CN104031389A - Humid-heat resisting room-temperature vulcanized silicone rubber composition - Google Patents
Humid-heat resisting room-temperature vulcanized silicone rubber composition Download PDFInfo
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Abstract
The invention discloses a novel tackifier and a preparation method of a humid-heat resisting room-temperature vulcanized silicone rubber composition. The tackifier is a siloxane compound, which simultaneously contains amino and an epoxy group. The silicone rubber composition comprises the following components in parts by weight: 100 parts of poly-organic siloxane, 5-10 parts of plasticizer, 80-120 parts of packing, 0.2-2 parts of water absorbent, 5-15 parts of cross-linking agent, 0.5-2 parts of self-prepared tackifier and 0.1-1 part of catalyst. The homemade tackifier is added to the components, so that the mechanical property and the bonding strength of the prepared product are reduced by less than 15% by a humid-heat ageing test (dual '85'), and the performance retention rate and the storage stability are high.
Description
Technical field
The present invention relates to a kind of moisture-proof pattern of fever room temperature silicon sulfide rubber composition.The present invention is specifically related to that a kind of humidity resistance is good, mechanical property and bonding strength retentivity is good, stability in storage is high self cure (RTV) organosilicon sealing material and preparation method thereof.
Background technology
Organosilicon sealant is a kind of material of excellent property, and ageing-resistant performance is good, adaptable to high low temperature, and toxicity is little, environmentally friendly, is widely used in the adhering and sealing of the industries such as power electronics, household electrical appliance, photovoltaic module.Along with electronic product is more and more universal, a lot of products can directly leak in air cruelly, and this joint sealant to electronic product has proposed higher performance requriements: have good weather-proof ability; Can tolerate the test of high and low temperature environment; Moistureproof and anti-environmental corrosion ability; Good adhesiveproperties; Anti-mechanical shock and shock resistance; Good insulation and flame retardant properties.In addition, also to improve its heat resistance aging.But often mechanical properties decrease is obvious after hydrothermal aging (two " 85 ") for the organosilicon sealant of producing in the market, to base material just begin bonding but after hydrothermal aging test adhesiveproperties degradation.Therefore, for the RTV silicon rubber that it is good that market provides a kind of wet and heat ageing resistant performance just becomes very urgent.
The patent documentation of relevant aging-resisting type room temperature vulcanized silicone rubber is more, for example Granted publication number discloses a kind of double-component condensed type room curing silicon rubber of wet and heat ageing resistant for the patent of CN102424742B, at A, in B component, add respectively compound and the amino containing silane coupling agent compound containing epoxide group, the silicon rubber of preparation has excellent bonding force, and can keep good mechanics and adhesiveproperties under hygrothermal environment, but two-component silicone rubber before use will be first by A, B component mixes, and vacuumize after removing bubble and could use, cause complex operation, use inconvenience.And the glycidyl allyl ether flash-point adding in A component lower (57 ℃), has special stink, and safety in utilization and operating environment can be affected.
Application publication number is that the patent of CN101717582A discloses a kind of photovoltaic module double component room temperature vulcanization silicon rubber, adopt organo-bismuth and organic titanium composite catalyst to improve the high temperature resistant of product and wet and heat ageing resistant performance, be packaged into A, B component, curing speed more easily meets processing requirement, but during actual use, need first A, B component to be mixed in proportion, to operator, make troubles; And organic bismuth catalyst belongs to new catalyst, Development Techniques is still immature, high cost.
Application publication number is that the patent of CN101353563A discloses a kind of single-component silicone sealant and manufacture method thereof for solar module, adopt methyl three isobutyl ketone oximino silanes and vinyl three isobutyl ketone oximino silanes to make linking agent, KH-550 and KH-560 make coupling agent, petroleum resin and elite filler, make weather xanthochromia, water resistance is more permanent, water vapor transmission rate (WVTR) is low, prevent the photovoltaic component seal gum of mould-growth, but the methyl three isobutyl ketone oximino silanes of selecting and the production technology of vinyl three isobutyl ketone oximino silanes are monopolized by Honeywell, on the high side,
Application publication number is that the patent of CN102268234A discloses the two component sealing gum of silicone and injection process thereof for a kind of solar module, select inorganic combustion inhibitor and photostabilizer collocation to use, make the photovoltaic component seal gum to bonding good, the resistance to xanthochromia of colloid of glass, aluminium, back veneer material, but there is no specifically to investigate the wet and heat ageing resistant performance of seal gum.
Summary of the invention
The object of this invention is to provide a kind of moisture-proof pattern of fever room temperature silicon sulfide rubber composition.
