CN102424742B - Hot-wet resistant and aging resistant dual-component condensation type room temperature curing silicone rubber - Google Patents
Hot-wet resistant and aging resistant dual-component condensation type room temperature curing silicone rubber Download PDFInfo
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- CN102424742B CN102424742B CN 201110369701 CN201110369701A CN102424742B CN 102424742 B CN102424742 B CN 102424742B CN 201110369701 CN201110369701 CN 201110369701 CN 201110369701 A CN201110369701 A CN 201110369701A CN 102424742 B CN102424742 B CN 102424742B
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Abstract
The present invention discloses a hot-wet resistant and aging resistant dual-component condensation type room temperature curing silicone rubber. According to the rubber, a epoxy group-containing compound and an amino silane coupling agent compound are respectively added to a component A and a component B of the dual-component condensation type room temperature curing silicone rubber; treatments of mixing and curing are performed to form a elastomer, wherein the elastomer provides excellent adhesion for the substrate, and retains good mechanical property and good adhesion property under the hot-wet environment. According to the present invention, during the rubber applying process, the component A and the component B of the dual-component condensation type room temperature curing siliconerubber are uniformly mixed according to a weight ratio or a volume ratio automatically calculated by equipment, then bubbles are removed, and the curing treatment is performed for a plurality of hours or days at the room temperature to form the elastomer, wherein the elastomer has good mechanical property and good adhesion property. Compared to the silicone rubber without addition of the epoxy group-containing compound, the silicone rubber of the present invention has significant hot-wet resistance.
Description
Technical field
The present invention is a kind of preparation method of double-component condensed type room curing silicon rubber of wet and heat ageing resistant.
Background technology
Not heat release when the double-component condensed type room curing silicon rubber solidifies, shrinking percentage is little, and internal stress is low, can deep layer vulcanization, have characteristics such as thermotolerance, winter hardiness, dielectricity, anti-ozone and anti-environmental aging after the curing, be highly suitable for many specific industry assemblings.In the art, a large amount of condensation reactions of passing through has been arranged, be cross-linked into elastomeric bicomponent normal temperature cure silicone rubber.These silicon rubber main components have: hydroxyl-terminated injecting two methyl siloxane, methyl-silicone oil, fillers such as white carbon black, silicon powder, calcium carbonate, alkoxy silane cross linked dose, organo-tin compound catalyzer, tackifier such as amino containing silane coupling agent.Usually filler and hydroxyl-terminated injecting two methyl siloxane or a small amount of methyl-silicone oil are pre-mixed, as the A component; A small amount of methyl-silicone oil, catalyzer, linking agent, tackifier and coloured material etc. are mixed as the B component; Be transported to the applying glue scene after the packing respectively, mix by certain weight ratio or volume ratio by artificial or fully-automatic equipment, a few hours or a couple of days are placed in surfaces such as applying glue is bonding to needing, the material of embedding, sealing such as aluminium, glass, plastics under the room temperature, can be cross-linked to form silicon rubber.This class silicon rubber has good mechanical performance and adhesiveproperties, is widely used in industries such as building, electronics, automobile, photovoltaic at present.
Above-mentioned bicomponent normal temperature cure silicone rubber provide be adhesively fixed in, need also to consider that silicon rubber is in the aging influence of applied environment.The architectural design life-span requires 30-50 usually at present, and photovoltaic module requires 25 years, and automobile can bear more than 10 years, and the electronic product that numerous electron devices particularly use out of doors also has the wet and heat ageing resistant requirement.Some standards of industries such as building, photovoltaic have been done relevant regulations to the wet and heat ageing resistant performance of material, the silicon rubber that requires to solidify as " structural silicone sealant for building GB 16776-2005 " soaks back detection mechanics and adhesiveproperties in hot water, it is aging that " identify and typing IEC61215 with Crystalline Silicon PV Module design on ground " requires photovoltaic module can bear the following 1000 hours moisture of 85 ℃, 85% relative humidity, so the wet-hot aging performance of silicon rubber seems extremely important in some industry.
