CN102827479A - Liquid silicone rubber - Google Patents
Liquid silicone rubber Download PDFInfo
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- CN102827479A CN102827479A CN2012102965310A CN201210296531A CN102827479A CN 102827479 A CN102827479 A CN 102827479A CN 2012102965310 A CN2012102965310 A CN 2012102965310A CN 201210296531 A CN201210296531 A CN 201210296531A CN 102827479 A CN102827479 A CN 102827479A
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- carbon black
- white carbon
- weight
- liquid silastic
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- 229920002379 silicone rubber Polymers 0.000 title abstract description 35
- 239000004944 Liquid Silicone Rubber Substances 0.000 title abstract 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000006229 carbon black Substances 0.000 claims abstract description 42
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 26
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 125000000304 alkynyl group Chemical group 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 47
- 229920000260 silastic Polymers 0.000 claims description 22
- 238000004513 sizing Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 15
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 12
- 229920002554 vinyl polymer Polymers 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 239000002512 suppressor factor Substances 0.000 claims description 9
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 5
- 229910052736 halogen Inorganic materials 0.000 claims description 4
- 150000002367 halogens Chemical class 0.000 claims description 4
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 4
- 150000001345 alkine derivatives Chemical class 0.000 claims description 3
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims description 3
- KWEKXPWNFQBJAY-UHFFFAOYSA-N (dimethyl-$l^{3}-silanyl)oxy-dimethylsilicon Chemical compound C[Si](C)O[Si](C)C KWEKXPWNFQBJAY-UHFFFAOYSA-N 0.000 claims description 2
- 239000004215 Carbon black (E152) Substances 0.000 claims description 2
- 229910018540 Si C Inorganic materials 0.000 claims description 2
- UFPSGVDBVFTGTR-UHFFFAOYSA-N [Pt].CC1=CCCC=C(CC1)C Chemical compound [Pt].CC1=CCCC=C(CC1)C UFPSGVDBVFTGTR-UHFFFAOYSA-N 0.000 claims description 2
- BUEPLEYBAVCXJE-UHFFFAOYSA-N [ethenyl-methyl-(trimethylsilylamino)silyl]ethene Chemical compound C(=C)[Si](N[Si](C)(C)C)(C=C)C BUEPLEYBAVCXJE-UHFFFAOYSA-N 0.000 claims description 2
- 229910014307 bSiO Inorganic materials 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- JAGYXYUAYDLKNO-UHFFFAOYSA-N hepta-2,5-diene Chemical compound CC=CCC=CC JAGYXYUAYDLKNO-UHFFFAOYSA-N 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 2
- 125000001261 isocyanato group Chemical group *N=C=O 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 14
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000003112 inhibitor Substances 0.000 abstract description 2
- 239000004945 silicone rubber Substances 0.000 abstract 2
- 241000907661 Pieris rapae Species 0.000 abstract 1
- 230000006866 deterioration Effects 0.000 abstract 1
- 239000012763 reinforcing filler Substances 0.000 abstract 1
- 235000019241 carbon black Nutrition 0.000 description 34
- -1 siloxanes Chemical class 0.000 description 20
- 238000001723 curing Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- RCNRJBWHLARWRP-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane;platinum Chemical compound [Pt].C=C[Si](C)(C)O[Si](C)(C)C=C RCNRJBWHLARWRP-UHFFFAOYSA-N 0.000 description 5
- 230000001404 mediated effect Effects 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 229910004283 SiO 4 Inorganic materials 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 241000872198 Serjania polyphylla Species 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 150000005840 aryl radicals Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- 125000002769 thiazolinyl group Chemical group 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 1
- 125000006017 1-propenyl group Chemical group 0.000 description 1
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- MCAPDUSPBSEQQO-UHFFFAOYSA-N O1[SiH2]O[SiH2]O[SiH2]O[SiH2]1.CC=C Chemical compound O1[SiH2]O[SiH2]O[SiH2]O[SiH2]1.CC=C MCAPDUSPBSEQQO-UHFFFAOYSA-N 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- FSIJKGMIQTVTNP-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C=C)C=C FSIJKGMIQTVTNP-UHFFFAOYSA-N 0.000 description 1
