CN103709759A - Room temperature cured single-component high temperature resisting silica gel and preparation method thereof - Google Patents
Room temperature cured single-component high temperature resisting silica gel and preparation method thereof Download PDFInfo
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- CN103709759A CN103709759A CN201310720589.8A CN201310720589A CN103709759A CN 103709759 A CN103709759 A CN 103709759A CN 201310720589 A CN201310720589 A CN 201310720589A CN 103709759 A CN103709759 A CN 103709759A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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- C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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- C08G77/16—Polysiloxanes containing silicon bound to oxygen-containing groups to hydroxyl groups
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
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Abstract
The invention discloses room temperature cured single-component high temperature resisting silica gel. The silica gel is prepared from raw materials including hydroxy-terminated polysiloxane, silicone oil, polymethyl triethoxysilane, synthetic rectifier, reinforcing filler, high temperature resisting filler, a cross-linking agent, a coupling agent and a catalyst, and belongs to room temperature cured single-component silica gel. The synthetic rectifier is adopted, and the reinforcing filler and a high temperature resisting additive are compounded, so the silica gel has good high temperature resistance as well as excellent mechanical properties, and is mainly applied to adhesion and sealing of materials like ceramic, metal, stainless steel and the like in high-temperature environment. The invention also provides a preparation method of the room temperature cured single-component high temperature resisting silica gel. By the preparation method disclosed by the invention, the mechanical properties and high temperature resistance of organic silica gel are both improved, types of organic silica gel are enriched, the application field of organic silica gel is widened, and good application prospect is realized.
Description
technical field
The invention relates to a kind of room temperature curing type one-component thermostable silica gel and preparation method thereof.
background technology
Room temperature curing type one-component thermostable silica gel is to take the resistant to elevated temperatures silica gel of a class that hydroxy-end capped polysiloxane makes as raw material, and it is containing organic solvent, and shrinking percentage is little, free from environmental pollution, ambient temperature curable, and save energy, easy to use.Yet the silicon rubber of traditional processing mode can only be in 180-200 ℃ of situation life-time service, while surpassing 200 ℃, silicon rubber will hardness rise, be full of cracks is followed the string, and has no value for use.But under given conditions, the resistance to elevated temperatures of silica gel is had to very high requirement, in prior art, the TRANSIENT HIGH TEMPERATURE that the common high temperature resistant silica gel of producing produces in the time of can not bearing for a long time 200 ℃ of above high temperature of engine sealing element and igniting, recovery of elasticity is good not, flexibility decrease under low temperature, long-time use easily produces elastic fatigue, affects sealing property.
Application number is that 200810091446.4 patent [1] discloses a kind of motor car engine, chassis adhering and sealing material, one-component thermostable seal gum, the high temperature that its ability is 260 ℃.Application number is the method for making that 201010560756.3 patent [2] discloses a kind of one-component thermostable silicone sealant, the high temperature that its ability is 260 ℃.Application number is that 201010551795.7 patent [3] discloses a kind of high-temperature-resisting silicon rubber and method for making thereof, it is roasting after four hours in 300 ℃ of baking boxs, its tensile strength drops to 7 MPa by 11MPa, elongation drops to 340% by 628%, tear strength drops to 16KN.M by 26KN.M, all has decline by a relatively large margin.Application number is the composition of raw materials that the patent [4] of 201110348679.X discloses a kind of high-temperature-resisting silicon rubber, and adopting methyl vinyl silicone rubber is base glue, adds nanometer heat-resisting additive, can resistance to 400 ℃ of following high temperature.
Mainly by three kinds of methods, improve at present the resistance toheat of silicon rubber: 1. by changing the structure of silicon rubber molecule side group, crosslinked and the DeR [5] that phenyl etc. suppresses to cause because of oxygenolysis due to organic side group of silicon rubber as introduced is 2. by introduce the segment of large volume in silicon rubber molecular backbone chain, as carbon decaborane base etc. prevents the degraded that silicon rubber main chain causes because of oxidative degradation; 3. by adding heat resistance accessory, the side chain that suppresses silicon rubber as ferric oxide, rare earth element etc. is crosslinked.Wherein to add in silicon rubber heat-resistant filler be the most effectively, economic, method [6] conveniently.