Moisture-proof pattern of fever room temperature silicon sulfide rubber composition, its component is as follows by weight:
Described self-control tackifier are according to the product of following steps reaction gained: the silane coupling agent containing amino and the silane coupling agent containing epoxy group(ing) are added in there-necked flask by proportioning, under nitrogen atmosphere, slowly drip micro-dibutyl tin laurate, be warming up to 80~120 ℃ of back flow reaction 3~4 hours, wherein the consumption of dibutyl tin laurate is 0.5 of the total consumption of silane coupling agent~2 ‰.
Described containing amino silane coupling agent, comprise a kind of in aminopropyl trimethoxysilane, aminopropyl triethoxysilane, aminopropyl methyl dimethoxysilane, 2-(aminoethyl)-3-aminopropyl trimethoxysilane, urea propyl trimethoxy silicane, urea propyl-triethoxysilicane.
The described silane coupling agent containing epoxy group(ing) comprises 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane, 3-(2,3-epoxy the third oxygen) propyl trimethoxy silicane, 3-(2,3-epoxy the third oxygen) a kind of in propyl-triethoxysilicane, 3-(2,3-epoxy the third oxygen) propyl group methyl dimethoxysilane.
In self-control tackifier described in the present invention, containing amino silane coupling agent, be 1: 5~5: 1 with the ratio that contains the silane coupling agent of epoxy group(ing), preferably 1: 3~3: 1.
Described hydroxyl-terminated injecting two methyl siloxane, in the time of 25 ℃, viscosity is 5000~100000mPas, is preferably 10000~80000mPas;
Described softening agent is dimethyl silicone oil, and in the time of 25 ℃, viscosity is preferably 100~1000mPas;
Described filler is two or more in calcium carbonate, white carbon black, titanium dioxide, aluminium hydroxide, aluminum oxide, zinc oxide, silicon powder, white fused alumina, cristobalite, high ridge scholar, wilkinite.
Described water suction profit is one or more in calcium chloride, magnesium chloride, molecular sieve, silazane, alkoxyl silicone carboxylicesters, silane coupling agent.
Described linking agent is one or more in methyl tributanoximo silane, methyl tri acetylacetonate oximino silane, vinyl tributyl ketoximyl silane, four Diacetylmonoxime base silanes, is preferably two or more in methyl tributanoximo silane, vinyl tributyl ketoximyl silane, four Diacetylmonoxime base silanes.
Described catalyzer is one or more in monoalkyl organo-tin compound, dialkyl group organo-tin compound, trialkyl organo-tin compound, inorganic tin compound, tetraalkyl organo-tin compound and their inner complex.
The present invention further comprises the method for preparing moisture-proof pattern of fever room temperature silicon sulfide rubber composition, and concrete steps are as follows:
1) by hydroxyl-terminated injecting two methyl siloxane, softening agent and filler in stirrer, mix original position dehydration 3~4 hours, 100~120 ℃ of temperature, vacuum-0.09~0.1MPa, obtains sizing;
2) sizing is cooled to below 40 ℃, adds linking agent, under vacuum seal, mix 8~10 minutes;
3) then add water-retaining agent, self-control tackifier and catalyzer, mix 8~10 minutes, after the part lower-molecular substance generating in vacuum removal bubble and reaction, obtain the wet and heat ageing resistant type room temperature vulcanized silicone rubber that stability in storage is good.
Moisture-proof pattern of fever room temperature silicon sulfide rubber composition provided by the invention, preparation method is simple, after finishing, rubber composition reaction can use, the loaded down with trivial details step such as avoided mixing before two-component silicone rubber is used, find time, and possess the advantage that stability in storage is good simultaneously.
Containing amino silane coupling agent, can improve the cementability of RTV silicon rubber, but can seriously reduce wet-hot aging performance; Silane coupling agent containing epoxy group(ing) is less on the wet-hot aging performance impact of RTV silicon rubber, but bonding strength is on the low side.The deficiency existing for this two classes coupling agent, the invention provides a kind of novel tackifier, to react under certain condition containing amino silane coupling agent with containing the silane coupling agent of epoxy group(ing), reduced the activity containing amino silane coupling agent, improve its impact on RTV silicon rubber wet-hot aging performance, obviously do not reduced again the bonding strength of RTV silicon rubber simultaneously.The room temperature vulcanized silicone rubber that these tackifier prepare as raw material of take has the high and good beneficial effect of wet-hot aging performance of bonding strength simultaneously.
Embodiment
Below by embodiment, concrete description is done in this aspect; be necessary to be pointed out that at this following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make according to the present invention nonessential improvement and adjustment.
