式为R1 3SiO1/2、R1SiO3/2和/或SiO4/2的单元组成,如果合适还含有分子式为R1 2SiO1/2的单元,其用量相对于硅橡胶的总重可达50%(重量),优选20%(重量)。这些树脂聚有机硅氧烷中的单官能和三官能或四官能单元之间的摩尔比是0.5∶1至1.5∶1。其中也可含有官能基团,特别是链烯基团,分子式为RR1 2SiO1/2和RR1SiO2/2。
特别地,该组合物也可含有控制调节可固化橡胶组合物的加工时间和交联速度的添加剂。已知的阻聚剂和稳定剂是炔醇,如乙炔基环己醇、2-甲基-3-丁炔醇-2,聚甲基乙烯基环硅氧烷,如甲基乙烯基环四硅氧烷,带有乙烯基二甲基甲硅氧基的低分子硅氧烷油;氰尿酸三甲基酯、马来酸烷基酯,如马来酸二烯丙基酯、马来酸二甲基酯;富马酸烷基酯,如富马酸二乙基酯和富马酸二烯丙基酯;有机氢过氧化物,如异丙基苯氢过氧化物,叔丁基氢过氧化物、哌烷氢过氧化物;有机过氧化物,苯并三唑,有机亚砜、有机胺、酰胺、膦、亚磷酸盐、腈、二氮丙啶、肟。
本发明还进一步涉及本发明的组合物的制备方法。
本发明的组合物的制备是采用通常制备硅橡胶组合物的方法,即混合1-组分或2-组分(1-C或2-C)。
本发明的组合物是用通常的1-C或2-C混合和计量装置来加工。
缩合交联化合物优选在25℃的室温下进行交联。
加成交联化合物交联条件是温度为25-200℃,交联时间为5分钟至24小时。温度优选为100-150℃,时间为5分钟至1小时。
本发明进一步涉及由本发明的组合物、由本发明的制备方法制备的组合物制得的可压缩成形物品、密封体、包埋组合物及其制备方法。
本发明的组合物可用于加工成包埋化合物和成形制品,如密封体,如O-形环、圆形线和片。这些O-形环,圆形线和片特别适用于温度在65°-250℃变化的场合。这样的温度变化通常发生在机械或车辆运行中,由于其操作或外界温度变化导致温度升高。其应用于所有有火花发动机的机器如车辆,如摩托车、建筑机械和长时间运转的机器,如发动机等。
本发明的组合物的优点是相对于没有空心塑料体的硅橡胶而言,具有高的可压缩性。压缩性比没有空心塑料体的硅橡胶要大20-40倍。
结果是比较低的压力可产生较紧的密封效果。另一个优点是高的可压缩性可以减少温度变化时所产生的热应力。因为虽然加热时膨胀的程度与传统的组合物相同,但它遇到阻力时会压缩而不会进一步增加与被密封面之间的距离,所以当温度回落到膨胀前的温度时,密封仍完好无损。这意味着当温度改变时密封不受影响。这样的密封体在温度升高时不会损坏垫圈,如使垫圈开裂。在这种情况下,本发明的组合物将会压缩。
本发明的组合物的另一个优点是它可以很容易地被浇铸,而不需要复杂、昂贵的机器。例如,一个二组分发泡体,可用一个简单的方法,如1-C计量装置,通过二组分发泡料引入模具而在使用位置制备一个O形密封环,即使模具拆除后,发泡体仍然保持在原位。这种措施可以防止O-形环在不注意时脱离、没有O形环时重新安装以及没有O形环时再次损坏。O型环脱落可导致不必要的静置时间。例如,摩托车电瓶中用于密封电瓶以防潮气的O形环脱落时,潮气进入电瓶中,从而使电瓶不再起作用,由此导致汽车发动不起来。
本发明组合物可进一步用于制备包埋组合物。这种组合物可用于包埋电子元件。尽管硅氧烷和一般硅氧烷化合物一样有较高的热膨胀系数,本发明的组合物的另一个优点是由于它的可压缩性,即使当温度发生变化时,其也不会损坏电子元件。
本发明的组合物的另一优点是与一般硅氧烷化合物相比有特别低的密度,这样可减轻元件的重量。这一特点应用于汽车上可有助于节约燃料。
本发明的加成交联组合物的一个显著特点是通过采用末端具有Si-H基团的二甲基聚硅氧烷(IIb)可随意调节化合物的肖氏硬度。0-50范围内的硝氏硬度可通过调节二甲基聚硅氧烷(IIa、IIb)的比例来实现。不同的方式可产生不同的密封作用。
实施例实施例1
80份粘度为1,000mPa·s,每个分子末端有硅-羟基的二甲基聚硅氧烷顺次与10份在气相中制备的、BET比表面为200m2/g的二氧化硅,和1份Expancel1 DE91、5份肟硅烷、、0.6份的氨硅烷和0.6份缩聚催化剂混合,制得一种自由流动的、粘度为30,000mPa·s的可隔水保存的RTV-1硅橡胶。
通入大气中的潮气即可制得可压缩的固化橡胶。
下面的数值是在室温下测定放置28天,6mm厚的固化橡胶的数值:
密度:0.8g/cm3
肖氏硬度A:26
压缩固化橡胶5%所需的力:1.6N/mm2
压缩固化橡胶25%所需的力:9N/,mm2
比较实施例1
采用与实施例1同样方法制备同样的化合物,但化合物中不包含Expancell DE91,得到粘度为10,000mPa·s,可自由流动,可隔水保存的硅橡胶,下面的数据是在室温下测定6mm厚,放置14天的固化橡胶:
肖氏硬度A:25
压缩固化橡胶5%所需的力:10N/mm2
压缩固化橡胶25%所需的力:不可能
实施例2
63份末端含有乙烯基、粘度为1000mPa·s的二甲基聚硅氧烷、30份末端含有Si-H,粘度为1,000mPa·s的二甲基聚硅氧烷、2份Expancell DE91、0.5份乙炔基环己醇、0.2份铂催化剂和5份聚甲基氢化硅氧烷充分混合,制得由流动、粘度为6,000mPas·的加成交联硅橡胶。这种硅橡胶在室温下可稳定储存6个月,加热时交联产生可压缩固化橡胶。
下面是测定20mm厚、在150℃下固化一小时的固化橡胶的数据:
密度:0.6g/cm3
肖氏硬度A:8
压缩固化橡胶5%所需的力:0.3N/mm2
压缩固化橡胶25%所需的力:1.7N/,mm2比较例2
采用实施例2的方法制备同样的化合物,但化合物中不含Expancell DE91,得到可自由流动、粘度为1,000mPa·s的加成交联硅橡胶。该硅橡胶在室温下可放置6个月,加热时产生可压缩固化橡胶。
