CN105086925B - A kind of environmental protection flame retardant silicone sealant and preparation method thereof - Google Patents
A kind of environmental protection flame retardant silicone sealant and preparation method thereof Download PDFInfo
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- CN105086925B CN105086925B CN201510524661.9A CN201510524661A CN105086925B CN 105086925 B CN105086925 B CN 105086925B CN 201510524661 A CN201510524661 A CN 201510524661A CN 105086925 B CN105086925 B CN 105086925B
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Abstract
The invention discloses a kind of novel environment friendly flame-proof silicone sealant and preparation method thereof, include the component of following parts by weight：100 parts of α, ω polysiloxanediol, 1 ~ 50 part of dimethyl silicone polymer, 5 ~ 150 parts of filler, 1 ~ 10 part of phosphorus silicon fire retardant, 1 ~ 15 part of crosslinking agent, 0.1 ~ 3 part of catalyst, 0.5 ~ 4 part of coupling agent.The dealcoholized type flame-proof silicone sealant that the present invention is prepared using the method for addition novel environment friendly fire retardant, solves the problems, such as that dealcoholized type fluid sealant product flame retardant property is poor, and gas preparation process is succinct, and is lost low in production process, and product processing performance is good.
Description
Technical field
The present invention relates to a kind of flame-proof silicone sealants and preparation method thereof, belong to high molecule sealing materials field.
Background technology
Silicone sealant have the characteristics that excellent heatproof, it is weather-proof, anti-aging, be not cracked, antidetonation and moisture-proof, building,
Electronic apparatus, automobile, field of aerospace are widely used.With the enhancing that people's security against fire is realized, fluid sealant is prevented
Fiery rank requirement is higher and higher.Although common silicone sealant has certain flame retardant property, its flame retardant property cannot still reach
Industry requirement.By adding in fire retardant into silicone sealant to improve product flame retardant property, become a kind of feasible effective side
Method.
Additive flame retardant such as aluminium hydroxide, magnesium hydroxide, they are nontoxic, smokeless, cheap, but aluminium hydroxide, hydrogen
The grain size of magnesium oxide powder is affected to the anti-flammability and fillibility of silicone sealant, exist mixing it is uneven or reunite so that
It is poor that power is combined between polymer, the problems such as superpolymer performance is caused to decline.
Halogen flame has good flame retardant effect in fluid sealant, but not only releases substantial amounts of smog during burning,
Noxious material can be also discharged, harmful effect is generated to environment.
Phosphorus flame retardant and polysiloxanes compatibility are bad, the problems such as layering can be generated in addition fluid sealant, is permeated, influence
It stores and uses.Therefore, phosphorus flame retardant uses less in fluid sealant.
Silicon-series five-retardant silicon systems row fire retardant domestic production kind and output all very littles, use more silicone polymer
It is a kind of transparent, sticky polysiloxane polymer.As the silicone polymer of fire retardant, usually with one or more synergists
It is used in combination.Since silicon-series five-retardant is mostly smokelessly few malicious, combustion heat value is low, and flame propagation velocity is slow, therefore is concerned by people,
Its development potentiality and application prospect are very considerable.
The content of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies of the above problem, provide a kind of flame retardant sealant and its preparation
The improved technology of method.
The technical solution of the present invention
A kind of novel environment friendly flame-proof silicone sealant, by weight, including following component：
Further preferably include following component：
The phosphorus silicon fire retardant is phosphorus active in miscellaneous phenanthrene -10- oxides (DOPO) derivative of 9,10- dihydro-9-oxies
The fire retardant that the siloxanes of hydrogen bond and the carbon-carbon double bond containing there are two occurs addition reaction and generates, the structural formula of the fire retardant is such as
Under：
Wherein, R1, R2, R3, R4, alkyl that C1-C5 is selected from, the alkoxy of C1-C5, aryl, aryloxy group；R5With R6For C0-
The alkylidene of C5；R7-R14Selected from hydrogen atom, the alkyl of C1-C5, nitro, the alkoxy of C1-C5, aryl, aryloxy group；N is 1-
10。
The α, alpha, omega-dihydroxy polysiloxanes viscosity at 25 DEG C is 16000~80000mPa/s.
Dimethyl silicone polymer viscosity at 25 DEG C is 50~1000mPa/s.
The filler at least one of for gas-phase silica, nano-calcium carbonate, silicon powder, quartz and diatomite,
Preferably nano-calcium carbonate and gas-phase silica, and, the weight ratio of nano-calcium carbonate and gas-phase silica is 15：1.
The crosslinking agent is ethyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane and vinyl three
At least one of Ethoxysilane is preferably methyltriethoxysilane.
The catalyst for dibutyl tin laurate, dibutyltin diacetate, butyl titanate, at least one of,
Preferably dibutyltin diacetate.