- 210000005252 bulbus oculi Anatomy 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 150000001925 cycloalkenes Chemical class 0.000 description 1
- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 description 1
- 150000001941 cyclopentenes Chemical class 0.000 description 1
- 125000002704 decyl 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])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 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
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 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 1
- 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 1
- 150000002432 hydroperoxides Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 125000001400 nonyl 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])C([H])([H])[H] 0.000 description 1
- 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 1
- 239000003921 oil Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000005504 styryl group Chemical group 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to liquid silicone rubber. The liquid silicone rubber is prepared by uniformly mixing an aliphatic unsaturated group-containing organopolysiloxane, a silicon-hydrogen-bonded organopolysiloxane, white carbon black, a platinum catalyst and an alkynyl-containing inhibitor and carrying out heating curing of the mixture at a temperature of 130 to 200 DEG C. White carbon black of which the surface is treated by hexamethyldisilazane and one or more silane coupling agents is used as a reinforcing filler of the liquid silicone rubber and is mixed with other components well so that a silicone rubber net structure is changed and the liquid silicone rubber is obtained. The liquid silicone rubber has large tearing strength, enlarges a liquid silicone rubber application range, can be stored for a long time without deterioration and improves a silicone rubber service life.
Description
Technical field
The present invention relates to the Zylox field, be specifically related to the high anti-tear liquid silastic of a kind of add-on type.
Background technology
The high anti-tear Zylox of add-on type liquid (can be described as LSR or LSE) is the higher veriety of class in the Zylox.At first, addition-type silicon rubber and condensed type Zylox relatively, it have sulfidation do not produce by product, shrinking percentage minimum, can deep layer vulcanization etc. advantage, stopping property at high temperature is also better than the condensed type.Secondly, add-on type liquid silicon rubber also has an outstanding advantage: technology is easy, with low cost.This is because the liquid silastic molecular weight is little, viscosity is low, machine-shaping is convenient, can save operations such as mixing, premolding, arrangement afterwards, realizes robotization easily, and can save the energy and labor force, and is with short production cycle and efficient is high.So though the cost of material of add-on type liquid silicon rubber is slightly higher than ordinary silicon rubber, total cost is lower than ordinary silicon rubber, more shows its meliority in this respect when particularly making the smallclothes product.And higher at high anti-tear Zylox of aspect add-on type liquids such as preparation insulator, cold shrink tube, electric wire and cable jackets than common liq Zylox tearing toughness, effectively raise work-ing life of goods.
Summary of the invention
In order further to improve the tearing toughness of existing liquid silastic, the purpose of this invention is to provide the high anti-tear liquid silastic of a kind of add-on type.
Liquid silastic provided by the invention, under 130～200 ℃, being heating and curing after being mixed by following component by weight makes:
(ⅰ) contain organopolysiloxane 50～300 weight parts of two or more unsaturated group of aliphatic series;
(ⅱ) contain organopolysiloxane 0.1～20 weight part of silicon keyed jointing Wasserstoffatoms;
(ⅲ) WHITE CARBON BLACK 1～100 weight part;
(ⅳ) platinum catalyst 0.001～0.1 weight part;
(ⅴ) contain the alkynyl suppressor factor, its content is the alkynyl group that each Pt atom pairs is answered 1～100mol in the said platinum catalyst.
The described WHITE CARBON BLACK of component (ⅲ) can be precipitated silica or thermal silica or the mixture of the two, and with the surface of BET method mensuration WHITE CARBON BLACK filler, the specific surface area of these WHITE CARBON BLACKs is at least 50m
2/ g is preferably 50～500m
2/ g, more preferably 200～400m
2/ g.
