CN103911112A - Silicone sealant and its preparation method - Google Patents
Silicone sealant and its preparation method Download PDFInfo
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- CN103911112A CN103911112A CN201310002365.3A CN201310002365A CN103911112A CN 103911112 A CN103911112 A CN 103911112A CN 201310002365 A CN201310002365 A CN 201310002365A CN 103911112 A CN103911112 A CN 103911112A
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Abstract
The invention provides a silicone sealant, which comprises 20-70wt parts of matrix resin, 30-90wt parts of strengthening agent, 0.1-20 wt parts of silane coupling agent, 1-20wt parts of color paste, 0.001-10wt parts of catalyst, 0.1-10wt parts of cross-linking agent, 0.1-20wt parts of mineral oil and 1-10wt parts of mildew inhibitor. According to the invention, a mildew inhibitor with wide spectrum mildew resistance is introduced in the silicone sealant, an active function group in the cross-linking agent and matrix resin are subjected to crosslinking effect, so that the sealant is solidified, and the sealant has mildew resistance performance; additionally, the strengthening agent and the silane coupling agent are added for increasing the strength and cohesiveness of the silicone sealant.
Description
Technical field
The present invention relates to seal gum technical field, relate in particular to a kind of 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 being formed by materials such as water glass, organosilicon and silicone structure polymkeric substance.Silicone sealant has excellent weather, damp and hot, ultraviolet ray 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 to the improving constantly of the functional requirements such as building energy conservation, waterproof, heat insulation, sound insulation and comfortableness, 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, for example in production process, there will be viscosity peak too high; In use occur that rubber vulcanization speed is excessively slow; And seal gum is under damp and hot condition, it likely grows various moulds.In order to improve the adaptive faculty of seal gum under various envrionment conditionss, need to carry out mildew-resistant processing to seal gum, otherwise can cause biological degradation due to the erosion of mould and secretory product, cause the carbochain in seal gum molecular structure to rupture, physicals suffers damage, even produce larger harm, thereby affect production cost, threaten the quality of seal gum to bring loss to construction work.
Summary of the invention
The technical problem that the present invention solves be to provide a kind of mildew-resistant seal gum and preparation method thereof.
In view of this, the invention provides a kind of silicone sealant, comprising:
Preferably, described matrix resin is 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 mould inhibitor be the two phenoxazine arsenic of 10,10 ＇-oxo, methyl 2-benzimidazolecarbamate, p-nitrophenol, ethyl naphthol, sodium pentachlorophenate, dimethyl fumarate and 1,2-benzisothiazole-3-ketone one or more.
Preferably, described mill base is the mill base obtaining 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.
The present invention also provides a kind of preparation method of silicone sealant, comprising:
The matrix resin of 20 ~ 70 weight parts is mixed with the strengthening agent of 30 ~ 90 weight parts, obtain basic glue;
The mould inhibitor 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, 1 ~ 10 weight part is mixed with described basic glue, after reaction, obtain 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 mould inhibitor of 1 ~ 10 weight part.Under the effect of catalyzer, there is crosslinking reaction in matrix resin of the present invention and linking agent, has formed silicone elastomer, thereby obtained organic silicone sealing agent.Owing to having introduced the mould inhibitor with wide spectrum mildew resistance in silicone sealant, and active function groups and matrix resin generation crosslinked action in linking agent, make sealing glue solidifying, thereby make seal gum there is mildew resistance.Secondly,, by adding strengthening agent and silane coupling agent, be conducive to improve intensity and the cohesiveness of silicone sealant.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The embodiment of the invention discloses a kind of silicone sealant, comprising:
The invention provides a kind of stone material 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 mould inhibitor of 1 ~ 10 weight part.Matrix resin of the present invention and linking agent are under the effect of catalyzer, there is crosslinking reaction, form silicone elastomer, thereby complete the preparation of organic silicone sealing agent, owing to having introduced the mould inhibitor with mildew resistance in silicone sealant, and the active function groups in linking agent and matrix resin generation crosslinked action, make sealing glue solidifying, thereby make the seal gum of preparation there is mildew resistance.Secondly,, by adding strengthening agent and silane coupling agent, improved intensity and the cohesiveness of silicone sealant.