The coupling agent is gamma-aminopropyl-triethoxy-silane, γ-(the third oxygen of 2,3- epoxies) propyl trimethoxy silicon
Alkane, γ-(methacryloxypropyl) propyl trimethoxy silicon, N- (β-aminoethyl)-gamma-aminopropyl-triethoxy silicon and it is double (γ-
At least one of trimethoxy-silylpropyl) amine, it is preferably double (γ-trimethoxy-silylpropyl) amine.
The preparation method of the novel environment friendly flame-proof silicone sealant, comprises the following steps：
By α, 100 parts of alpha, omega-dihydroxy polysiloxanes, 1~50 part of dimethyl silicone polymer, 5~150 parts of filler, Novel ring
1~10 part of environment friendly flame-retardant agent, 1~15 part of crosslinking agent, 0.1~3 part of catalyst, 0.5~4 part of coupling agent are added in planetary mixer,
- 0.1~-0.09, rotating speed discharges vacuum degree after stirring 2~6h under conditions of being 12~50rmp, you can obtains silicone seal
Glue.
The beneficial effects of the invention are as follows：For the present invention using α, alpha, omega-dihydroxy polysiloxanes is basic polymer, passes through addition
The auxiliary agents such as fire retardant prepare Dealcoholization type silicone sealant.When fluid sealant is prepared, first novel environment friendly fire retardant is mixed with 107 glue
Base-material uniformly is made, then adds in the auxiliary agents such as dimethyl silicone polymer, filler, crosslinking agent, catalyst and is configured to fluid sealant, it is made
Standby fluid sealant has the type of resistance to combustion and self-extinguishing type in use, and flame retardant rating can reach V0 grades, has low toxicity, without dirt
The advantages of dye, cementability good stable storing.
Specific embodiment
The present invention is described further with reference to specific embodiment.
Embodiment 1
Respectively by each component described in following table 1 by α, alpha, omega-dihydroxy polysiloxanes, dimethyl silicone polymer, gas phase
White carbon, two [(the own ring -6- ketone of 6- oxygen -6- hydrogen-dibenzo-(c, e) (1,2)-oxygen phospha)-ethyl]-siloxanes add in planet
In mixer, for vacuum degree -0.1~-0.09, rotating speed stirs 2-6h under conditions of being 12~50rmp, after mixing by KH550, just
Silester, di lauric dibutyl rubber tin are added thereto, discharge after 10~20min, you can obtain silicone sealant.Then survey
Various performances are tried, product test the results are shown in Table 2.
Embodiment 2
The method that embodiment 1 is repeated by each component content described in following table 1, but fire retardant with two [(6- oxygen -6- hydrogen -
Own ring -6- the ketone of dibenzo-(c, e) (1,2)-oxygen phospha)-propyl]-siloxanes two [(6- oxygen -6- hydrogen-dibenzo-(c, e) of replacement
Own ring -6- the ketone of (1,2)-oxygen phospha)-ethyl]-siloxanes, filler surface substitutes gas through stearic acid modified nano-calcium carbonate
Phase white carbon, crosslinking agent substitute ethyl orthosilicate with methyltrimethoxysilane, and coupling agent substitutes KH550, catalyst with KH560
Di lauric dibutyl rubber tin is substituted with butyl titanate.Product test the results are shown in Table 2.
Embodiment 3
By described in following table 1 each component content repeat embodiment 1 method, but filler active nano-calcium carbonate and
(wherein the weight ratio of active nano-calcium carbonate and gas-phase silica is 15 to gas-phase silica:1) compounding use, which substitutes, is used alone
Gas-phase silica, crosslinking agent substitute ethyl orthosilicate with methyltriethoxysilane, and catalyst is substituted with dibutyltin diacetate
Di lauric dibutyl rubber tin, coupling agent substitute KH550 with KH170, and product test the results are shown in Table 2.
Embodiment 4
The method that embodiment 1 is repeated by each component content described in following table 1, but filler silicon powder and gas phase hard charcoal
It is black that (wherein the weight ratio of silicon powder and gas-phase silica is 1:1) compounding use, which substitutes, is used alone gas-phase silica, crosslinking agent
Ethyl orthosilicate is substituted with vinyltriethoxysilane, product test the results are shown in Table 2.
Embodiment 5
By described in following table 1 each component content repeat embodiment 1 method, but filler active nano-calcium carbonate and
(wherein the weight ratio of active nano-calcium carbonate and silicon powder is 6 to silicon powder:1) compounding use substitutes gas-phase silica, and product is surveyed
Test result is shown in Table 2.
Comparative example
The method that embodiment 1 is repeated by each component content described in following table 1, material therefor are consistent with case study on implementation 1.
Product test the results are shown in Table 2.
