CN103911113B - Thermostable silicone sealant and preparation method thereof - Google Patents
Thermostable silicone sealant and preparation method thereof Download PDFInfo
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- CN103911113B CN103911113B CN201310002398.8A CN201310002398A CN103911113B CN 103911113 B CN103911113 B CN 103911113B CN 201310002398 A CN201310002398 A CN 201310002398A CN 103911113 B CN103911113 B CN 103911113B
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Abstract
The invention provides a kind of thermostable silicone sealant, comprising: the matrix resin of 20 ~ 70 weight parts, the strengthening agent of 30 ~ 90 weight parts, the silane coupling agent of 0.1 ~ 20 weight part, the mill base of 1 ~ 20 weight part, the part by weight of catalyst of 0.001 ~ 10, the linking agent of 0.1 ~ 10 weight part; The mineral oil of 0.1 ~ 20 weight part; The ceramic with heat resistance powder of 5 ~ 15 weight parts.Owing to introducing the ceramic with heat resistance powder with resistance to elevated temperatures in silicone sealant, and active function groups in linking agent and matrix resin generation crosslinked action, make sealing glue solidifying, thus make seal gum have higher high thermal resistance.Present invention also offers a kind of preparation method of thermostable silicone sealant.
Description
Technical field
The present invention relates to seal gum technical field, particularly relate to a kind of thermostable silicone sealant and preparation method thereof.
Background technology
Silicone sealant is the one in seal gum, belongs to same system with glass cement, a kind of material namely formed by materials such as water glass, organosilicon and silicone structure polymkeric substance.Silicone sealant has excellent weather, damp and hot, ultraviolet and ozone ageing performance thereof, is one of building sealant preferred material.Along with the modernization of urban architecture, design and construction are progressive and the update of finishing class, and improving constantly functional requirements such as building energy conservation, waterproof, heat insulation, sound insulation and comfortablenesses, the development of silicone sealant has good market atmosphere.
Although building sealant market outlook are more and more prosperous, still there are many seal gum products to occur many problems in production and use procedure, such as, there will be viscosity peak in production process too high; The a series of problems such as in use occur that rubber vulcanization speed is excessively slow, sulfuration back draft intensity and elongation at break are not up to standard, package stability difference.The thermotolerance of seal gum of the prior art is especially poor, as: long-time sealing more than 200 DEG C, position Working environment can not be born, or the Working environment of the instantaneous temperature of less than 300 DEG C.In order to improve the resistance to elevated temperatures of conventional seals glue, the present invention proposes a kind of thermostable silicone sealant.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of resistant to elevated temperatures silicone sealant and preparation method thereof.
In view of this, the invention provides a kind of silicone sealant, comprising:
Matrix resin 20 ~ 70 weight part;
Strengthening agent 30 ~ 90 weight part;
Silane coupling agent 0.1 ~ 20 weight part;
Mill base 1 ~ 20 weight part;
Catalyzer 0.001 ~ 10 weight part;
Linking agent 0.1 ~ 10 weight part;
Mineral oil 0.1 ~ 20 weight part;
Ceramic with heat resistance powder 5 ~ 15 weight part.
Preferably, described matrix resin is the α-ω polysiloxanediol with formula I structure, and the viscosity of described α-ω polysiloxanediol is 20000mPas ~ 80000mPas;
Wherein, R is CH
3-or CH
3cH
2-; N is 50 ~ 5000.
Preferably, described strengthening agent is one or more in titanium dioxide, coarse whiting, active nano-calcium carbonate and light calcium carbonate.
Preferably, described silane coupling agent is one or more in vinyl three ('beta '-methoxy oxyethyl group) silane, vinyltriethoxysilane, γ-thin propyl trimethoxy silicane, APTES and γ-glycidyl ether oxygen propyl trimethoxy silicane.
Preferably, described catalyzer is one or more in di-n-butyl tin acetate in February, dibutyl tin dilaurate and isopropyl titanate.
Preferably, described linking agent is one or more in methyl tributanoximo silane, vinyl tributyl ketoximyl silane and methyl triacetoxysilane.
Preferably, described ceramic with heat resistance powder is the density of described ceramic with heat resistance powder is 1.85 ~ 2.5g/cm
3, particle diameter is 20 ~ 120 μm.