According to the present invention, described matrix resin is preferably α-ω polysiloxanediol with formula I structure, and the viscosity of described α-ω polysiloxanediol is preferably 20000mPas ~ 80000mPas, more preferably 35000mPas ~ 65000mPas; Described matrix resin is containing active function groups, can with linking agent generation crosslinking reaction.The character such as the molecular size range of matrix resin described in the present invention, molecular structure, molecular weight distribution, can affect the performance of the aspects such as the hardness, viscosity, levelling property, flow of sealing agent.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 has added the strengthening agent with strengthening action in silicone sealant, and kind, the modification situation etc. of described strengthening agent also can affect the character such as tensile strength, tear strength and the viscosity of seal gum.Described strengthening agent is preferably one or more in titanium dioxide, coarse whiting, active nano-calcium carbonate and light calcium carbonate.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 bond strength and weather resistance between resin and strengthening agent surface.Described silane coupling agent is preferably 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.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 obtaining 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 200mPas ~ 500mPas, and described 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, add catalyzer, described catalyst matrix resin reacts with linking agent, and the factors such as its addition and interpolation kind can affect set time, intensity and the application property etc. of linking agent.Described catalyzer is preferably one or more in di-n-butyl tin acetate in February, di-n-butyl two tin laurates and isopropyl titanate.Described catalyzer is 0.001 ~ 10 weight part, is preferably 1 ~ 8 weight part.
In described linking agent, contain active function groups, can with matrix resin generation crosslinking reaction, make sealing glue solidifying.Described linking agent is preferably one or more in methyl tributanoximo silane, vinyl tributyl ketoximyl silane and methyl triacetoxysilane.Described linking agent is 0.1 ~ 10 weight part, is preferably 2 ~ 8 weight parts.
The present invention has added 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, 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, in silicone sealant, also add mould inhibitor, described mould inhibitor mainly has mildew resistance, can effectively prevent growing of mould, thereby has avoided the infringement of seal gum physicals under moist and other severe environment.In addition, by the selection to mould inhibitor, make seal gum there is broad spectrum and there is outstanding character for the environment of some particular requirement.Described mould inhibitor be preferably the two phenoxazine arsenic of 10,10 ＇-oxo, methyl 2-benzimidazolecarbamate, p-nitrophenol, ethyl naphthol, sodium pentachlorophenate, dimethyl fumarate and 1,2-benzisothiazole-3-ketone one or more.Described mould inhibitor is 1 ~ 10 weight part, more preferably 2 ~ 8 weight parts.
The present invention also provides the preparation method of silicone sealant, comprising: the matrix resin of 20 ~ 70 weight parts is mixed with the strengthening agent of 30 ~ 90 weight parts, stir, obtain basic glue;
The mould inhibitor 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, 1 ~ 10 weight part is mixed with described basic glue, stir, obtain stone material silicone sealant.
According to the present invention, in the process of preparing silicone sealant, first carry out the preparation of basic glue, described basic glue is matrix resin and mixes obtained colloid with strengthening agent, in order to make the performance of silicone sealant more more excellent, as preferred version, the preparation method of described basic glue is specially:
1/2 ~ 2/3 base resin is placed in to 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 agents drop into, mediate to temperature of charge and rise to 110 ℃, rotating speed 50r/min.In the time that temperature rises to 110 ℃, vacuumize, mediate 0.5 ~ 4h, rotating speed 50r/min after being evacuated to-0.04～-0.1Mpa.Then unload vacuum, 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, vacuumize to mediate after 0.5 ~ 4h and unload vacuum ON cycle pump, the 10min that circulates while stirring, rotating speed 50r/min.In basic glue glue preparation process, if temperature rise to 130 ℃ reduces rotating speed to 35r/min, in the time that temperature does not reduce yet and reach 150 ℃, ON cycle water coolant rapidly, during lower than 120 ℃, closes recirculated cooling water, and rotating speed rises to 50r/min.