Claims (4)
1. a kind of environmental protection flame retardant silicone sealant, which is characterized in that its preparation method is：α, alpha, omega-dihydroxy polysiloxanes 100
Part, 5 parts of dimethyl silicone polymer, 15 parts of gas-phase silica, two [(6- oxygen -6- hydrogen-dibenzo -（c,e）（1,2）- oxygen phospha oneself
Ring -6- ketone)-ethyl] 2 parts of-siloxanes added in planetary mixers, vacuum degree in -0.1 ~ -0.09MPa, rotating speed for 12 ~
2-6h is stirred under conditions of 50rpm, by 1 part of KH550,6 parts of ethyl orthosilicate, 0.2 part of dibutyl tin laurate after mixing
It is added thereto, discharges after 10 ~ 20min, you can obtain silicone sealant, the α, alpha, omega-dihydroxy polysiloxanes is at 25 DEG C
Viscosity is 16000 ~ 80000mPa s, and dimethyl silicone polymer viscosity at 25 DEG C is 50 ~ 1000mPa s.
2. a kind of environmental protection flame retardant silicone sealant, which is characterized in that its preparation method is：
α, 100 parts of alpha, omega-dihydroxy polysiloxanes, 8 parts of dimethyl silicone polymer, surface are through stearic acid modified nano-calcium carbonate
100 parts, two [(6- oxygen -6- hydrogen-dibenzo -（c,e）（1,2）Own ring -6- the ketone of-oxygen phospha)-propyl] 4 parts of addition rows of-siloxanes
In star mixer, for vacuum degree in -0.1 ~ -0.09 MPa, rotating speed stirs 2-6h under conditions of being 12 ~ 50rpm, will after mixing
1.5 parts of KH560,12 parts of methyltrimethoxysilane, 1 part of butyl titanate are added thereto, discharge after 10 ~ 20min, you can obtain
Silicone sealant, the α, alpha, omega-dihydroxy polysiloxanes viscosity at 25 DEG C is 16000 ~ 80000mPa s, described
Dimethyl silicone polymer viscosity at 25 DEG C is 50 ~ 1000mPa s.
3. a kind of environmental protection flame retardant silicone sealant, which is characterized in that its preparation method is：
α, 100 parts of alpha, omega-dihydroxy polysiloxanes, 15 parts of dimethyl silicone polymer, active nano-calcium carbonate and gas-phase silica
Weight ratio is 15:1 80 parts of mixture, two [(6- oxygen -6- hydrogen-dibenzo -（c,e）（1,2）Own ring -6- the ketone of-oxygen phospha)-second
Base] 6 parts of-siloxanes added in planetary mixers, and vacuum degree is in -0.1 ~ -0.09MPa, under conditions of rotating speed is 12 ~ 50rpm
2-6h is stirred, is added thereto 1.5 parts of KH170,10 parts of methyltriethoxysilane, 1 part of dibutyltin diacetate after mixing,
It discharges after 10 ~ 20min, you can obtain silicone sealant, the α, alpha, omega-dihydroxy polysiloxanes viscosity at 25 DEG C is
16000 ~ 80000mPa s, dimethyl silicone polymer viscosity at 25 DEG C is 50 ~ 1000mPa s.
4. a kind of environmental protection flame retardant silicone sealant, which is characterized in that its preparation method is：
α, 100 parts of alpha, omega-dihydroxy polysiloxanes, 20 parts of dimethyl silicone polymer, the weight ratio of silicon powder and gas-phase silica are
1:1 20 parts of mixture, two [(6- oxygen -6- hydrogen-dibenzo -（c,e）（1,2）Own ring -6- the ketone of-oxygen phospha)-ethyl]-siloxanes
8 parts add in planetary mixer, and for vacuum degree in -0.1 ~ -0.09MPa, rotating speed stirs 2-6h under conditions of being 12 ~ 50rpm, mixes
By 2 parts of KH550,8 parts of vinyltriethoxysilane after even, 2 parts of dibutyl tin dilaurate is added thereto, after 10 ~ 20min
Discharging, you can obtain silicone sealant, the α, alpha, omega-dihydroxy polysiloxanes at 25 DEG C viscosity for 16000 ~
80000mPa s, dimethyl silicone polymer viscosity at 25 DEG C is 50 ~ 1000mPa s.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105440480A (en) * | 2015-12-10 | 2016-03-30 | 无锡普瑞腾传动机械有限公司 | Organic silicon sealant for automotive windscreen |
| CN107011661A (en) * | 2017-03-14 | 2017-08-04 | 清华大学 | Feedstock composition, quasi-iso static pressing soft mode and its manufacture method for manufacturing quasi-iso static pressing soft mode |
| CN108977166A (en) * | 2018-06-28 | 2018-12-11 | 芜湖市棠华建材科技有限公司 | A kind of silicone sealant and preparation method thereof |
| CN108795367A (en) * | 2018-06-28 | 2018-11-13 | 芜湖市棠华建材科技有限公司 | Neutral room temperature sealing silicone sulfide glue |
| CN109810670B (en) * | 2019-01-30 | 2022-02-01 | 江苏赛欧信越消泡剂有限公司 | Bi-component fireproof silicone sealant and preparation method thereof |
| CN115851219B (en) * | 2023-01-05 | 2023-11-07 | 山东元腾新材料科技有限公司 | Silicone flame-retardant sealant for building |
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