[1] one-component thermostable silicone sealant, application number: 200810091446.4, invention designer: Chen Ping Qiang; Liang Yinsheng; Chen Ping Yao; Zhang Yitian;
[2] one-component thermostable silicone sealant, application number: 201010560756.3, invention designer: Chen Ping Yao; Liang Yinqi; Zhang Qiuming;
[3] high-temperature-resisting silicon rubber and preparation method thereof, application number: 201010551795.7, invention designer: Cai Enfu;
[4] composition of raw materials for high-temperature-resisting silicon rubber, application number: 201110348679.X, invention designer: Zhang Qing;
[5] cutting edge of a knife or a sword that strengthens the army, Jing Xinli, Wang Yangyong, etc. the progress of silicon rubber heat-resisting [J].New Chemical Materials, 2003,31(10): 5-12;
[6] Peng Yalan, Su Zhengtao, Liu Jun, etc. red iron oxide is on the impact of hot-vulcanized silicone rubber heat aging performance [J]. organosilicon material, 2005,19 (4): 14-16.
summary of the invention
The object of the invention is to make up the deficiency of currently available products, a kind of room temperature curing type one-component thermostable silica gel and preparation method thereof is provided, main by synthesizing the composite of strengthening agent, reinforced filling and high temperature resistant auxiliary agent, mechanical property and the resistance to elevated temperatures of organic silica gel are all improved, enriched organic silica gel kind, the Application Areas of having expanded organic silica gel, has a good application prospect.
Technical scheme of the present invention is:
A room temperature curing type one-component thermostable silica gel, its formulation ratio is:
Hydroxy-end capped polysiloxane 100 weight parts;
Silicone oil 1～5 weight part;
Poly-Union carbide A-162 5～20 weight parts;
Synthetic strengthening agent 10～20 weight parts;
Reinforced filling 10～20 weight parts;
High temperature resistant filler 50～200 weight parts;
Linking agent 2～10 weight parts;
Coupling agent 2～5 weight parts;
Catalyzer 0.2～2 weight part.
As preferably, described hydroxy-end capped polysiloxane adopts α, alpha, omega-dihydroxy polydimethyl siloxane; Silicone oil adopts phenyl silicone oil; Reinforced filling adopts nano imvite; High temperature resistant filler adopts black silicon carbide; Linking agent adopts one of them kind in methyl tributanoximo silane, vinyl tributyl ketoximyl silane; Coupling agent adopts γ-aminopropyl triethoxysilane; Catalyzer adopts dibutyl tin dilaurate.
The preparation process of room temperature curing type one-component thermostable silica gel is as follows as mentioned above:
S1, by hydroxy-end capped polysiloxane 100 weight parts, silicone oil 1～5 weight part, poly-Union carbide A-162 5～20 weight parts, synthetic strengthening agent 10～20 weight parts, reinforced filling 10～20 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 20～60rpm 60 minutes;
S2, add high temperature resistant filler 50～200 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 20～60rpm 120 minutes;
S3, add linking agent 2～10 weight parts, coupling agent 2～5 weight parts, catalyzer 0.5～2 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1～0.5 MPa, revolution 20～60rpm.
The preparation method of above-mentioned synthetic strengthening agent is as follows: tetraethoxy, poly-Union carbide A-162, trimethyl silanol, ethanol, aqueous acetic acid are reacted 3～4 hours for 100:20～100:150～300:60～80:5～15 mix successively by weight under the condition of 40～60 ℃, reacted mixture is at 40～60 ℃, and under the condition of-0.1～-0.5MPa, underpressure distillation makes.
The invention overcomes the shortcoming of prior art, main by synthesizing the composite of strengthening agent, reinforced filling and high temperature resistant auxiliary agent, mechanical property and the resistance to elevated temperatures of organic silica gel are all improved, enriched organic silica gel kind, expanded the Application Areas of organic silica gel, have a good application prospect, specific as follows:
1. adopt synthetic strengthening agent to improve the mechanical property of organic silica gel.On the one hand, after macromole in synthetic strengthening agent disperses, a plurality of 3 D cross-linked centers have been formed, crosslinked center and high-polymer molecular interchain have stronger effect, they adsorb mutually, and interchain is wound around mutually, present dispersion, effectively eliminate interfacial energy between the two poor, further improved the ability to bear of high-temp glue counter stress of the present invention; On the other hand, because crosslinked center itself is polysiloxane structure, there is good flexible ability, increased the tensile yield of system, also delayed the fracture process of compound system simultaneously, increased the tensile yield of high-temperature plastic of the present invention; Thereby reach the effect of reinforcement.