Preferably, described mill base is the mill base obtained after carbon black mixes with α-ω polysiloxanediol or polydimethylsiloxane; With the weight percent meter of mill base, described carbon black is 30 ~ 100 weight parts, and the viscosity of described α-ω polysiloxanediol is 2000mPas ~ 4000mPas, and the viscosity of described polydimethylsiloxane is 200mPas ~ 500mPas.
Preferably, described mineral oil is white oil.
Present invention also offers a kind of preparation method of silicone sealant, comprising:
The strengthening agent of the matrix resin of 20 ~ 70 weight parts with 30 ~ 90 weight parts is mixed, obtains basic glue;
The ceramic with heat resistance powder of the linking agent of the catalyzer of the mill base of silane coupled, 1 ~ 20 weight part of 0.1 ~ 20 weight part, 0.001 ~ 10 weight part, 0.1 ~ 10 weight part, 0.1 ~ 20 weight part mineral oil, 5 ~ 15 weight parts is mixed with described basic glue, after reaction, obtains silicone sealant.
The invention provides a kind of silicone sealant, comprising: the matrix resin of 20 ~ 70 weight parts; The strengthening agent of 30 ~ 90 weight parts; The silane coupling agent of 0.1 ~ 20 weight part; The mill base of 1 ~ 20 weight part; The catalyzer of 0.001 ~ 10 weight part; The linking agent of 0.1 ~ 10 weight part; The mineral oil of 0.1 ~ 20 weight part; The ceramic with heat resistance powder of 5 ~ 15 weight parts.Under the effect of catalyzer, there is crosslinking reaction, define silicone elastomer, thus obtain organic silicone sealing agent in matrix resin of the present invention and linking agent.Owing to introducing ceramic with heat resistance powder in silicone sealant, and active function groups in linking agent and matrix resin generation crosslinked action, make sealing glue solidifying, thus make seal gum have good high thermal resistance.Secondly, by adding strengthening agent and silane coupling agent, be conducive to the intensity and the cohesiveness that improve silicone sealant.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The embodiment of the invention discloses a kind of thermostable silicone sealant, comprising:
Matrix resin 20 ~ 70 weight part;
Strengthening agent 30 ~ 90 weight part;
Silane coupling agent 0.1 ~ 20 weight part;
Mill base 1 ~ 20 weight part;
Catalyzer 0.001 ~ 10 weight part;
Linking agent 0.1 ~ 10 weight part;
Mineral oil 0.1 ~ 20 weight part;
Ceramic with heat resistance powder 5 ~ 15 weight part.
The invention provides a kind of thermostable silicone sealant, comprising: the matrix resin of 20 ~ 70 weight parts; The strengthening agent of 30 ~ 90 weight parts; The silane coupling agent of 0.1 ~ 20 weight part; The mill base of 1 ~ 20 weight part; The catalyzer of 0.001 ~ 10 weight part; The linking agent of 0.1 ~ 10 weight part; The mineral oil of 0.1 ~ 20 weight part; The ceramic with heat resistance powder of 5 ~ 15 weight parts.Matrix resin of the present invention and linking agent are under the effect of catalyzer, there is crosslinking reaction, define silicone elastomer, thus complete the preparation of organic silicone sealing agent, owing to introducing the ceramic with heat resistance powder with high heat resistance in silicone sealant, and active function groups in linking agent and matrix resin generation crosslinked action, make sealing glue solidifying, make seal gum have higher thermotolerance.Secondly, by adding strengthening agent and silane coupling agent, thus improve intensity and the cohesiveness of silicone sealant.
According to the present invention, described matrix resin preferably has the α-ω polysiloxanediol of formula I structure, and the viscosity of described α-ω polysiloxanediol is preferably 20000mPas ~ 80000mPas, is more preferably 35000mPas ~ 65000mPas; Described matrix resin containing active function groups, can with linking agent generation crosslinking reaction.The character such as molecular size range, molecular structure, molecular weight distribution of matrix resin described in the present invention, can affect the performance of the aspects such as the hardness of sealing agent, viscosity, levelling property, flow.Described matrix resin is 20 ~ 70 weight parts, is preferably 30 ~ 60 weight parts.