When said WHITE CARBON BLACK is hydrophobic silicic aerogels, is easy to mix and increases not too large depositing the process medium viscosity with component (ⅰ).Therefore, the WHITE CARBON BLACK after WHITE CARBON BLACK is preferably and handles with hexamethyldisilazane, the consumption of said hexamethyldisilazane is 10～50% of a WHITE CARBON BLACK weight.
(CH
3)
3SiNHSi (CH
3)
3In Si-NH-Si under proper condition hydrolyzable form Si-OH, again with the WHITE CARBON BLACK surface-OH carries out condensation, thereby can improve the consistency of organic materials and inorganic materials in the liquid silastic component.
In order further to improve the performance of Zylox, said WHITE CARBON BLACK also adopts the silane coupling agent that contains vinyl to handle, and the said dosage of silane coupling agent that contains vinyl is 0.1～15% of a WHITE CARBON BLACK weight, and preferred 1～10%.
The said silane coupling agent that contains vinyl is selected from one or more in vinyltrimethoxy silane, vinyltriethoxysilane, the tetramethyl divinyl disilazane.
The silane coupling agent that the surface hydroxyl of WHITE CARBON BLACK is contained vinyl replaces; Vinyl and hydrogen-containing siloxane carry out addition; The siloxanes that contains vinyl also can be crosslinked with hydrogen-containing siloxane; Thereby making WHITE CARBON BLACK is not only reinforced filling, has also participated in the network structure of Zylox, makes the Zylox tear resistance after the curing better.
The surface treatment method of WHITE CARBON BLACK is: WHITE CARBON BLACK and hexamethyldisilazane and/or the silane coupling agent that contains vinyl are mixed, stirred 1-5 hour, can under normal temperature, normal pressure, carry out, for accelerating treatment progress, also can suitably heat, pressurize.
Component (ⅰ) is the organopolysiloxane of linearity, ring-type or collateralization that structural unit constituted shown in the following formula, and its molar mass is 10
2～10
5G/mol:
R
aR
1 bSiO
(4-a-b)/2
Wherein, R be halogen ,-CN ,-SCN ,-replacement or the non-substituted hydrocarbon radical of NCO or C1～C18;
R
1Replacement or non-substituted olefine base or alkynes base for the C2～C10 of Si-C keyed jointing;
A is that 0～3 integer, b are 0～2 integer, and a+b≤3.
Specifically; R can be identical or different; Said alkyl comprises aliphatic group and aryl radical; Said aliphatic group can be methyl, ethyl, n-propyl, sec.-propyl, normal-butyl, isobutyl-, the tertiary butyl, normal-butyl, isobutyl-, isopentyl, neo-pentyl, tert-pentyl, hexyl, heptyl, octyl group, nonyl, decyl etc.; Said aryl radical can be phenyl, benzyl etc.; Preferred alkyl is aliphatic group or the phenyl of C1 ~ C6; More preferably methyl or phenyl.
R
1Be preferably vinyl, propenyl, methylallyl, 1-propenyl, ethynyl, butadienyl, hexadienyl, ethenylphenyl or styryl etc.
The organopolysiloxane of component (ⅰ) can be the lower alkylene ZGK 5 of relative molecular weight, also can be on the chain or the end of the chain has the height polymeric YSR 3286 of two silicon keyed jointing vinyl at least; Structure oligomeric or the height polymer siloxane can be the structure of linearity, ring-type or collateralization, also can be similar branch or netted structure.Linear perhaps cyclic polysiloxanes is mainly by formula R
3SiO
1/2, R
2R
1SiO
1/2, R
1RSiO
2/2Or R
2SiO
2/2Structural unit constitute; R wherein
1, R defines as above.Collateralization or netted ZGK 5 also comprise trifunctional or four functional unit, as by formula RSiO
3/2, R
1SiO
3/2Or SiO
4/2Structural unit; R wherein
1, R defines as above.Can certainly use the mixture of any different silicones that satisfies the said standard of component (ⅰ).
Component (ⅰ) most preferably is linear polysiloxane viscosity in 1mPas ~ 10
5The polydiorganosiloxane of mPas (temperature 25 ℃ time).