2. adopt nano imvite to substitute traditional white carbon black and as reinforced filling, improve the mechanical property of organic silica gel.Nano imvite is applied the nano modification that is mainly used in rubber item in rubber, improves its resistance to air loss, the power that surely extends and wear resistance, preservative property, weather resisteant, chemical resistant properties.By adding appropriate nano imvite, can make the performance such as intensity, elongation of rubber increase substantially, some performances can improve several times, alternative current White Carbon black.Adopt nano imvite replacement white carbon black to have three aspects as the reason of reinforced filling:
(1) white carbon black surface, with the higher hydroxyl of activity, at high temperature makes Si-O bond fission, causes main chain DeR;
(2) planar water of white carbon black remained on surface at high temperature also can make Si-O hydrolytic cleavage, causes silicon rubber poor heat stability at high temperature, and use temperature is not high;
(3) white carbon black is difficult to infiltrate and disperse in organic phase.
3. because poly-Union carbide A-162 has hydrophobic nature and higher thermotolerance, in silica gel, add appropriate poly-Union carbide A-162 as high temperature resistant auxiliary agent, can improve the resistance to elevated temperatures of organic silica gel.
4. high phenyl silicone oil thermostability is higher, also has good radiation resistance, can be used as thermal treatment bath, heat oil, the gas-chromatography carrier of metal products, the high sub-zero oil of electronics, electric installation, the high temperature grease that adds carbon black, lithium soap or molybdenumdisulphide to make can be used for the lubricated of high temperature fan shaft bearing, spot contact bearing, motor car engine, textile drying machine etc.In silica gel, add appropriate high phenyl silicone oil as high temperature resistant auxiliary agent, can improve the resistance to elevated temperatures of organic silica gel.
5. the performances such as silicon carbide is corrosion-resistant owing to having, high temperature resistant, intensity is large, heat conductivility is good, shock resistance, wear resisting property is good, frictional coefficient is little.It is the ideal material of manufacturing high temperature material and high-performance sealed device.By adding a certain amount of silicon carbide as high temperature resistant filler in silica gel, can improve the resistance to elevated temperatures of organic silica gel.
UUU
accompanying drawing explanation
Fig. 1 is the production material figure of the preferred embodiment of the invention;
U
embodiment
The invention provides a kind of room temperature curing type one-component thermostable silica gel, its formulation ratio is:
Hydroxy-end capped polysiloxane 100 weight parts;
Silicone oil 1～5 weight part;
Poly-Union carbide A-162 5～20 weight parts;
Synthetic strengthening agent 10～20 weight parts;
Reinforced filling 10～20 weight parts;
High temperature resistant filler 50～200 weight parts;
Linking agent 2～10 weight parts;
Coupling agent 2～5 weight parts;
Catalyzer 0.2～2 weight part.
As preferably, described hydroxy-end capped polysiloxane adopts α, alpha, omega-dihydroxy polydimethyl siloxane; Silicone oil adopts phenyl silicone oil; Reinforced filling adopts nano imvite; High temperature resistant filler adopts black silicon carbide; Linking agent adopts one of them kind in methyl tributanoximo silane, vinyl tributyl ketoximyl silane; Coupling agent adopts γ-aminopropyl triethoxysilane; Catalyzer adopts dibutyl tin dilaurate.
The preparation method of room temperature curing type one-component thermostable silica gel as mentioned above, its preparation process is as follows:
S1, by hydroxy-end capped polysiloxane 100 weight parts, silicone oil 1～5 weight part, poly-Union carbide A-162 5～20 weight parts, synthetic strengthening agent 10～20 weight parts, reinforced filling 10～20 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 20～60rpm 60 minutes;
S2, add high temperature resistant filler 50～200 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 20～60rpm 120 minutes;
S3, add linking agent 2～10 weight parts, coupling agent 2～5 weight parts, catalyzer 0.5～2 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1～0.5 MPa, revolution 20～60rpm.