Wherein, R is independently selected from CH
3-or CH
3cH
2-; N is 50 ~ 5000.
The present invention adds the strengthening agent with strengthening action in silicone sealant, and the kind, modification situation etc. of described strengthening agent also can affect the character such as the tensile strength of seal gum, tear strength and viscosity.Described strengthening agent be preferably in titanium dioxide, coarse whiting, active nano-calcium carbonate and light calcium carbonate one or more.Described strengthening agent is 30 ~ 90 weight parts, is preferably 40 ~ 80 weight parts.
Described silane coupling agent can increase the consistency of strengthening agent and other components, improves the bond strength between resin and strengthening agent surface and weather resistance.Described silane coupling agent is preferably one or more in propyl trimethoxy silicane, APTES and γ-glycidyl ether oxygen propyl trimethoxy silicane of vinyl three ('beta '-methoxy oxyethyl group) silane, vinyltriethoxysilane, γ-dredge.Described silane coupling agent is 0.1 ~ 20 weight part, is preferably 5 ~ 15 weight parts.
Described mill base mainly plays toning effect, and described mill base is preferably the mill base obtained after carbon black mixes with α-ω polysiloxanediol or polydimethylsiloxane; With the weight percent meter of mill base, described carbon black is 30 ~ 100 weight parts, the viscosity of described α-ω polysiloxanediol is 2000mPas ~ 4000mPas, the viscosity of described polydimethylsiloxane is that 200mPas ~ 500mPas, α-ω polysiloxanediol or polydimethylsiloxane are preferably 100 ~ 250 weight parts.Described mill base is 1 ~ 20 weight part, is preferably 4 ~ 16 weight parts.
According to the present invention, in silicone sealant, with the addition of catalyzer, the reaction of described catalyst matrix resin and linking agent, its addition and add the factor such as kind and can affect set time of linking agent, intensity and application property etc.Described catalyzer be preferably in di-n-butyl tin acetate in February, di-n-butyl tin dilaurate tin and isopropyl titanate one or more.Described catalyzer is 0.001 ~ 10 weight part, is preferably 1 ~ 8 weight part.
Containing active function groups in described linking agent, can with matrix resin generation crosslinking reaction, make sealing glue solidifying.Described linking agent be preferably in methyl tributanoximo silane, vinyl tributyl ketoximyl silane and methyl triacetoxysilane one or more.Described linking agent is 0.1 ~ 10 weight part, is preferably 2 ~ 8 weight parts.
The present invention with the addition of mineral oil in silicone sealant, and described mineral oil mainly plays plastification, can change the elasticity after sealing glue solidifying, regulates the character such as elongation rate of tensile failure, elastic restoration ratio of seal gum.Described mineral oil is 0.1 ~ 20 weight part, is preferably 2 ~ 15 weight parts.Described mineral oil is preferably white oil, is more preferably one or more in white oil 10#, white oil 15#, white oil 26#, white oil 46# and white oil 68#.
According to the present invention, with the addition of ceramic with heat resistance powder in silicone sealant, described ceramic with heat resistance powder is preferably zirconia-based ceramic powder, such as Nd
2zr
2o
7or CeO
2-Nd
2o-ZrO
2ceramic powder.The density of described ceramic with heat resistance powder is preferably 1.85 ~ 2.5g/cm
3, particle diameter is preferably 20 ~ 120 μm.Described ceramic with heat resistance powder has higher high thermal resistance, it can be used as the component of seal gum, and seal gum also can be made to have higher high thermal resistance.Described ceramic with heat resistance powder is 5 ~ 15 weight parts, is more preferably 8 ~ 10 weight parts.
Present invention also offers the preparation method of thermostable silicone sealant, comprising: the strengthening agent of the matrix resin of 20 ~ 70 weight parts with 30 ~ 90 weight parts is mixed, stir, obtain basic glue;
The ceramic with heat resistance powder of the linking agent of the catalyzer of the mill base of silane coupled, 1 ~ 20 weight part of 0.1 ~ 20 weight part, 0.001 ~ 10 weight part, 0.1 ~ 10 weight part, 0.1 ~ 20 weight part mineral oil, 5 ~ 15 weight parts is mixed with described basic glue, stir, obtain stone material silicone sealant.