Component (ⅱ) is the organopolysiloxane that structural unit shown in the following formula constitutes:
R
cH
dSiO
(4-c-d)/2
Wherein, R be halogen ,-CN ,-SCN ,-replacement or the non-replacement saturated hydrocarbyl of NCO, phenyl, benzyl or C1～C18;
C is 0～3 integer, and d is 0～2 integer, and c+d≤3;
On average contain 3 silicon keyed jointing Wasserstoffatomss in each molecule at least; Its molar mass is 10
2～10
5G/mol;
Described organopolysiloxane preferably contains the silicon keyed jointing Wasserstoffatoms of 0.1～1.6 weight %.
The organopolysiloxane of said component (ⅱ) can be the functional oligosiloxane of low-molecular-weight relatively SiH, like tetramethyl disiloxane; Also can be on chain or the end of the chain has the height polymeric YSR 3286 of SiH group, also can use any existing ability to satisfy the different silicones mixture that solidifies the back standard of performance certainly.The organopolysiloxane usage quantity of component (ⅱ) must make the SiH group to the mol ratio of all unsaturated group of aliphatic series in the Zylox composition between 1 to 10.
Component (ⅱ) most preferably is linear polysiloxane viscosity in 1mPas ~ 10
4The organopolysiloxane of mPas (temperature 25 ℃ time).
The described platinum catalyst of component (ⅳ) is compatible platinic compound in organopolysiloxane preferably, can use the example of solvable platinic compound to be formula (PtCl. alkene)
2And platinum-olefin(e)complex of H (PtCl. alkene).Alkene preferably uses the alkene with 2 to 8 carbon atoms, for example ethene, propylene, butylene and octene etc. and isomers thereof; The cycloolefin that perhaps has 5 to 7 carbon atoms.For example cyclopentenes, tetrahydrobenzene and suberene.Other soluble platinum catalysts are formula (PtCl
2C
3H
6)
2Platinum-Trimetylene title complex; The reactant of chloroplatinic acid and alcohol, ether, aldehyde and composition thereof; Perhaps chloroplatinic acid and the reactant of methyl ethylene cyclotetrasiloxane under the sodium hydrogencarbonate existence condition in ethanolic soln.The title complex of especially preferred platinum and vinylsiloxane, for example 1,3-divinyl-1,1; 3,3-tetramethyl disiloxane platinum complex or 1,3,5; 7-tetrem thiazolinyl-1,3,5,7; The title complex of-tetramethyl-ring siloxanes has good consistency and higher hydrosilation reaction activity, and better preserve stability is arranged in the Zylox composition.
Preferably, component (ⅳ) is selected from 1,3-divinyl-1; 1,3,3-tetramethyl disiloxane platinum complex, two (alkynyls) (1; The 5-cyclooctadiene) platinum complex, two (alkynyl) (two ring [2.2.1] heptan-2,5-diene) platinum complex, two (alkynyl) (1,5-dimethyl--1; The 5-cyclooctadiene) platinum complex or two (alkynyl) (1,6-dimethyl--1,5-cyclooctadiene) platinum complex.
The usage quantity of platinum catalyst depends on the factors such as service condition of rate of crosslinking and economic and each component, and it is (one of per 1,000,000 weight parts of ppm=weight part) between 2 to 5000 ppm by weight that the curable organic ZGK 5 of per 100 weight parts uses the amount of platinum catalyst usually.
Component (ⅴ) is described to contain process period, initial temperature and the rate of crosslinking that the alkynes suppressor factor is used for regulating and controlling Zylox of the present invention.Suppressor factor commonly used is an alkynol class suppressor factor, for example 1-ethynyl-1-hexalin, 2-methyl-3-butyne-2-alcohol or 3,5-dimethyl--1-hexin-3-alcohol; Gather the methyl ethylene cyclosiloxane, as 1,3,5,7-tetrem thiazolinyl tetramethyl-ring siloxanes; Has methyl ethylene SiO
2/2Group and or R
2Vinyl SiO
1/2The low-molecular-weight siloxane oil of end group, for example divinyl tetramethyl disiloxane, tetrem thiazolinyl dimethyl-sily oxide; Organic hydroperoxide is like cumene hydroperoxide; Organo-peroxide; Organic sulfoxide; Organic amine; Acid amides; Phosphoric acid salt; Eyeball; Two Soluol XC 100 etc.