After prepared by basic glue, carry out the preparation of silicone sealant, described mill base, catalyzer, linking agent, silane coupling agent, mineral oil are mixed with mould inhibitor, after stirring, obtain silicone sealant, wherein mill base is as the main raw material of making seal gum, as preferred version, the preparation method of described mill base is specially:
The α that is 2000mPas ~ 4000mPas by viscosity, one or both kneading limit, limit pan feedings in alpha, omega-dihydroxy polysiloxane and 200mPas ~ 500mPas polydimethyl silica, rotating speed is 50r/min, progressively drops into whole carbon blacks, rotating speed is 50r/min.After whole carbon blacks drop 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 and mill base, be evacuated to-0.04～-more than 0.09MPa, starting vacuum stirring 10 ~ 60min, the rotating speed of stirrer is adjusted to 300r/min; When material is cooled to lower than 30 ~ 60 ℃ in still, in still, add linking agent, 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, in still, adds mould inhibitor, silane coupling agent and catalyzer, vacuumizes, and rotating speed is 300r/min, and churning time 10 ~ 30min stops stirring, and separates vacuum and rise kettle cover, 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 mould inhibitor of 1 ~ 10 weight part.Under the effect of catalyzer, there is crosslinking reaction in matrix resin of the present invention and linking agent, has formed silicone elastomer, thereby completed the preparation of organic silicone sealing agent.Owing to having introduced the mould inhibitor with wide spectrum mildew resistance in silicone sealant, and active function groups and matrix resin generation crosslinked action in linking agent, make sealing glue solidifying, thereby make seal gum there is mildew resistance.Secondly,, by adding strengthening agent and silane coupling agent, be conducive to improve intensity and the cohesiveness of silicone sealant.On the other hand, the present invention, in the process of preparing silicone sealant, by first preparing basic glue, then is mixed with seal gum by basic glue and other interpolation auxiliary agent, makes the mechanical property of seal gum obtain larger raising.
In order further to understand the present invention, below in conjunction with embodiment, silicone sealant provided by the invention and preparation method thereof is elaborated, protection scope of the present invention is not limited by the following examples.
Basic glue, strengthening agent, silane coupling agent, mill base, catalyzer, linking agent, mineral oil and mould inhibitor in the embodiment of the present invention all can obtain by outsourcing; The equipment such as described kneader and stirrer are conventional equipment.
Embodiment 1
The α of kneader suction 25 weight parts is opened in the preparation of basis glue, alpha, omega-dihydroxy polysiloxane, and kneading limit, limit pan feeding, 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, mediates temperature of charge to 110 ℃, and rotating speed is 50r/min, mediate temperature and vacuumize while rising to 110 ℃, mediate 4h after being evacuated to-0.04～-0.1Mpa; Then kneader is unloaded to 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, treat to close material sucking valve after the whole suction of base resin, open vacuum valve, be evacuated to-0.04～-0.1Mpa, after vacuumizing kneading 2h, unload vacuum ON cycle pump, the 10min that circulates while stirring, rotating speed is 50r/min, obtains basic glue.In the process of preparing at basic glue, if the temperature rise to 130 of kneader ℃ reduces rotating speed to 35r/min, when temperature does not reduce yet and reaches 150 ℃, ON cycle water coolant rapidly, during lower than 120 ℃, closes recirculated cooling water, and rotating speed rises to 50r/min.
The preparation of mill base is kneading limit, 200mPas polydimethyl silica limit pan feeding by the viscosity of 100 weight parts, and the rotating speed of kneader is 50r/min, progressively drops into the carbon black of 30 weight parts, and rotating speed is 50r/min, treats to mediate 2h after carbon black drops into, and obtains mill base.