According to the present invention, in the process preparing silicone sealant, first carry out the preparation of basic glue, described basic glue mixes obtained colloid by matrix resin with strengthening agent, in order to make the performance of silicone sealant more excellent, preferably, the preparation method of described basic glue is specially:
The base resin of 1/2 ~ 2/3 is placed in kneader, kneading limit, limit pan feeding, rotating speed is 40 ~ 50r/min, base resin add complete after, progressively drop into the strengthening agent of 30 ~ 90 weight parts, rotating speed is 40 ~ 50r/min.After treating that whole strengthening agent drops into, mediate to temperature of charge and rise to 110 DEG C, rotating speed 50r/min.Vacuumize when temperature rises to 110 DEG C, after being evacuated to-0.04 ~-0.1Mpa, mediate 0.5 ~ 4h, rotating speed 50r/min.Then vacuum is unloaded, open solvent or diluent valve, suction residue base resin, rotating speed 50r/min, after treating the whole suction of base resin, close material sucking valve, open vacuum valve, be evacuated to-0.04 ~-0.1Mpa, after vacuumizing kneading 0.5 ~ 4h, unload vacuum ON cycle pump, circulate 10min while stirring, rotating speed 50r/min.In basic glue glue preparation process, if temperature rises to 130 DEG C, reduce rotating speed to 35r/min, when temperature does not reduce yet and reaches 150 DEG C, should ON cycle water coolant rapidly, during lower than 120 DEG C, closedown recirculated cooling water, rotating speed rises to 50r/min.
After prepared by basic glue, namely the preparation of silicone sealant is carried out, described mill base, catalyzer, linking agent, silane coupling agent, mineral oil are mixed with ceramic with heat resistance powder, silicone sealant is obtained after stirring, wherein mill base is as the main raw material making seal gum, preferably, the preparation method of described mill base is specially:
Be the α of 2000mPas ~ 4000mPas by viscosity, one or both kneading limit, limit pan feedings in alpha, omega-dihydroxy polysiloxane and 200mPas ~ 500mPas polydimethylsiloxanes, rotating speed is 50r/min, progressively drops into whole carbon black, and rotating speed is 50r/min.After whole carbon black drops into, mediate 1 ~ 5h, obtain mill base.
According to the present invention, the preparation method of described pollution-free stone material silicone silicone sealant is specially:
In stirrer still, add basic glue, mineral oil, mill base and ceramic with heat resistance powder, be evacuated to more than-0.04 ~-0.09MPa, then start vacuum stirring 10 ~ 60min, the rotating speed of stirrer is adjusted to 300r/min; In still, material is cooled to and in still, adds linking agent lower than when 30 ~ 60 DEG C, and vacuumize, the rotating speed of stirrer is adjusted to 300r/min, and churning time is 10 ~ 60min; Stop stirring, emptying solution vacuum, rises kettle cover, adds silane coupling agent and catalyzer, vacuumize in still, and rotating speed is 300r/min, churning time 10 ~ 30min, stops stirring, and separates vacuum and rise kettle cover, obtain silicone sealant.
The invention provides a kind of thermostable silicone sealant, comprising: the matrix resin of 20 ~ 70 weight parts; The strengthening agent of 30 ~ 90 weight parts; The silane coupling agent of 0.1 ~ 20 weight part; The mill base of 1 ~ 20 weight part; The catalyzer of 0.001 ~ 10 weight part; The linking agent of 0.1 ~ 10 weight part; The mineral oil of 0.1 ~ 20 weight part; The ceramic with heat resistance powder of 5 ~ 15 weight parts.Matrix resin of the present invention and linking agent are under the effect of catalyzer, there is crosslinking reaction, define silicone elastomer, thus complete the preparation of organic silicone sealing agent, owing to introducing the ceramic with heat resistance powder with high thermal resistance in silicone sealant, and active function groups in linking agent and matrix resin generation crosslinked action, make sealing glue solidifying, thus make seal gum have higher resistance to elevated temperatures.Secondly, by adding strengthening agent and silane coupling agent, thus being conducive to the intensity and the cohesiveness that improve silicone sealant, in various boisterous environment, still can keeping good physicals.On the other hand, basic glue and other, in the process preparing silicone sealant, by first preparing basic glue, then are added auxiliary agent and are mixed with seal gum, make the mechanical property of seal gum obtain larger raising by the present invention.