Preferably, component (ⅴ) is selected from 1-ethynyl-1-hexalin, 2-methyl-3-butyne-2-alcohol, 3,5-dimethyl--1-hexin-3-alcohol or gather the methyl ethylene cyclosiloxane.
Alkynol class suppressor factor in use has volatile shortcoming, and is volatile owing to alkynol in the mixing deaeration process before particularly two components use, and has the surperficial first sulfuration of linking agent can cause the accordion unfairness, influences outward appearance.When being used for the single-component of requirement stable for extended periods of time property; Because the increase of use level has the problem of and sulfuration property variation bad with the sizing material consistency; For this reason; Can be through with the alkynol silylanization, the alkynes-oxyl be introduced siloxane structure or with other suppressor factor and method improvement alkynol class inhibitor structure such as use, thus its performance improved, and said method can adopt the existing method of any this area.
Comprehensive above-mentioned consideration, liquid silastic provided by the invention are preferably composed of the following components by weight:
(ⅰ) contain organopolysiloxane 100～300 weight parts of two or more unsaturated group of aliphatic series;
(ⅱ) contain organopolysiloxane 1～10 weight part of silicon keyed jointing Wasserstoffatoms;
(ⅲ) WHITE CARBON BLACK 10～100 weight parts, its specific surface area is 50～500m
2/ g is preferably 200～400m
2/ g;
(ⅳ) platinum catalyst 0.001～0.1 weight part;
(ⅴ) contain alkynyl suppressor factor 0.01～0.1 weight part.
Preferably, the process that under 130～200 ℃, is heating and curing of back that mixes according to the invention is: with component (ⅰ) and (ⅲ) mix and obtain sizing; Get mass percent and be in 40～60% the said sizing and add component (ⅳ), stirring, it is subsequent use to make component (A); Add component (ⅱ) and (ⅴ) in the sizing in residue, it is subsequent use for making component (B) to stir; Component (A) and component (B) are mixed, and under 130～200 ℃, being heating and curing promptly gets.
Mixing in the above-mentioned process that is heating and curing, process step such as stir, be heating and curing all adopt this area prior art.
Liquid silastic provided by the invention; Adopted WHITE CARBON BLACK that WHITE CARBON BLACK, especially surface handle through hexamethyldisilazane and silane coupling agent as reinforced filling; Can mix well with all the other components; Changed the network structure of Zylox, the liquid silastic product tearing toughness that obtains is big, can reach more than the 30KN/m.The increase of tearing toughness can enlarge the range of application of liquid silicon rubber material.And liquid silastic product long storage time provided by the invention is not perishable, the work-ing life of having improved rubber.In addition, various added ingredientss source is easy to get, and the preparation method is easy, has excellent industrial applications prospect.
Embodiment
Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.
Embodiment 1
In WHITE CARBON BLACK, add the hexamethyldisilazane of 20wt% and the vinyltriethoxysilane of 1.5wt%, mixed under normal temperature, the normal pressure 2-3 hour.
In vacuum kneader, add 200 weight part α; (viscosity is 10000mPas to ε-vinyl-dimethyl base YSR 3286; 25 ℃), add 60 parts of WHITE CARBON BLACK (specific surface area 300m that handle with 20wt% (calculating) hexamethyldisilazane and 1.5wt% (calculating) vinyltriethoxysilane with WHITE CARBON BLACK with WHITE CARBON BLACK
2/ g) mix, be warming up to 150 ℃, heating was mediated 2 hours, took off low molecule 2 hours through vacuum, and cooling is filtered after three-roller grinds, and obtains liquid silicon rubber sizing at last.