The preparation method of described synthetic strengthening agent is as follows: tetraethoxy, poly-Union carbide A-162, trimethyl silanol, ethanol, aqueous acetic acid are reacted 3～4 hours for 100:20～100:150～300:60～80:5～15 mix successively by weight under the condition of 40～60 ℃, reacted mixture is at 40～60 ℃, and under the condition of-0.1～-0.5MPa, underpressure distillation makes.
The present invention mainly, by synthesizing the composite of strengthening agent, reinforced filling and high temperature resistant auxiliary agent, is all improved the mechanical property of organic silica gel and resistance to elevated temperatures, specific as follows:
1. adopt synthetic strengthening agent to improve the mechanical property of organic silica gel.On the one hand, after macromole in synthetic strengthening agent disperses, a plurality of 3 D cross-linked centers have been formed, crosslinked center and high-polymer molecular interchain have stronger effect, they adsorb mutually, and interchain is wound around mutually, present dispersion, effectively eliminate interfacial energy between the two poor, further improved the ability to bear of high-temp glue counter stress of the present invention; On the other hand, because crosslinked center itself is polysiloxane structure, there is good flexible ability, increased the tensile yield of system, also delayed the fracture process of compound system simultaneously, increased the tensile yield of high-temperature plastic of the present invention; Thereby reach the effect of reinforcement.
2. adopt nano imvite to substitute traditional white carbon black and as reinforced filling, improve the mechanical property of organic silica gel.Nano imvite is applied the nano modification that is mainly used in rubber item in rubber, improves its resistance to air loss, the power that surely extends and wear resistance, preservative property, weather resisteant, chemical resistant properties.By adding appropriate nano imvite, can make the performance such as intensity, elongation of rubber increase substantially, some performances can improve several times, alternative current White Carbon black.Adopt nano imvite replacement white carbon black to have three aspects as the reason of reinforced filling:
(1) white carbon black surface, with the higher hydroxyl of activity, at high temperature makes Si-O bond fission, causes main chain DeR;
(2) planar water of white carbon black remained on surface at high temperature also can make Si-O hydrolytic cleavage, causes silicon rubber poor heat stability at high temperature, and use temperature is not high;
(3) white carbon black is difficult to infiltrate and disperse in organic phase.
3. because poly-Union carbide A-162 has hydrophobic nature and higher thermotolerance, in silica gel, add appropriate poly-Union carbide A-162 as high temperature resistant auxiliary agent, can improve the resistance to elevated temperatures of organic silica gel.
4. high phenyl silicone oil thermostability is higher, also has good radiation resistance, can be used as thermal treatment bath, heat oil, the gas-chromatography carrier of metal products, the high sub-zero oil of electronics, electric installation, the high temperature grease that adds carbon black, lithium soap or molybdenumdisulphide to make can be used for the lubricated of high temperature fan shaft bearing, spot contact bearing, motor car engine, textile drying machine etc.In silica gel, add appropriate high phenyl silicone oil as high temperature resistant auxiliary agent, can improve the resistance to elevated temperatures of organic silica gel.
5. the performances such as silicon carbide is corrosion-resistant owing to having, high temperature resistant, intensity is large, heat conductivility is good, shock resistance, wear resisting property is good, frictional coefficient is little.It is the ideal material of manufacturing high temperature material and high-performance sealed device.By adding a certain amount of silicon carbide as high temperature resistant filler in silica gel, can improve the resistance to elevated temperatures of organic silica gel.
By specific embodiment, the present invention is described below, but the present invention is not merely defined in these embodiment, simultaneously in embodiment, umber is by weight.
Embodiment 1:
1. by α, alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, phenyl silicone oil 2 weight parts, poly-Union carbide A-162 12 weight parts, synthetic strengthening agent 12 weight parts, nano imvite 15 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 60 minutes;
2. add black silicon carbide 140 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1 MPa, stirs under revolution 40rpm 120 minutes;
3. add vinyl tributyl ketoximyl silane 4 weight parts, methyl tributanoximo silane 3 weight parts, γ-aminopropyl triethoxysilane 4 weight parts, dibutyl tin dilaurate 0.4 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1MPa, revolution 40rpm.