The molecular chain main chain of silicon rubber or cross-linking set easily by the stronger material damage of acid-basicity, cause mechanics and adhesiveproperties to descend under hygrothermal environment after solidifying, and do not reach design requirements.In double-component condensed type room curing silicon rubber prescription, in order to allow silicon rubber and base material form good cementability, add the amino containing silane coupling agent as tackifier in the B component usually.And the normal amine propyl-triethoxysilicane that uses, the alkalescence of amino containing silane coupling agents such as amine ethylamine propyl-triethoxysilicane is stronger, may cause silicon rubber to be degraded under wet heat condition, degradation.
Summary of the invention
The object of the present invention is to provide a kind of double-component condensed type room curing silicon rubber of wet and heat ageing resistant.
The present invention is achieved in that
A kind of double-component condensed type room curing silicon rubber of wet and heat ageing resistant, by A, B component by weight or volume ratio mix condensation reaction and form elastomerics mutually.
The A component comprises following composition:
The hydroxyl-terminated injecting two methyl siloxane of A1:50 to 100 weight part or PSI have 1 under 25 ℃, 000mPa.s to 1, the viscosity of 000,000mPa.s;
The methyl-silicone oil of A2:0 to 30 weight part has 50 to 10,000mPa.s viscosity under 25 ℃;
The reinforced filling of A3:0 to 150 weight part, these fillers provide mechanical strength for the silicon rubber that solidifies, and applicatory have: thermal silica, precipitated silica, silicon powder, diatomite, talcum powder, kaolin, calcium carbonate etc.White carbon black should use specific surface area greater than 100m
2The hydrophobic thermal silica of/g.Calcium carbonate should be the nano-calcium carbonate of fatty acid treatment with the surface.Can mix use by one or more fillers.
A4:0.5 to 10 weight part band oxygen groups organic compound.The compound that comprises has: conventional Resins, epoxy E51, dihydroxyphenyl propane compounds such as E44, epoxy cyclohexane compounds, aliphatic epoxy resin, some contains the epoxide group compound, as glycidyl ether derivatives etc.Determine at present these compounds all in this patent can and the B component in amino containing silane at room temperature can react the wet-hot aging performance of raising silicon rubber.The equivalent of epoxide group is greater than the equivalent of amido in the silicone rubber formulations, and optimal is that the epoxide group equivalent is more than 1 times of amine groups equivalent in the B component.
Above component is mixed in mixing equipment such as kneader, stirring, and the dispersion of milling of three roller runner millings is packaged into the A component behind the vacuum removal bubble.
The B component:
B1:0 to 60 weight part methyl-silicone oil has 50 to 100,000mPa.s viscosity under 25 ℃.
B2:0 to 50 weight part coloured material is as carbon black, titanium dioxide etc.
B3:5 to 70 weight part linking agent is as tetraethoxy, positive silicic acid propyl ester, methyltrimethoxy silane, Union carbide A-162, silicate hydrolyzate oligopolymer, Union carbide A-162 hydrolyzed oligomers etc.But one or more mix use.
B4:0.5 to 5 weight part organic tin catalyzer is as dibutyl tin laurate, dibutyltin diacetate, dimethoxy dibutyl tin, dibutyl tin diacetyl acetonate, stannous octoate class organic compound.Above catalyzer can mix use.
B5:5 to 50 portions of amine by weight base silane coupling agent.Amino containing silane coupling agent kind comprises the oligopolymer of amine propyl-triethoxysilicane, amine propyl trimethoxy silicane, amine ethylamine propyl trimethoxy silicane, amine ethylamine propyl-triethoxysilicane or its partial hydrolysis.
Above component is blending dispersion in mixing equipment such as stirring, is packaged into the B component after removing bubble.