In order to understand the present invention further, be described in detail to silicone sealant provided by the invention and preparation method thereof below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
The various components that the present embodiment adopts are commercially available prod.
Embodiment 1
The α of kneader suction 25 weight part, alpha, omega-dihydroxy polysiloxane are opened in the preparation of basis glue, kneading limit, limit pan feeding, and the rotating speed of kneader is adjusted to 50r/min; Progressively drop into the active nano-calcium carbonate of 60 weight parts and the water-ground limestone of 10 weight parts, the rotating speed of kneader is 50r/min, and mediate temperature of charge to 110 DEG C, rotating speed is 50r/min, mediate when temperature rises to 110 DEG C and vacuumize, after being evacuated to-0.04 ~-0.1Mpa, mediate 4h; Then kneader is unloaded vacuum, open solvent or diluent valve, the α of remaining 25 weight parts of suction, alpha, omega-dihydroxy polysiloxane, the rotating speed of kneader is adjusted to 50r/min, close material sucking valve after treating the whole suction of base resin, open vacuum valve, be evacuated to-0.04 ~-0.1Mpa, vacuumize after mediating 2h and unload vacuum ON cycle pump, circulate 10min while stirring, and rotating speed is 50r/min, obtains basic glue.In process prepared by basic glue, if the temperature of kneader rises to 130 DEG C, then reduce rotating speed to 35r/min, do not reduce yet when temperature and reach 150 DEG C, should ON cycle water coolant rapidly, during lower than 120 DEG C, closedown recirculated cooling water, rotating speed rises to 50r/min.
The viscosity of 100 weight parts is kneading limit, 200mPas polydimethylsiloxanes limit pan feeding by the preparation of mill base, and the rotating speed of kneader is 50r/min, and progressively drop into the carbon black of 30 weight parts, rotating speed is 50r/min, treats that carbon black mediates 2h after dropping into, obtains mill base.
The preparation of silicone sealant adds basic glue, the white oil of 6 weight parts, the mill base of 12 weight parts of above-mentioned preparation in stirrer still, is evacuated to more than-0.04 ~-0.09MPa, and start vacuum stirring 30min, rotating speed is 300r/min; When material is cooled to lower than 30 DEG C in still, adds the methyl tributanoximo silane of 9 weight parts, vacuumize in still, rotating speed is 300r/min, and churning time is 40min; Then stop stirring, emptying solution vacuum, rise kettle cover, in still, add the di-n-butyl tin acetate in February of the zirconia powder of 5 weight parts, the APTES of 1 weight part, the γ-glycidyl ether oxygen propyl trimethoxy silicane of 0.5 weight part and 0.05 weight part, vacuumize, rotating speed is 300r/min, churning time is 20min, finally stop stirring, and separate vacuum and rise kettle cover, obtain silicone sealant.The silicone sealant prepared by the present embodiment is tested under 1000 DEG C of oxy-acetylene flames, and silicone sealant can to remain unchanged shape at 10 ~ 15min.
Embodiment 2
The α of kneader machine suction 10 weight part is opened in the preparation of basis glue, alpha, omega-dihydroxy polysiloxane, kneading limit, limit pan feeding, the rotating speed of kneader is adjusted to 50r/min, progressively drop into the active nano-calcium carbonate of 70 weight parts and the light calcium carbonate of 20 weight parts, the rotating speed of kneader is 50r/min, mediates to temperature of charge and rises to 110 DEG C; The temperature of kneader vacuumizes when rising to 110 DEG C, mediates 4h after being evacuated to-0.04 ~-0.1Mpa, and the rotating speed of kneader is 50r/min.Then unload vacuum, open solvent or diluent valve, the α of remaining 10 weight parts of suction, alpha, omega-dihydroxy polysiloxane, the rotating speed of kneader is 50r/min, after treating the whole suction of base resin, closes material sucking valve, open vacuum valve, be evacuated to-0.04 ~-0.1Mpa, vacuumize after mediating 2h and unload vacuum ON cycle pump, circulate 10min while stirring, rotating speed 50r/min, obtains basic glue.