Embodiment 2:
1. by α, alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, phenyl silicone oil 3 weight parts, poly-Union carbide A-162 10 weight parts, synthetic strengthening agent 15 weight parts, nano imvite 12 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 60 minutes;
2. add black silicon carbide 100 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1 MPa, stirs under revolution 40rpm 120 minutes;
3. add vinyl tributyl ketoximyl silane 3 weight parts, methyl tributanoximo silane 4 weight parts, γ-aminopropyl triethoxysilane 3 weight parts, dibutyl tin dilaurate 0.6 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1MPa, revolution 40rpm.
Embodiment 3:
1. by α, alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, phenyl silicone oil 2.5 weight parts, poly-Union carbide A-162 16 weight parts, synthetic strengthening agent 13 weight parts, nano imvite 14 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 60 minutes;
2. add black silicon carbide 110 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1 MPa, stirs under revolution 40rpm 120 minutes;
3. add vinyl tributyl ketoximyl silane 5 weight parts, methyl tributanoximo silane 3 weight parts, γ-aminopropyl triethoxysilane 2.5 weight parts, dibutyl tin dilaurate 0.8 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1MPa, revolution 40rpm.
Embodiment 4:
1. by α, alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, phenyl silicone oil 4 weight parts, poly-Union carbide A-162 9 weight parts, synthetic strengthening agent 10 weight parts, nano imvite 17 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 60 minutes;
2. add black silicon carbide 90 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1 MPa, stirs under revolution 40rpm 120 minutes;
3. add vinyl tributyl ketoximyl silane 2 weight parts, methyl tributanoximo silane 5 weight parts, γ-aminopropyl triethoxysilane 3.5 weight parts, dibutyl tin dilaurate 0.5 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1MPa, revolution 40rpm.
Embodiment 5:
1. by α, alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, phenyl silicone oil 1.5 weight parts, poly-Union carbide A-162 17 weight parts, synthetic strengthening agent 14 weight parts, nano imvite 13 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 60 minutes;
2. add black silicon carbide 160 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1 MPa, stirs under revolution 40rpm 120 minutes;
3. add vinyl tributyl ketoximyl silane 2.5 weight parts, methyl tributanoximo silane 2.5 weight parts, γ-aminopropyl triethoxysilane 2 weight parts, dibutyl tin dilaurate 1 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1MPa, revolution 40rpm.
Embodiment 6:
1. by α, alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, phenyl silicone oil 2 weight parts, poly-Union carbide A-162 14 weight parts, synthetic strengthening agent 11 weight parts, nano imvite 16 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 60 minutes;
2. add black silicon carbide 120 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1 MPa, stirs under revolution 40rpm 120 minutes;
3. add vinyl tributyl ketoximyl silane 3 weight parts, methyl tributanoximo silane 2 weight parts, γ-aminopropyl triethoxysilane 2.8 weight parts, dibutyl tin dilaurate 0.4 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1MPa, revolution 40rpm.
Embodiment 7:
1. by α, alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, phenyl silicone oil 3.5 weight parts, poly-Union carbide A-162 8 weight parts, synthetic strengthening agent 16 weight parts, nano imvite 11 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 60 minutes;
2. add black silicon carbide 80 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1 MPa, stirs under revolution 40rpm 120 minutes;
3. add vinyl tributyl ketoximyl silane 2 weight parts, methyl tributanoximo silane 3 weight parts, γ-aminopropyl triethoxysilane 5 weight parts, dibutyl tin dilaurate 0.2 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1MPa, revolution 40rpm.
Embodiment 8:
1. by α, alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, phenyl silicone oil 3 weight parts, poly-Union carbide A-162 15 weight parts, synthetic strengthening agent 10 weight parts, nano imvite 18 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 60 minutes;
2. add black silicon carbide 150 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 120 minutes;
3. add vinyl tributyl ketoximyl silane 4 weight parts, methyl tributanoximo silane 4.5 weight parts, γ-aminopropyl triethoxysilane 4 weight parts, dibutyl tin dilaurate 0.3 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1MPa, revolution 40rpm.
Embodiment 9:
1. by α, alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, phenyl silicone oil 1 weight part, poly-Union carbide A-162 5 weight parts, synthetic strengthening agent 18 weight parts, nano imvite 10 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 60 minutes;
2. add black silicon carbide 50 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 120 minutes;
3. add vinyl tributyl ketoximyl silane 1 weight part, methyl tributanoximo silane 1 weight part, γ-aminopropyl triethoxysilane 4.5 weight parts, dibutyl tin dilaurate 1.2 weight parts, make room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1MPa, revolution 40rpm.