When applying glue, by weight or with equipment automatic gauge volume ratio, A, B component are mixed, remove bubble, for bonding, embedding and sealing.This silicon rubber at room temperature can solidify to form elastomerics after a few hours or a couple of days, and has good adhesiveproperties.Do not add the silica gel contrast of epoxide group compound, have the performance of more outstanding moisture-proof heat.
Detection method:
1, Mechanics Performance Testing: with silicon rubber A, B component mixed according to the rules, after the vacuum defoamation, be pressed in the mould of 150mm * 100mm * 2mm, self-vulcanizing or aging after, according to standard GB/T528-2009, cutting mechanical test batten, test tensile strength, elongation.
2, adhesive shear strength test: with silicon rubber A, B component mixed according to the rules, after the vacuum defoamation, according to standard GB/T 7124-86, do the tensile shear strength test sample, self-vulcanizing or aging after, test silicon rubber is to the aluminium adhesive shear strength.
3, hardness test: reference standard GB/T 531-1999, with the batten of mechanical test cutting, it is thick to be superimposed as 6mm, with rubber pocket sclerometer penetration hardness measurement of test method silicon rubber hardness (Shore A).
4, two 85 senile experiments: the silicon rubber mechanical test batten after will solidifying, it is 85 ℃ that the bonding shearing test print of aluminium-aluminium is put into the condition of setting, aging after 1000 hours in the climatic chamber of 85%RH, survey hardness, tensile strength and shearing resistance according to the method described above.
5, fast hydrothermal aging experiment: the silicon rubber Mechanics Performance Testing batten after will solidifying, the bonding shearing test print of aluminium-aluminium is put in 100 ℃ of hot water, soaks 4 days, then tested for hardness, tensile strength, shearing resistance according to the method described above.
Discover, in the A component, add and contain the epoxide group compound, in the applying glue solidification process, amido reaction with amino containing silane coupling agent in the B component, reduce the influence of amino containing silane, improve the wet-hot aging performance after silicon rubber solidifies, various base materials have been had excellent adhesiveproperties, be applicable to industries such as photovoltaic module sealing and automobile assembling, building glass sealing, electric encapsulation.
Embodiment
Embodiment 1
The polydimethylsiloxane of the viscosity 20000mPa.s that A component: 50g is hydroxy-end capped, the calcium carbonate that the stearic acid-treated median size of 50g is 0.06 micron mixes, and three rollers are milled, and add 3g Resins, epoxy E51, mix vacuum defoamation.
The B component: the methyl-silicone oil of 49g viscosity 10000mPa.s, 10g pigment carbon black, the 20g tetraethoxy, the 1g dibutyl tin laurate, 20g amine propyl-triethoxysilicane mixes, and vacuum defoamation packs.
During use A component and B component are mixed according to weight ratio at 10: 1, deaeration obtains the black bicomponent normal temperature and solidifies condensed type silicon rubber 1#.It the results are shown in Table 1.
Embodiment 2
The polydimethylsiloxane of the viscosity 10000mPa.s that A component: 55g is hydroxy-end capped, the calcium carbonate that the stearic acid-treated median size of 42g is 0.08 micron, 3g titanium dioxide, mix, three rollers are milled, and add 2g glycidyl ether propyl trimethoxy silicane, mix vacuum defoamation.
B component: 60g viscosity 5000mPa.s methyl-silicone oil, the specific surface area 200m that the 9g hexamethyldisilazane is handled
2The gas-phase silica of/g, the 1g stannous octoate, 10g amine propyl trimethoxy silicane, 20g methyltrimethoxy silane partial hydrolysis oligopolymer mixes, and vacuum defoamation packs.
During use A component and B component are mixed according to weight ratio at 10: 1, deaeration obtains white bicomponent normal temperature cure silicone rubber 2#.It the results are shown in Table 1.