The viscosity of 210 weight parts is 300mPas α by the preparation of mill base, kneading limit, alpha, omega-dihydroxy polysiloxane limit pan feeding, and the rotating speed of kneader is 50r/min, progressively drop into the carbon black of 100 weight parts, the rotating speed of kneader is 50r/min, mediates 5h, obtain mill base after whole carbon black drops into.
The preparation of silicone sealant adds basic glue, the white oil of 4 weight parts, the mill base of 18 weight parts of above-mentioned preparation in stirrer still, when being evacuated to-0.04 ~-0.09MPa, and vacuum stirring 30min, rotating speed is 300r/min; In still, material is cooled to lower than adding the vinyl tributyl ketoximyl silane of 2 weight parts and the methyl tributanoximo silane of 7 weight parts when 50 DEG C in still, and vacuumize, rotating speed is 300r/min, after churning time 40min; Stop stirring, emptying solution vacuum, rises kettle cover, adds the Nd of 10 weight parts in still
2zr
2o
7powder, vinyl three ('beta '-methoxy oxyethyl group) silane of 6 weight parts, the vinyltriethoxysilane of 4 weight parts and the dibutyl tin dilaurate of 0.05 weight part, vacuumize, rotating speed is 300r/min, churning time is 20min, stops stirring, and separates vacuum, rise kettle cover, obtain silicone sealant.The silicone sealant prepared by the present embodiment is tested under 1000 DEG C of oxy-acetylene flames, and silicone sealant can to remain unchanged shape at 12 ~ 15min.
Embodiment 3
The α of kneader suction 40 weight part is opened in the preparation of basis glue, alpha, omega-dihydroxy polysiloxane, kneading limit, limit pan feeding, rotating speed is 50r/min, progressively drop into the light calcium carbonate of 30 weight parts, the titanium dioxide of 20 weight parts and the water-ground limestone of 20 weight parts, rotating speed is 50r/min, mediates to temperature of charge and rises to 110 DEG C; Temperature vacuumizes when rising to 110 DEG C, mediates 4h after being evacuated to-0.04 ~-0.1Mpa, rotating speed 50r/min.Unload vacuum, open solvent or diluent valve, the α of remaining 20 weight parts of suction, alpha, omega-dihydroxy polysiloxane, rotating speed is 50r/min, after treating the whole suction of basic glue, closes material sucking valve, open vacuum valve, be evacuated to-0.04 ~-0.1Mpa, vacuumize after mediating 2h and unload vacuum ON cycle pump, rotating speed is 50r/min, circulate 10min while stirring, obtains basic glue.
The viscosity of preparation 110 weight part of mill base is 400mPas α, kneading limit, the polydimethylsiloxane limit pan feeding of alpha, omega-dihydroxy polysiloxane and 100 weight parts, and rotating speed is 50r/min, progressively drop into the carbon black of 100 weight parts, rotating speed is 50r/min, mediates 5h, obtain mill base after whole carbon black drops into.
The preparation of silicone sealant adds basic glue, the white oil of 4 weight parts, the mill base of 15 weight parts of above-mentioned preparation in stirrer still, is evacuated to more than-0.04 ~-0.09MPa, and start vacuum stirring 30min, rotating speed is 300r/min; In still, material is cooled to lower than adding the vinyl tributyl ketoximyl silane of 1.5 weight parts and the methyl triacetoxysilane of 6 weight parts when 60 DEG C in still, vacuumizes, and rotating speed is 300r/min, and churning time is 40min; Stop stirring, emptying solution vacuum, rises kettle cover, adds the CeO of 15 weight parts in still
2-Nd
2o-ZrO
2ceramic powder, the γ of 3 weight parts-dredge propyl trimethoxy silicane, the APTES of 5 weight parts and the di-n-butyl tin acetate in February of 0.05 weight part, vacuumize, rotating speed is 300r/min, churning time is 20min, stops stirring, and separates vacuum, rise kettle cover, obtain silicone sealant.