Embodiment 1
Selecting viscosity is the hydroxyl endblocked polydimethylsiloxane of 10000mPas, the dimethyl silicone oil that viscosity is 350mPas, and its component is as follows:
Component | Consumption |
Hydroxyl-terminated injecting two methyl siloxane | 100 |
Dimethyl silicone oil | 8 |
Calcium carbonate | 80 |
Aluminum oxide | 20 |
Gas-phase silica | 5 |
Calcium chloride | 2 |
Methyl tributanoximo silane | 3 |
Vinyl tributyl ketoximyl silane | 7 |
Self-control tackifier | 1 |
Stannous octoate | 0.2 |
The preparation method of self-control tackifier: first by γ-aminopropyltrimethoxysilane and 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane joins in there-necked flask by the proportioning of 1: 3, logical nitrogen temperature to 80 ℃, then slowly drip 2 ‰ dibutyl tin laurate, then keep thermotonus 3 hours, be finally down to room temperature sealing and preserve.
The preparation method of moisture-proof pattern of fever room temperature silicon sulfide rubber composition: 100 parts of hydroxyl endblocked polydimethylsiloxanes and 8 parts of dimethyl silicone oils, fillers are added in stirring tank, at 90~110 ℃, after stirring 2~4h under-0.09~0.1MPa vacuum condition, be cooled to below 40 ℃, add above-mentioned umber methyl tributanoximo silane, vinyl tributyl ketoximyl silane, under vacuum seal, mix 8~10 minutes; Add successively calcium chloride, self-control tackifier, stannous octoate to stir under vacuum condition, make moisture-proof pattern of fever room temperature vulcanized silicone rubber.
Product performance test result is in Table 1.
Embodiment 2
Selecting viscosity is that to select viscosity be the hydroxyl endblocked polydimethylsiloxane of 20000mPas, the dimethyl silicone oil that viscosity is 1000mPas, and its component is as follows:
Component | Consumption |
Hydroxyl-terminated injecting two methyl siloxane | 100 |
Dimethyl silicone oil | 5 |
Calcium carbonate | 80 |
Aluminum oxide | 10 |
Silicon powder | 8 |
Magnesium chloride | 0.5 |
Methyl tributanoximo silane | 8 |
Four Diacetylmonoxime base silanes | 2 |
Self-control tackifier | 1 |
Dibutyl tin laurate | 0.2 |
The preparation method of self-control tackifier: first by γ-aminopropyl triethoxysilane and 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane joins in there-necked flask by the proportioning of 1: 1, logical nitrogen temperature to 100 ℃, then slowly drip 1 ‰ dibutyl tin laurate, then keep thermotonus 3 hours, be finally down to room temperature sealing and preserve.
The preparation method of moisture-proof pattern of fever room temperature silicon sulfide rubber composition: 100 parts of hydroxyl endblocked polydimethylsiloxanes and 5 parts of dimethyl silicone oils, fillers are added in stirring tank, at 90~110 ℃, after stirring 2~4h under-0.09~0.1MPa vacuum condition, be cooled to below 40 ℃, add above-mentioned umber methyl tributanoximo silane, four Diacetylmonoxime base silanes, under vacuum seal, mix 8~10 minutes; Add successively magnesium chloride, self-control tackifier, dibutyl tin laurate to stir under vacuum condition, make moisture-proof pattern of fever room temperature vulcanized silicone rubber.
Product performance test result is in Table 1.
Embodiment 3
Selecting viscosity is that to select viscosity be the hydroxyl endblocked polydimethylsiloxane of 80000mPas, the dimethyl silicone oil that viscosity is 350mPas, and its component is as follows:
Component | Consumption |
Hydroxyl-terminated injecting two methyl siloxane | 100 |
Dimethyl silicone oil | 10 |
Calcium carbonate | 80 |
Aluminium hydroxide | 30 |
Zinc oxide | 5 |
Silazane | 3 |
Methyl tributanoximo silane | 4 |
Methyl tri acetylacetonate oximino silane | 6 |
Self-control tackifier | 1 |
Diacetyl acetonyl dibutyl tin | 0.8 |
The preparation method of self-control tackifier: first by γ-aminopropyltrimethoxysilane and 3-(2,3-epoxy the third oxygen) propyl-triethoxysilicane joins in there-necked flask by the proportioning of 3: 1, logical nitrogen temperature to 120 ℃, then slowly drip 0.5 ‰ dibutyl tin laurate, then keep thermotonus 3 hours, be finally down to room temperature sealing and preserve.