下面是测定20mm厚、在150℃下硫化一小时的固化橡胶的数据:
密度:1.0g/cm3
肖氏硬度A:8
压缩固化橡胶5%所需的力:6N/mm2
压缩固化橡胶25%所需的力:不可能
比较例3
采用实施例2的方法制备同样的化合物,但化合物中不含分子末端含有Si-H键的二甲基聚硅氧烷,得到可自由流动,粘度为6,000mPa·s的加成交联硅橡胶。该硅橡胶在室温下可放置6个月,加热时交联得到可压缩固化橡胶。
下面是测定20mm厚、150℃下固化一小时的固化橡胶的数据:
密度:0.6g/cm3
肖氏硬度A:28
压缩固化橡胶5%所需的力:1N/mm2
压缩固化橡胶25%所需的力:5N/mm2
Claims (7)
1、一种粘度为1,000-100,000、可交联产生弹性体的组合物,该组合物基于
(A)塑料空心体;
(B)可交联的有硅氧烷化合物。
2、如权利要求1所述的组合物,其特征在于所述的塑料空心体(A)的密度为10-80kg/m3,粒子大小为5-200μm;
3、制备如权利要求1或权利要求2所述的可交联产生弹性体的组合物的方法,包括将组分A和组分B混合。
4、由权利要求1或权利要求2所述的组合物或由权利要求3所述的方法制备的组合物制备的成型制品、密封体或包埋组合物。
5、如权利要求4所述的成形体、密封体、包埋化合物的制备方法,包括将权利要求1或权利要求2所述的组合物或由权利要求3所述的制备方法制备的组合物注入模具中。
6、如权利要求5所述密封体的制备方法,其特征在于所述的模具是槽;
7、如权利要求1至权利要求3中一项或多项所述的组合物用于制备成型体、密封体或包埋化合物。
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DE19540886A DE19540886A1 (de) | 1995-11-02 | 1995-11-02 | Kompressibler Siliconkautschuk |
DE19540886.1 | 1995-11-02 |
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US (1) | US5750581A (zh) |
EP (1) | EP0771842A1 (zh) |
JP (1) | JP2980852B2 (zh) |
KR (1) | KR100197347B1 (zh) |
CN (1) | CN1073602C (zh) |
CA (1) | CA2187263C (zh) |
DE (1) | DE19540886A1 (zh) |
TW (1) | TW362105B (zh) |
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- 1996-10-01 US US08/724,387 patent/US5750581A/en not_active Expired - Lifetime
- 1996-10-07 CA CA002187263A patent/CA2187263C/en not_active Expired - Fee Related
- 1996-10-14 JP JP8270821A patent/JP2980852B2/ja not_active Expired - Lifetime
- 1996-10-24 EP EP96117061A patent/EP0771842A1/de not_active Ceased
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CN1302215C (zh) * | 2000-03-07 | 2007-02-28 | 三菱自动车工业株式会社 | 摇臂罩的密封方法 |
CN101177530B (zh) * | 2006-06-07 | 2011-08-10 | 信越化学工业株式会社 | 消光用液体有机聚硅氧烷组合物和具有消光表面的固化制品 |
CN101802101B (zh) * | 2007-09-20 | 2012-08-08 | Abb研究有限公司 | 电气绝缘设备和具有该电气绝缘设备的电气设备 |
TWI569959B (zh) * | 2012-05-22 | 2017-02-11 | Sekisui Chemical Co Ltd | Sheet seal and laminated sheet seal |
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US5750581A (en) | 1998-05-12 |
CN1073602C (zh) | 2001-10-24 |
JPH09137063A (ja) | 1997-05-27 |
CA2187263A1 (en) | 1997-05-03 |
CA2187263C (en) | 2000-12-12 |
DE19540886A1 (de) | 1997-05-07 |
KR970027647A (ko) | 1997-06-24 |
KR100197347B1 (ko) | 1999-06-15 |
EP0771842A1 (de) | 1997-05-07 |
JP2980852B2 (ja) | 1999-11-22 |
TW362105B (en) | 1999-06-21 |
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