Embodiment 4
The α of kneader suction 30 weight part is opened in the preparation of basis glue, alpha, omega-dihydroxy polysiloxane, kneading limit, limit pan feeding, rotating speed is 50r/min, progressively drop into the active nano-calcium carbonate of the light calcium carbonate of 20 weight parts, the titanium dioxide of 30 weight parts, the water-ground limestone of 20 weight parts and 20 weight parts, rotating speed is 50r/min, and mediate and rise to 110 DEG C to temperature of charge, rotating speed is 50r/min; Temperature vacuumizes when rising to 110 DEG C, mediates 4h after being evacuated to-0.04 ~-0.1Mpa, and rotating speed is 50r/min.Then unload vacuum, open solvent or diluent valve, the α of remaining 20 weight parts of suction, alpha, omega-dihydroxy polysiloxane, rotating speed is 50r/min, after treating the whole suction of base resin, closes material sucking valve, open vacuum valve, be evacuated to-0.04 ~-0.1Mpa, vacuumize after mediating 2h and unload vacuum ON cycle pump, circulate 10min while stirring, rotating speed is 50r/min, obtains basic glue.
The viscosity of preparation 140 weight part of mill base is 300mPas α, kneading limit, the polydimethylsiloxane limit pan feeding of alpha, omega-dihydroxy polysiloxane and 80 weight parts, and rotating speed is 50r/min, progressively drop into the carbon black of 90 weight parts, rotating speed is 50r/min, mediates 5h, obtain mill base after whole carbon black drops into.
The preparation of silicone sealant adds basic glue, the white oil of 4 weight parts, the mill base of 10 weight parts of above-mentioned preparation in stirrer still, is evacuated to more than-0.04 ~-0.09MPa, and start vacuum stirring 30min, rotating speed is 300r/min; In still, material is cooled to the methyl triacetoxysilane lower than adding 7 weight parts when 30 ~ 60 DEG C in still, vacuumizes, and rotating speed is 300r/min, and churning time is 40min; Then stop stirring, emptying solution vacuum, rises kettle cover, adds the CeO of 12 weight parts in still
2-Nd
2o-ZrO
2ceramic powder, the γ of 3 weight parts-dredge propyl trimethoxy silicane, the APTES of 5 weight parts and the di-n-butyl tin acetate in February of 0.05 weight part, vacuumize, rotating speed is 300r/min, churning time is 20min, stops stirring, and separates vacuum, rise kettle cover, obtain silicone sealant.
In above-described embodiment, when reinforced in kneader, should notice that kneader table shows load value, when 80%≤load≤90%, can continue to feed in raw material; When load displayed value often jumps out 5 times, when wherein to have 3 times or more display >=100%, rotating speed should be adjusted to 35 ~ 40r/min by 50r/min; As the equal < 100% of 5 displayed values, rotating speed recalls to 50r/min.
The thermostable silicone sealant prepared by above-described embodiment carries out performance test, by the standard testing surface drying time of GB/T13477.5-2002; By the standard testing sag of GB/T13477.6-2002; By the standard testing elastic restoration ratio of GB/T13477.17-2002; By the standard testing tensile modulus of GB/T13477.8-2002; By the cohesiveness after the standard testing hot pressing-cold drawn of GB/T13477.13-2002; Surely cohesiveness is stretched by after the standard testing warm air-water cycle of GB/T13477.10-2002; By cohesiveness after the standard testing ultraviolet irradiation-water logging of JC/T486-20015.14; By the standard testing contaminative of GB/T13477.20-2002.Table 1 is the performance data of silicone sealant prepared by embodiment 1 ~ embodiment 4.
The performance data of silicone sealant prepared by table 1 embodiment
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.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 improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (8)
1. a thermostable silicone sealant, comprising:
Described mineral oil is one or more in white oil 10#, white oil 15#, white oil 26#, white oil 46# and white oil 68#;
Described ceramic with heat resistance powder is zirconia-based ceramic powder, and the density of described ceramic with heat resistance powder is 1.85 ~ 2.5g/cm
3, particle diameter is 20 ~ 120 μm.
2. thermostable silicone sealant according to claim 1, it is characterized in that, described matrix resin is the α-ω polysiloxanediol with formula I structure, and the viscosity of described α-ω polysiloxanediol is 20000mPas ~ 80000mPas;
Wherein, R is CH
3-or CH
3cH
2-; N is 50 ~ 5000.
3. thermostable silicone sealant according to claim 1, is characterized in that, described strengthening agent is one or more in titanium dioxide, coarse whiting, active nano-calcium carbonate and light calcium carbonate.