In 130 weight part liquid silicon rubber sizings, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part stirs, and de-bubbled is filtered, and makes component (A).
In 130 weight part liquid silicon rubber sizings, add polymethyl hydrogen siloxane (viscosity 50mPas, 25 ℃; H%=0.8%) 2.0 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part at room temperature mixes de-bubbled; Filter, make component (B).
Component (A) and component (B) the quality proportioning according to 1:1 is mixed, be expelled in the mould, being heating and curing under 160 ℃ forms liquid silicon rubber material, at 160 ℃ of following mold pressing 10min, processes the thick film of 6mm and 2mm.
Embodiment 2
In vacuum kneader, add 200 weight part α; (viscosity is 15000mPas to ε-vinyl-dimethyl base YSR 3286; 25 ℃), add WHITE CARBON BLACK (the specific surface area 300m that 70 parts of usefulness 20% (calculating with WHITE CARBON BLACK) hexamethyldisilazanes and 2.5% (calculating with WHITE CARBON BLACK) vinyltriethoxysilane is handled
2/ g) (treatment process is with embodiment 1) mix, be warming up to 150 ℃, heating was mediated 2 hours, took off low molecule 2 hours through vacuum, cooling is filtered after three-roller grinds.Obtain liquid silicon rubber sizing at last.
In 135 weight part liquid silicon rubber sizings, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part stirs, and de-bubbled is filtered, and makes component (A).
In 135 weight part liquid silicon rubber sizings, add polymethyl hydrogen siloxane (viscosity 50mPas, 25 ℃; H%=0.9%) 3.0 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 mass parts at room temperature mixes de-bubbled; Advance to filter, make component (B).
Component (A) and component (B) the quality proportioning according to 1:1 is mixed, be expelled in the mould, being heating and curing under 170 ℃ forms liquid silicon rubber material, at 170 ℃ of following mold pressing 10min, processes the thick film of 6mm and 2mm.
Embodiment 3
In vacuum kneader, add 200 weight part α; (viscosity is 8000mPas to ε-vinyl-dimethyl base YSR 3286; 25 ℃), add WHITE CARBON BLACK (the specific surface area 300m that 70 parts of usefulness 20% (calculating with WHITE CARBON BLACK) hexamethyldisilazanes and 3.0% (calculating with WHITE CARBON BLACK) vinyltriethoxysilane is handled
2/ g) (treatment process is with embodiment 1) mix, be warming up to 150 ℃, heating was mediated 2 hours, took off low molecule 2 hours through vacuum, cooling is filtered after three-roller grinds.Obtain liquid silicon rubber sizing at last.
In 130 weight part liquid silicon rubber sizings, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part stirs, and de-bubbled is filtered, and makes component (A).
In 140 weight part liquid silicon rubber sizings, add polymethyl hydrogen siloxane (viscosity 50mPas, 25 ℃; H%=1.0%) 3.2 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part at room temperature mixes de-bubbled; Advance to filter, make component (B).
Component (A) and component (B) the quality proportioning according to 1:1 is mixed, be expelled in the mould, being heating and curing under 190 ℃ forms liquid silicon rubber material, at 190 ℃ of following mold pressing 10min, processes the thick film of 6mm and 2mm.
Embodiment 4
In vacuum kneader, add 200 weight part α; (viscosity is 10000mPas to ε-vinyl-dimethyl base YSR 3286; 25 ℃), add 60 parts of WHITE CARBON BLACK (specific surface area 300m that handle with 20wt% (calculating) hexamethyldisilazane and 1.5wt% (calculating) vinyltriethoxysilane with WHITE CARBON BLACK with WHITE CARBON BLACK
2/ g) (treatment process is with embodiment 1) mix, be warming up to 150 ℃, heating was mediated 2 hours, took off low molecule 2 hours through vacuum, cooling is filtered after three-roller grinds, and obtains liquid silicon rubber sizing at last.