Embodiment 10:
1. by α, alpha, omega-dihydroxy polydimethyl siloxane 100 weight parts, phenyl silicone oil 5 weight parts, poly-Union carbide A-162 20 weight parts, synthetic strengthening agent 20 weight parts, nano imvite 20 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 60 minutes;
2. add black silicon carbide 200 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 40rpm 120 minutes;
3. add vinyl tributyl ketoximyl silane 4 weight parts, methyl tributanoximo silane 6 weight parts, γ-aminopropyl triethoxysilane 5 weight parts, dibutyl tin dilaurate 2 weight parts, make room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1MPa, revolution 40rpm.
A kind of room temperature curing type one-component thermostable silica gel above the invention enforcement being provided and preparation method thereof is described in detail, for one of ordinary skill in the art, thought according to the invention embodiment, all will change in specific embodiments and applications, in sum, this description should not be construed as the restriction to the invention.
Claims (10)
1. a room temperature curing type one-component thermostable silica gel, is characterized in that: its formulation ratio is:
Hydroxy-end capped polysiloxane 100 weight parts;
Silicone oil 1～5 weight part;
Poly-Union carbide A-162 5～20 weight parts;
Synthetic strengthening agent 10～20 weight parts;
Reinforced filling 10～20 weight parts;
High temperature resistant filler 50～200 weight parts;
Linking agent 2～10 weight parts;
Coupling agent 2～5 weight parts;
Catalyzer 0.2～2 weight part.
2. room temperature curing type one-component thermostable silica gel as claimed in claim 1, is characterized in that: described hydroxy-end capped polysiloxane is α, alpha, omega-dihydroxy polydimethyl siloxane.
3. room temperature curing type one-component thermostable silica gel as claimed in claim 1, is characterized in that: described silicone oil is phenyl silicone oil.
4. room temperature curing type one-component thermostable silica gel as claimed in claim 1, it is characterized in that: described reinforced filling is nano imvite, adopt nano imvite to substitute traditional white carbon black and as reinforced filling, improve the mechanical property of organic silica gel, nano imvite can improve its resistance to air loss, surely the power that extends and wear resistance, preservative property, weather resisteant, chemical resistant properties, by adding appropriate nano imvite, can make the performance such as intensity, elongation of rubber increase substantially, some performances can improve several times.
5. room temperature curing type one-component thermostable silica gel as claimed in claim 1, is characterized in that: described high temperature resistant filler is black silicon carbide.
6. room temperature curing type one-component thermostable silica gel as claimed in claim 1, is characterized in that: described linking agent is one of them kind in methyl tributanoximo silane, vinyl tributyl ketoximyl silane.
7. room temperature curing type one-component thermostable silica gel as claimed in claim 1, is characterized in that: described coupling agent is γ-aminopropyl triethoxysilane.
8. room temperature curing type one-component thermostable silica gel as claimed in claim 1, is characterized in that: described catalyzer is dibutyl tin dilaurate.
9. as described in as arbitrary in claim 1-8, the preparation method of room temperature curing type one-component thermostable silica gel, is characterized in that, the preparation process of described room temperature curing type one-component thermostable silica gel is as follows:
S1, by hydroxy-end capped polysiloxane 100 weight parts, silicone oil 1～5 weight part, poly-Union carbide A-162 5～20 weight parts, synthetic strengthening agent 10～20 weight parts, reinforced filling 10～20 weight parts add in stirrer, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 20～60rpm 60 minutes;
S2, add high temperature resistant filler 50～200 weight parts, be heated to 120 ℃, vacuumize, vacuum tightness 0.1MPa, stirs under revolution 20～60rpm 120 minutes;
S3, add linking agent 2～10 weight parts, coupling agent 2～5 weight parts, catalyzer 0.5～2 weight part, makes room temperature curing type one-component thermostable silica gel after stirring 10 minutes under vacuum tightness 0.1～0.5 MPa, revolution 20～60rpm.
10. the preparation method of room temperature curing type one-component thermostable silica gel as claimed in claim 9, it is characterized in that, the preparation method of described synthetic strengthening agent is as follows: tetraethoxy, poly-Union carbide A-162, trimethyl silanol, ethanol, aqueous acetic acid are reacted 3～4 hours for 100:20～100:150～300:60～80:5～15 mix successively by weight under the condition of 40～60 ℃, reacted mixture is at 40～60 ℃, and under the condition of-0.1～-0.5MPa, underpressure distillation makes.