The preparation of silicone sealant is to the basic glue, the white oil of 6 weight parts and the mill base of 12 weight parts that add above-mentioned preparation in stirrer still, be evacuated to-0.04～-more than 0.09MPa, starting vacuum stirring 30min, rotating speed is 300r/min; When in still, material is cooled to lower than 30 ℃, to the methyl tributanoximo silane that adds 9 weight parts in still, vacuumize, rotating speed is 300r/min, and churning time is 40min; Then stop stirring, emptying solution vacuum, rise kettle cover, in still, add the two phenoxazine arsenic of 10,10 ＇-oxo of 2 weight parts, the dimethyl fumarate of 2 weight parts, APTES, the γ-glycidyl ether oxygen propyl trimethoxy silicane of 0.5 weight part and the di-n-butyl tin acetate in February of 0.05 weight part of 1 weight part, vacuumize, rotating speed is 300r/min, and churning time is 20min, finally stops stirring, and separate vacuum and rise kettle cover, obtain silicone sealant.
Embodiment 2
The α of kneader machine suction 10 weight parts 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 ℃; The temperature of kneader vacuumizes while rising to 110 ℃, 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 to mediate after 2h and unload vacuum ON cycle pump, 10min while stirring circulates, rotating speed 50r/min, obtains basic glue.
The preparation of mill base is 300mPas α by the viscosity of 210 weight parts, 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, after whole carbon blacks drop into, mediates 5h, obtains mill base.
The preparation of silicone sealant is to the basic glue, the white oil of 4 weight parts and the mill base of 18 weight parts that add above-mentioned preparation in stirrer still, while being evacuated to-0.04～-0.09MPa, and vacuum stirring 30min, rotating speed is 300r/min; When material is cooled to lower than 50 ℃ in still, in still, add the vinyl tributyl ketoximyl silane of 2 weight parts and the methyl tributanoximo silane of 7 weight parts, vacuumize, rotating speed is 300r/min, after churning time 40min; Stop stirring, emptying solution vacuum, rise kettle cover, in still, add the Salicylanlide of 3 weight parts, the ethyl naphthol of 2 weight parts, vinyl three ('beta '-methoxy oxyethyl group) silane, the vinyltriethoxysilane of 4 weight parts and the dibutyl tin dilaurate of 0.05 weight part of 6 weight parts, vacuumize, rotating speed is 300r/min, churning time is 20min, stops stirring, and separates vacuum, rise kettle cover, obtain silicone sealant.
Embodiment 3
The α of kneader suction 40 weight parts 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 light calcium carbonate, the titanium dioxide of 20 weight parts and the water-ground limestone of 20 weight parts of 30 weight parts, rotating speed is 50r/min, mediates to temperature of charge and rises to 110 ℃; Temperature vacuumizes while rising to 110 ℃, mediates 4h, rotating speed 50r/min after being evacuated to-0.04～-0.1Mpa.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 to mediate after 2h and unload vacuum ON cycle pump, rotating speed is 50r/min, the 10min that circulates while stirring, obtains basic glue.
The viscosity of preparation 110 weight parts 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, after whole carbon blacks drop into, mediates 5h, obtains mill base.
The preparation of silicone sealant is to the basic glue, the white oil of 4 weight parts and the mill base of 15 weight parts that add above-mentioned preparation in stirrer still, be evacuated to-0.04～-more than 0.09MPa, starting vacuum stirring 30min, rotating speed is 300r/min; When material is cooled to lower than 60 ℃ in still, in still, add the vinyl tributyl ketoximyl silane of 1.5 weight parts and the methyl triacetoxysilane of 6 weight parts, vacuumize, rotating speed is 300r/min, and churning time is 40min; Stop stirring, emptying solution vacuum, rise kettle cover, to the γ-dredge propyl trimethoxy silicane, the APTES of 5 weight parts and the di-n-butyl tin acetate in February of 0.05 weight part of 2-Carbendazim, 3 weight parts of p-nitrophenol, 2 weight parts that adds 2 weight parts in still, 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 parts 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 20 weight parts, titanium dioxide, the water-ground limestone of 20 weight parts and the active nano-calcium carbonate of 20 weight parts of 30 weight parts, rotating speed is 50r/min, mediates to temperature of charge and rises to 110 ℃, and rotating speed is 50r/min; Temperature vacuumizes while rising to 110 ℃, 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 to mediate after 2h and unload vacuum ON cycle pump, 10min while stirring circulates, rotating speed is 50r/min, obtains basic glue.