The preparation method of moisture-proof pattern of fever room temperature silicon sulfide rubber composition: 100 parts of hydroxyl endblocked polydimethylsiloxanes and 10 parts of dimethyl silicone oils, fillers are added in stirring tank, at 90~110 ℃, after stirring 2~4h under-0.09~0.1MPa vacuum condition, be cooled to below 40 ℃, add above-mentioned umber methyl tributanoximo silane, methyl tri acetylacetonate oximino silane, under vacuum seal, mix 8~10 minutes; Add successively silazane, self-control tackifier, diacetyl acetonyl dibutyl tin to stir under vacuum condition, make moisture-proof pattern of fever room temperature vulcanized silicone rubber.
Product performance test result is in Table 1.
Comparative example 1
Selecting viscosity is that to select viscosity be the hydroxyl endblocked polydimethylsiloxane of 20000mPas, the dimethyl silicone oil that viscosity is 350mPas, and its component is as follows:
Component | Consumption |
Hydroxyl-terminated injecting two methyl siloxane | 100 |
Dimethyl silicone oil | 20 |
Calcium carbonate | 100 |
Aluminium hydroxide | 20 |
Gas-phase silica | 8 |
Titanium dioxide | 2 |
Methyl tributanoximo silane | 4 |
Vinyl tributyl ketoximyl silane | 6 |
γ-aminopropyltrimethoxysilane | 1 |
Dibutyltin diacetate | 0.3 |
The preparation method of moisture-proof pattern of fever room temperature silicon sulfide rubber composition: 100 parts of hydroxyl endblocked polydimethylsiloxanes and 20 parts of dimethyl silicone oils, fillers are added in stirring tank, at 90~110 ℃, after stirring 2~4h under-0.09~0.1MPa vacuum condition, be cooled to below 40 ℃, add above-mentioned umber methyl tributanoximo silane, vinyl tributyl ketoximyl silane, under vacuum seal, mix 8~10 minutes; Add successively γ-aminopropyltrimethoxysilane, dibutyltin diacetate to stir under vacuum condition, make moisture-proof pattern of fever room temperature vulcanized silicone rubber.
Product performance test result is in Table 1.
Comparative example 2
Selecting viscosity is that to select viscosity be the hydroxyl endblocked polydimethylsiloxane of 10000mPas, the dimethyl silicone oil that viscosity is 1000mPas, and its component is as follows:
Component | Consumption |
Hydroxyl-terminated injecting two methyl siloxane | 100 |
Dimethyl silicone oil | 20 |
Calcium carbonate | 70 |
Aluminium hydroxide | 20 |
Silicon powder | 8 |
Titanium dioxide | 2 |
Methyl tributanoximo silane | 4 |
Methyl tri acetylacetonate oximino silane | 6 |
2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane | 1 |
Stannous octoate | 0.5 |
The preparation method of moisture-proof pattern of fever room temperature silicon sulfide rubber composition: 100 parts of hydroxyl endblocked polydimethylsiloxanes and 20 parts of dimethyl silicone oils, fillers are added in stirring tank, at 90~110 ℃, after stirring 2~4h under-0.09~0.1MPa vacuum condition, be cooled to below 40 ℃, add above-mentioned umber methyl tributanoximo silane, methyl tri acetylacetonate oximino silane, under vacuum seal, mix 8~10 minutes; Add successively 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane, stannous octoate to stir under vacuum condition, make moisture-proof pattern of fever room temperature vulcanized silicone rubber.
Product performance test result is in Table 1.
Comparative example 3
Selecting viscosity is that to select viscosity be the hydroxyl endblocked polydimethylsiloxane of 10000mPas, the dimethyl silicone oil that viscosity is 1000mPas, and its component is as follows:
Component | Consumption |
Hydroxyl-terminated injecting two methyl siloxane | 100 |
Dimethyl silicone oil | 20 |
Calcium carbonate | 70 |
Aluminium hydroxide | 20 |
Gas-phase silica | 8 |
Titanium dioxide | 2 |
Methyl tributanoximo silane | 4 |
Vinyl tributyl ketoximyl silane | 6 |
2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane | 1 |
γ-aminopropyltrimethoxysilane | 1 |
Dibutyltin diacetate | 0.5 |
The preparation method of moisture-proof pattern of fever room temperature silicon sulfide rubber composition: 100 parts of hydroxyl endblocked polydimethylsiloxanes and 20 parts of dimethyl silicone oils, fillers are added in stirring tank, at 90~110 ℃, after stirring 2~4h under-0.09~0.1MPa vacuum condition, be cooled to below 40 ℃, add above-mentioned umber methyl tributanoximo silane, vinyl tributyl ketoximyl silane, under vacuum seal, mix 8~10 minutes; Add successively 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane, γ-aminopropyltrimethoxysilane, dibutyltin diacetate to stir under vacuum condition, make moisture-proof pattern of fever room temperature vulcanized silicone rubber.