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| CN201310720589.8A CN103709759A (en) | 2013-12-24 | 2013-12-24 | Room temperature cured single-component high temperature resisting silica gel and preparation method thereof |
| PCT/CN2013/090838 WO2015096172A1 (en) | 2013-12-24 | 2013-12-30 | Room temperature-cured mono-component high-temperature-resistant silica gel and preparation method therefor |
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Cited By (6)
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| CN104610751A (en) * | 2015-01-23 | 2015-05-13 | 刘滨 | High-temperature-resisting and flame retardant single-component deoximation type room temperature vulcanized silicone rubber and preparation method thereof |
| CN105111935A (en) * | 2015-09-02 | 2015-12-02 | 航天材料及工艺研究所 | High-temperature-resistant and high-radiation-resistant thermal control coating and preparation method thereof |
| CN105602257A (en) * | 2015-11-19 | 2016-05-25 | 武汉市知富企业管理咨询有限公司 | High-temperature modified silicone rubber and preparation method thereof |
| CN110194898A (en) * | 2019-07-04 | 2019-09-03 | 宁波佳乐特橡塑机电有限公司 | A kind of high-strength rubber transmission belt and production method |
| CN111255168A (en) * | 2020-01-17 | 2020-06-09 | 安徽润辉高分子材料科技有限公司 | Five-layer self-adhesive moisture-proof material, application, equipment and manufacturing process thereof |
| CN114196371A (en) * | 2021-11-30 | 2022-03-18 | 广州市白云化工实业有限公司 | Dealcoholized silicone structure sealant |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103436028A (en) * | 2013-07-26 | 2013-12-11 | 深圳市钧泰丰新材料有限公司 | Room temperature curing type one-component high temperature resistant silica gel and preparation method thereof |
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| CN102020854A (en) * | 2010-11-19 | 2011-04-20 | 广东三和化工科技有限公司 | Single-component heat-resisting silicon sealant |
| CN103361023A (en) * | 2013-08-02 | 2013-10-23 | 东莞兆舜有机硅新材料科技有限公司 | Transparent dealcoholized single-component RTV silicone rubber sealant and preparation method thereof |
| CN103387811A (en) * | 2013-08-14 | 2013-11-13 | 福建瑞森化工有限公司 | Organic silicon rubber waterproof adhesive and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103436028A (en) * | 2013-07-26 | 2013-12-11 | 深圳市钧泰丰新材料有限公司 | Room temperature curing type one-component high temperature resistant silica gel and preparation method thereof |
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| CN104610751A (en) * | 2015-01-23 | 2015-05-13 | 刘滨 | High-temperature-resisting and flame retardant single-component deoximation type room temperature vulcanized silicone rubber and preparation method thereof |
| CN104610751B (en) * | 2015-01-23 | 2017-05-10 | 刘滨 | High-temperature-resisting and flame retardant single-component deoximation type room temperature vulcanized silicone rubber and preparation method thereof |
| CN105111935A (en) * | 2015-09-02 | 2015-12-02 | 航天材料及工艺研究所 | High-temperature-resistant and high-radiation-resistant thermal control coating and preparation method thereof |
| CN105111935B (en) * | 2015-09-02 | 2017-08-29 | 航天材料及工艺研究所 | A kind of high temperature resistant height radiation thermal control coating and preparation method thereof |
| CN105602257A (en) * | 2015-11-19 | 2016-05-25 | 武汉市知富企业管理咨询有限公司 | High-temperature modified silicone rubber and preparation method thereof |
| CN110194898A (en) * | 2019-07-04 | 2019-09-03 | 宁波佳乐特橡塑机电有限公司 | A kind of high-strength rubber transmission belt and production method |
| CN111255168A (en) * | 2020-01-17 | 2020-06-09 | 安徽润辉高分子材料科技有限公司 | Five-layer self-adhesive moisture-proof material, application, equipment and manufacturing process thereof |
| CN114196371A (en) * | 2021-11-30 | 2022-03-18 | 广州市白云化工实业有限公司 | Dealcoholized silicone structure sealant |
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| WO2015096172A1 (en) | 2015-07-02 |
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