The viscosity of preparation 140 weight parts 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, after whole carbon blacks drop into, mediates 5h, obtains mill base.
The preparation of silicone sealant is to the basic glue, the white oil of 4 weight parts and the mill base of 10 weight parts that add above-mentioned preparation in stirrer still, be evacuated to-0.04～-more than 0.09MPa, starting vacuum stirring 30min, rotating speed is 300r/min; When in still, material is cooled to lower than 30 ~ 60 ℃, to the methyl triacetoxysilane that adds 7 weight parts in still, vacuumize, rotating speed is 300r/min, and churning time is 40min; Then stop stirring, emptying solution vacuum, rises kettle cover, in still, adds 10 of 0.05 weight part, the γ of the ethyl naphthol of the two phenoxazine arsenic of 10 ＇-oxo, 3 weight parts, the sodium pentachlorophenate of 1 weight part, 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, and churning time is 20min, stop stirring, separate vacuum, rise kettle cover, obtain silicone sealant.
In above-described embodiment, when reinforced in kneader, should notice that kneader table show load value, when 80%≤load≤90% time, can continue to feed in raw material; Often jump out 5 times when load displayed value, wherein have 3 times or when above demonstration >=100%, rotating speed should be adjusted to 35 ~ 40r/min by 50r/min; In the time of 5 equal < 100% of displayed value, rotating speed is recalled to 50r/min.
Silicone sealant prepared by above-described embodiment carries out performance test, by the standard testing surface drying time of GB/T13477.5-2002; Press the standard testing sag of GB/T13477.6-2002; Press the standard testing elastic restoration ratio of GB/T13477.17-2002; Press the standard testing tensile modulus of GB/T13477.8-2002; Press the cohesiveness after the standard testing hot pressing of GB/T13477.13-2002-cold drawn; By surely stretching cohesiveness after standard testing warm air-water cycle of GB/T13477.10-2002; Press cohesiveness after standard testing ultraviolet irradiation-water logging of JC/T486-20015.14; Carry out the mensuration of mildew grade by HB8530.13-86.The performance data of the silicone sealant that table 1 is prepared for embodiment 1 ~ embodiment 4.
The performance data of silicone sealant prepared by table 1 embodiment
The explanation of above embodiment is just for helping to understand method of the present invention 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.
To the above-mentioned explanation of the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple modification of these embodiment, 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 silicone sealant, comprising:
2. silicone sealant according to claim 1, is characterized in that, described matrix resin is 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. 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. 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-thin propyl trimethoxy silicane, APTES and γ-glycidyl ether oxygen propyl trimethoxy silicane.
5. 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. 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. silicone sealant according to claim 1, it is characterized in that, described mould inhibitor be the two phenoxazine arsenic of 10,10 ＇-oxo, methyl 2-benzimidazolecarbamate, p-nitrophenol, ethyl naphthol, sodium pentachlorophenate, dimethyl fumarate and 1,2-benzisothiazole-3-ketone one or more.
8. according to the silicone sealant under claim 1, it is characterized in that, described mill base is the mill base obtaining 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.
9. silicone sealant according to claim 1, is characterized in that, described mineral oil is white oil.
10. a preparation method for silicone sealant, comprising:
The matrix resin of 20 ~ 70 weight parts is mixed with the strengthening agent of 30 ~ 90 weight parts, obtain basic glue;
The mould inhibitor 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, 1 ~ 10 weight part is mixed with described basic glue, after reaction, obtain silicone sealant.