Product performance test result is in Table 1.
Table 1 performance perameter table
The explanation of above embodiment is just for helping to understand product of the present invention, method and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Above-mentioned explanation to the disclosed embodiments, makes professional and technical personnel in the field can realize or use the present invention.To the multiple modification of these embodiment, will be apparent for those skilled in the art, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a moisture-proof pattern of fever room temperature silicon sulfide rubber composition, is characterized in that, its component is as follows by weight:
Described self-control tackifier are that the silane coupling agent containing amino and the silane coupling agent containing epoxy group(ing) are added in flask by proportioning, under nitrogen atmosphere, slowly drip micro-dibutyl tin laurate, be warming up to the product of 3~4 hours gained of 80~120 ℃ of back flow reaction;
Wherein the consumption of dibutyl tin laurate is 0.5 of the total consumption of silane coupling agent~2 ‰.
2. a kind of moisture-proof pattern of fever room temperature silicon sulfide rubber composition according to claim 1, is characterized in that, described softening agent is dimethyl silicone oil, and in the time of 25 ℃, viscosity is 50~3000mPas, is preferably 100~1000mPas.
3. a kind of moisture-proof pattern of fever room temperature silicon sulfide rubber composition according to claim 1, it is characterized in that, described filler is two or more mixture in calcium carbonate, white carbon black, titanium dioxide, aluminium hydroxide, aluminum oxide, zinc oxide, silicon powder, white fused alumina, cristobalite, kaolin, wilkinite.
4. a kind of moisture-proof pattern of fever room temperature silicon sulfide rubber composition according to claim 1, is characterized in that, described water-retaining agent is one or more in calcium chloride, magnesium chloride, molecular sieve, silazane, alkoxyl silicone carboxylicesters, silane coupling agent.
5. a kind of moisture-proof pattern of fever room temperature silicon sulfide rubber composition according to claim 1, it is characterized in that, described containing amino silane coupling agent, comprise a kind of in aminopropyl trimethoxysilane, aminopropyl triethoxysilane, aminopropyl methyl dimethoxysilane, 2-(aminoethyl)-3-aminopropyl trimethoxysilane, urea propyl trimethoxy silicane, urea propyl-triethoxysilicane.
6. a kind of moisture-proof pattern of fever room temperature silicon sulfide rubber composition according to claim 1, it is characterized in that, the described silane coupling agent containing epoxy group(ing) comprises 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane, 3-(2,3-epoxy the third oxygen) propyl trimethoxy silicane, 3-(2,3-epoxy the third oxygen) a kind of in propyl-triethoxysilicane, 3-(2,3-epoxy the third oxygen) propyl group methyl dimethoxysilane.
7. a kind of moisture-proof pattern of fever room temperature silicon sulfide rubber composition according to claim 1, is characterized in that 1: 3~3: 1.
8. a kind of moisture-proof pattern of fever room temperature silicon sulfide rubber composition according to claim 1, it is characterized in that, described linking agent is one or more in methyl tributanoximo silane, methyl tri acetylacetonate oximino silane, vinyl tributyl ketoximyl silane, four Diacetylmonoxime base silanes, is preferably two or more in methyl tributanoximo silane, vinyl tributyl ketoximyl silane and four Diacetylmonoxime base silanes.
9. a kind of moisture-proof pattern of fever room temperature silicon sulfide rubber composition according to claim 1, it is characterized in that, described catalyzer is one or more in monoalkyl organo-tin compound, dialkyl group organo-tin compound, trialkyl organo-tin compound, inorganic tin compound, tetraalkyl organo-tin compound and their inner complex.
10. prepare a method for moisture-proof pattern of fever room temperature silicon sulfide rubber composition as claimed in claim 1, it is characterized in that, comprise the following steps:
1) by hydroxyl-terminated injecting two methyl siloxane, softening agent and filler in stirrer, mix original position dehydration 3~4 hours, 100~120 ℃ of temperature, vacuum-0.09~0.1MPa, obtains sizing;
2) sizing is cooled to below 40 ℃, adds linking agent, under vacuum seal, mix 8~10 minutes;
3) then add water-retaining agent, self-control tackifier and catalyzer, mix 8~10 minutes, after the part lower-molecular substance generating in vacuum removal bubble and reaction, obtain the room temperature vulcanized silicone rubber that wet and heat ageing resistant is good.
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