4. thermostable silicone sealant according to claim 1, it is characterized in that, described silane coupling agent is one or more in vinyl three ('beta '-methoxy oxyethyl group) silane, vinyltriethoxysilane, γ-mercaptopropyl trimethoxysilane, APTES and γ-glycidyl ether oxygen propyl trimethoxy silicane.
5. thermostable silicone sealant according to claim 1, is characterized in that, described catalyzer is one or more in di-n-butyl tin acetate in February, dibutyl tin dilaurate and isopropyl titanate.
6. thermostable silicone sealant according to claim 1, is characterized in that, described linking agent is one or more in methyl tributanoximo silane, vinyl tributyl ketoximyl silane and methyl triacetoxysilane.
7. thermostable silicone sealant according to claim 1, is characterized in that, described mill base is the mill base obtained after carbon black mixes with α-ω polysiloxanediol or polydimethylsiloxane; With the weight percent meter of mill base, described carbon black is 30 ~ 100 weight parts, and the viscosity of described α-ω polysiloxanediol is 2000mPas ~ 4000mPas, and the viscosity of described polydimethylsiloxane is 200mPas ~ 500mPas.
8. a preparation method for thermostable silicone sealant according to claim 1, comprising:
The strengthening agent of the matrix resin of 20 ~ 70 weight parts with 30 ~ 90 weight parts is mixed, obtains basic glue;
The ceramic with heat resistance powder of the linking agent of the catalyzer of the mill base of silane coupled, 1 ~ 20 weight part of 0.1 ~ 20 weight part, 0.001 ~ 10 weight part, 0.1 ~ 10 weight part, 0.1 ~ 20 weight part mineral oil, 5 ~ 15 weight parts is mixed with described basic glue, after reaction, obtains thermostable silicone sealant.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310002398.8A CN103911113B (en) | 2013-01-05 | 2013-01-05 | Thermostable silicone sealant and preparation method thereof |
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|---|---|---|---|
| CN201310002398.8A CN103911113B (en) | 2013-01-05 | 2013-01-05 | Thermostable silicone sealant and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
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| CN103911113A CN103911113A (en) | 2014-07-09 |
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| CN109251720A (en) * | 2018-07-13 | 2019-01-22 | 中国航发北京航空材料研究院 | High-temperature resistant one-component depickling type room temperature vulcanized organosilicon sealant and preparation method thereof |
| CN109971181A (en) * | 2019-04-24 | 2019-07-05 | 深圳市华创威实业有限公司 | PET insulating sleeve glue |
| CN112300751A (en) * | 2020-11-24 | 2021-02-02 | 佛山市高建硅胶实业有限公司 | Silicone sealant and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2004045847A1 (en) * | 2002-11-21 | 2004-06-03 | Chengdu New West-Point Science And Technology Co., Ltd. | A new fire retarding board and manufacturing method thereof |
| CN101353563A (en) * | 2008-09-11 | 2009-01-28 | 成都硅宝科技股份有限公司 | Single-component silicone fluid sealant for solar energy cell assembly and manufacturing method thereof |
| CN101985550A (en) * | 2010-11-05 | 2011-03-16 | 江苏天源华威电气集团公司 | One-component room temperature vulcanizing silicone fireproof sealant and preparation method thereof |
| CN102093837A (en) * | 2010-09-14 | 2011-06-15 | 抚顺哥俩好化学有限公司 | One-component high temperature-resistant gasket-free sealant and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004045847A1 (en) * | 2002-11-21 | 2004-06-03 | Chengdu New West-Point Science And Technology Co., Ltd. | A new fire retarding board and manufacturing method thereof |
| CN101353563A (en) * | 2008-09-11 | 2009-01-28 | 成都硅宝科技股份有限公司 | Single-component silicone fluid sealant for solar energy cell assembly and manufacturing method thereof |
| CN102093837A (en) * | 2010-09-14 | 2011-06-15 | 抚顺哥俩好化学有限公司 | One-component high temperature-resistant gasket-free sealant and preparation method thereof |
| CN101985550A (en) * | 2010-11-05 | 2011-03-16 | 江苏天源华威电气集团公司 | One-component room temperature vulcanizing silicone fireproof sealant and preparation method thereof |
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