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| CN (1) | CN103911112A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104232012A (en) * | 2014-10-14 | 2014-12-24 | 泸州北方化学工业有限公司 | Mold-proof silicone sealant and preparation method thereof |
| CN104479608A (en) * | 2014-12-30 | 2015-04-01 | 北京天山新材料技术有限公司 | Environment-friendly mildewproof silicone-modified polyether sealant |
| CN105001828A (en) * | 2015-06-27 | 2015-10-28 | 山东晨旭新材料股份有限公司 | Mildew-resistant flame-retardant potting adhesive and preparation method thereof |
| CN105925200A (en) * | 2016-05-06 | 2016-09-07 | 烟台图文马克化工科技有限公司 | Silicone sealant for automotive chassis |
| CN106189903A (en) * | 2016-07-21 | 2016-12-07 | 苏州泰仑电子材料有限公司 | The height with firmoviscosity glues protecting film |
| CN106189904A (en) * | 2016-07-21 | 2016-12-07 | 苏州泰仑电子材料有限公司 | Anti-acid acrylate pressure-sensitive adhesive protecting film |
| CN108314989A (en) * | 2018-02-26 | 2018-07-24 | 重庆建工第七建筑工程有限责任公司 | A kind of purification air-conditioning air hose fluid sealant and preparation method thereof |
| CN109207118A (en) * | 2018-07-27 | 2019-01-15 | 广东和天新材料科技有限公司 | Communication apparatus bonded adhesives production method and its product |
| CN115851204A (en) * | 2022-03-24 | 2023-03-28 | 安徽牛元新材料有限公司 | External mildew-proof adhesive for building construction and preparation method thereof |
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| WO2008109865A2 (en) * | 2007-03-07 | 2008-09-12 | Saint-Gobain Performance Plastics Corporation | Articles containing silicone compositions and methods of making such articles |
| CN102277127A (en) * | 2011-08-05 | 2011-12-14 | 曾庆铭 | Acidic silicone sealant |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008109865A2 (en) * | 2007-03-07 | 2008-09-12 | Saint-Gobain Performance Plastics Corporation | Articles containing silicone compositions and methods of making such articles |
| CN102277127A (en) * | 2011-08-05 | 2011-12-14 | 曾庆铭 | Acidic silicone sealant |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104232012A (en) * | 2014-10-14 | 2014-12-24 | 泸州北方化学工业有限公司 | Mold-proof silicone sealant and preparation method thereof |
| CN104479608A (en) * | 2014-12-30 | 2015-04-01 | 北京天山新材料技术有限公司 | Environment-friendly mildewproof silicone-modified polyether sealant |
| CN105001828A (en) * | 2015-06-27 | 2015-10-28 | 山东晨旭新材料股份有限公司 | Mildew-resistant flame-retardant potting adhesive and preparation method thereof |
| CN105925200A (en) * | 2016-05-06 | 2016-09-07 | 烟台图文马克化工科技有限公司 | Silicone sealant for automotive chassis |
| CN106189903A (en) * | 2016-07-21 | 2016-12-07 | 苏州泰仑电子材料有限公司 | The height with firmoviscosity glues protecting film |
| CN106189904A (en) * | 2016-07-21 | 2016-12-07 | 苏州泰仑电子材料有限公司 | Anti-acid acrylate pressure-sensitive adhesive protecting film |
| CN108314989A (en) * | 2018-02-26 | 2018-07-24 | 重庆建工第七建筑工程有限责任公司 | A kind of purification air-conditioning air hose fluid sealant and preparation method thereof |
| CN108314989B (en) * | 2018-02-26 | 2021-05-04 | 重庆建工第七建筑工程有限责任公司 | Sealant for purifying air-conditioning air duct and preparation method thereof |
| CN109207118A (en) * | 2018-07-27 | 2019-01-15 | 广东和天新材料科技有限公司 | Communication apparatus bonded adhesives production method and its product |
| CN115851204A (en) * | 2022-03-24 | 2023-03-28 | 安徽牛元新材料有限公司 | External mildew-proof adhesive for building construction and preparation method thereof |
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Application publication date: 20140709 |