In 120 weight part liquid silicon rubber sizings, { its molecular structure is [(CH to add 5 weight part ZGK 5
3)
3SiO
1/2]
m[(CH
3)
2(CH
2=CH) SiO
1/2]
n[SiO
4/2]
z((m+n)/z=0.7 wherein, z=30) contents of ethylene is that 0.36%} adds 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part stirs, and de-bubbled is filtered, and makes component (A).
In 140 weight part liquid silicon rubber sizings, add polymethyl hydrogen siloxane (viscosity 50mPas, 25 ℃; H%=1.0%) 3.2 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part at room temperature mixes; De-bubbled is advanced to filter, and makes component (B).
Component (A) and component (B) the quality proportioning according to 1:1 is mixed, be expelled in the mould, being heating and curing under 170 ℃ forms liquid silicon rubber material, at 170 ℃ of following mold pressing 10min, processes the thick film of 6mm and 2mm.
Embodiment 5
In vacuum kneader, add 200 weight part α; (viscosity is 10000mPas to ε-vinyl-dimethyl base YSR 3286; 25 ℃), add 60 parts of WHITE CARBON BLACK (specific surface area 300m that handle with 20wt% (calculating) hexamethyldisilazane and 1.5wt% (calculating) vinyltriethoxysilane with WHITE CARBON BLACK with WHITE CARBON BLACK
2/ g) (treatment process is with embodiment 1) mix, be warming up to 150 ℃, heating was mediated 2 hours, took off low molecule 2 hours through vacuum, cooling is filtered after three-roller grinds, and obtains liquid silicon rubber sizing at last.
In 130 weight part liquid silicon rubber sizings, { its molecular structure is [(CH to add 3 weight part ZGK 5
3)
3SiO
1/2]
m[(CH
3)
2(CH
2=CH) SiO
1/2]
n[SiO
4/2]
z((m+n)/z=0.7 wherein, z=30) contents of ethylene is that 0.36%} adds 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part stirs, and de-bubbled is filtered, and makes component (A).
In 130 weight part liquid silicon rubber sizings, { its molecular structure is [(CH to add the 3.0g ZGK 5
3)
2HSiO
1/2]
m[SiO
4/2]
z, m/z=1.8 in the formula, z=35) H% is 0.99%} weight part and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mixes, de-bubbled is advanced to filter, and makes component (B).
Component (A) and component (B) the quality proportioning according to 1:1 is mixed, be expelled in the mould, being heating and curing under 170 ℃ forms liquid silicon rubber material, at 170 ℃ of following mold pressing 10min, processes the thick film of 6mm and 2mm.
The film that 6mm among the embodiment 1-5 is thick is used for test (standard GB/T531.1-2008) experiment of hardness, and the film that 2mm is thick is used for the physical mechanical property, and experimental result is seen table 1.
Table 1 physical and mechanical properties test-results
Though, the present invention has been done detailed description in the preceding text with general explanation and specific embodiments, on the basis of the present invention, can to some modifications of do or improvement, this is conspicuous as far as these those skilled in the art.Therefore, these modifications or the improvement on the basis of not departing from spirit of the present invention, made all belong to the scope that requirement of the present invention is protected.
Claims (10)
1. a liquid silastic is characterized in that, under 130～200 ℃, being heating and curing after being mixed by following component by weight makes:
(ⅰ) contain organopolysiloxane 50～300 weight parts of two or more unsaturated group of aliphatic series;
(ⅱ) contain organopolysiloxane 0.1～20 weight part of silicon keyed jointing Wasserstoffatoms;
(ⅲ) WHITE CARBON BLACK 1～100 weight part;
(ⅳ) platinum catalyst 0.001～0.1 weight part;
(ⅴ) contain the alkynyl suppressor factor, its content is the alkynyl group that each Pt atom pairs is answered 1～100mol in the said platinum catalyst.
2. liquid silastic according to claim 1 is characterized in that, component (ⅲ) is for carrying out the WHITE CARBON BLACK after the surface treatment with hexamethyldisilazane, and the consumption of said hexamethyldisilazane is 10～50% of a WHITE CARBON BLACK weight.