Embodiment 3
The polydimethylsiloxane of the viscosity 20000mPa.s that A component: 87g is hydroxy-end capped, the specific surface area 200m that the 13g hexamethyldisilazane is handled
2The gas-phase silica of/g mixes, and three rollers are milled, and adds the 2g glycidyl allyl ether, mixes vacuum defoamation.
B component: the methyl-silicone oil of 55g viscosity 1000mPa.s, the specific surface area 200m that the 4g hexamethyldisilazane is handled
2The gas-phase silica of/g, 20g amine ethylamine propyl-triethoxysilicane, the positive silicic acid propyl ester of 20g, the 1g dibutyl tin diacetyl acetonate mixes, and vacuum defoamation packs.
During use A component and B component are mixed according to weight ratio at 10: 1, deaeration obtains translucent bicomponent normal temperature and solidifies condensed type silicon rubber 3#.It the results are shown in Table 1.
Embodiment 4
The polydimethylsiloxane of the viscosity 5000mPa.s that A component: 50g is hydroxy-end capped, the dimethyl silicone oil of 5g viscosity 100mPa.s, the silicon powder that the 45g particle diameter is 5 microns, three rollers are milled, and add epoxy cyclohexane base ethyl trimethoxy silane 2g, mix deaeration.
The B component: with the methyl-silicone oil of 45g viscosity 100mPa.s, 15g amine ethylamine propyl trimethoxy silicane, 15g teos hydrolysis oligopolymer, the 24g titanium dioxide, the 1g dibutyltin diacetate mixes, and deaeration packs.
During use A component and B component are mixed according to weight ratio at 10: 1, vacuum defoamation obtains white bicomponent normal temperature cure silicone rubber 4#.It the results are shown in Table 1.
Comparative Examples 1
With embodiment 1, wherein do not use Resins, epoxy E51 in the A component.Obtain bicomponent normal temperature cure silicone rubber 5#, it the results are shown in Table 1.
Comparative Examples 2
The polydimethylsiloxane of the viscosity 20000mPa.s that 50g silicon is hydroxy-end capped, the calcium carbonate that the stearic acid-treated median size of 50g is 0.06 micron, mix, thermal dehydration, three rollers are milled, and add the methyl-silicone oil of 5g viscosity 100mPa.s successively, 4g methyl three Diacetylmonoxime silane, 1g amine propyl-triethoxysilicane, the 0.05g dibutyl tin laurate.Mix, vacuum defoamation is packaged in the silicone tubing, obtains single component and takes off oxime type room curing silicon rubber.
During use the component in the silicone tubing is extruded, obtained silicon rubber 6# after the curing, it the results are shown in Table 1.
Table 1:
As can be seen from the table, in the A component, add an amount of epoxy compounds, improved the wet-hot aging performance of double-component condensed type room curing silicon rubber.
Claims (1)
1. the double-component condensed type room curing silicon rubber of a wet and heat ageing resistant is characterized in that: mixed deaeration and obtaining at 10: 1 according to weight ratio by A component and B component;
The polydimethylsiloxane of the viscosity 20000mPa.s that A component: 87g is hydroxy-end capped, the gas-phase silica of specific surface area 200 ㎡/g that the 13g hexamethyldisilazane is handled mixes, three rollers are milled, add the 2g glycidyl allyl ether, mix vacuum defoamation;
B component: the methyl-silicone oil of 55g viscosity 1000mPa.s, the gas-phase silica of specific surface area 200 ㎡/g that the 4g hexamethyldisilazane is handled, 20g aminoethyl aminopropyl triethoxysilane, the positive silicic acid propyl ester of 20g, the 1g dibutyl tin diacetyl acetonate mixes, vacuum defoamation packs.
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| JPH03258876A (en) * | 1990-03-07 | 1991-11-19 | Nippon Paint Co Ltd | Coating compound composition of middle coating for covering silicone rubber |
| US20050192387A1 (en) * | 2004-03-01 | 2005-09-01 | Williams David A. | RTV silicone composition offering rapid bond strength |
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