3. liquid silastic according to claim 2 is characterized in that, said WHITE CARBON BLACK also adopts the silane coupling agent that contains vinyl to carry out surface treatment, and the said dosage of silane coupling agent that contains vinyl is 1～10% of a WHITE CARBON BLACK weight.
4. liquid silastic according to claim 3 is characterized in that, the said silane coupling agent that contains vinyl is selected from one or more in vinyltrimethoxy silane, vinyltriethoxysilane, the tetramethyl divinyl disilazane.
5. liquid silastic according to claim 1 is characterized in that, component (ⅰ) is the organopolysiloxane of linearity, ring-type or collateralization that structural unit constituted shown in the following formula, and its molar mass is 10
2～10
5G/mol:
R
aR
1 bSiO
(4-a-b)/2
Wherein, R be halogen ,-CN ,-SCN ,-replacement or the non-substituted hydrocarbon radical of NCO or C1～C18;
R
1Replacement or non-substituted olefine base or alkynes base for the C2～C10 of Si-C keyed jointing;
A is that 0～3 integer, b are 0～2 integer, and a+b≤3.
6. liquid silastic according to claim 1 is characterized in that, component (ⅱ) is the organopolysiloxane that structural unit shown in the following formula constitutes:
R
cH
dSiO
(4-c-d)/2
Wherein, R be halogen ,-CN ,-SCN ,-replacement or the non-replacement saturated hydrocarbyl of NCO, phenyl, benzyl or C1～C18;
C is 0～3 integer, and d is 0～2 integer, and c+d≤3;
On average contain 3 silicon keyed jointing Wasserstoffatomss in each molecule at least; Its molar mass is 10
2～10
5G/mol;
Described organopolysiloxane preferably contains the silicon keyed jointing Wasserstoffatoms of 0.1～1.6 weight %.
7. liquid silastic according to claim 1 is characterized in that, component (ⅳ) is selected from 1,3-divinyl-1; 1,3,3-tetramethyl disiloxane platinum complex, two (alkynyls) (1; The 5-cyclooctadiene) platinum complex, two (alkynyl) (two ring [2.2.1] heptan-2,5-diene) platinum complex, two (alkynyl) (1,5-dimethyl--1; The 5-cyclooctadiene) platinum complex or two (alkynyl) (1,6-dimethyl--1,5-cyclooctadiene) platinum complex.
8. liquid silastic according to claim 1 is characterized in that, component (ⅴ) is selected from 1-ethynyl-1-hexalin, 2-methyl-3-butyne-2-alcohol, 3,5-dimethyl--1-hexin-3-alcohol or gather the methyl ethylene cyclosiloxane.
9. according to each described liquid silastic of claim 1-8, it is characterized in that under 130～200 ℃, being heating and curing after said liquid silastic is mixed by following component by weight makes:
(ⅰ) contain organopolysiloxane 100～300 weight parts of two or more unsaturated group of aliphatic series;
(ⅱ) contain organopolysiloxane 1～10 weight part of silicon keyed jointing Wasserstoffatoms;
(ⅲ) WHITE CARBON BLACK 10～100 weight parts, its specific surface area is 50～500m
2/ g is preferably 200～400m
2/ g;
(ⅳ) platinum catalyst 0.001～0.1 weight part;
(ⅴ) contain alkynyl suppressor factor 0.01～0.1 weight part.
10. according to each described liquid silastic of claim 1-9, it is characterized in that the said process that under 130～200 ℃, is heating and curing of back that mixes is: with component (ⅰ) and (ⅲ) mix and obtain sizing; Get mass percent and be in 30～70% the said sizing and add component (ⅳ), stirring, it is subsequent use to make component (A); Add component (ⅱ) and (ⅴ) in the sizing in residue, it is subsequent use for making component (B) to stir; Component (A) and component (B) are mixed, and under 130～200 ℃, being heating and curing promptly gets.
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Application publication date: 20121219 |