CN101942201A - Room-temperature vulcanized antiflaming single-component dealcoholization-type silicone rubber sealant and preparation method thereof - Google Patents
Room-temperature vulcanized antiflaming single-component dealcoholization-type silicone rubber sealant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a room-temperature vulcanized antiflaming single-component dealcoholization-type silicone rubber sealant and a preparation method thereof. The room-temperature vulcanized antiflaming single-component dealcoholization-type silicone rubber sealant comprises 40-60 parts of alpha, omega-divinyl polydimethylsiloxane (A), 5-15 parts of polydimethylsiloxane (B) the end group of which is hydrogen group, 1-5 parts of vinyltrimethoxysilane (C), 1-5 parts of platinum catalyst (D), 1-10 parts of gas phase method white carbon black (E), 15-30 parts of inorganic fire retardant (F), 5-10 parts of crosslinker (G), 2-8 parts of titanate catalyst (H), 1-5 parts of silane coupling agent (I) and 1-3 parts of hydroxyl and moisture scavenger (J). The preparation method comprises: evenly mixing components (A), (B) and (C) under the protection of N2; adding (D), reacting for 4 hours to finish blocking under the protection of N2; when the vacuum degree is more than -0.09, removing bubble for 10-30 minutes; successively adding components (F), (J) and (E); evenly mixing when the vacuum degree is more than -0.09; adding components (G), (H) and (I); and reacting for 30-60 minutes when the vacuum degree is more than -0.09.
Description
Technical field
The present invention relates to a kind of silicone rubber sealant and preparation method, relate in particular to fire-retardant single-component de-alcoholized silicone rubber sealant of a kind of self cure and preparation method.
Background technology
At present, be that the flat panel display development of principal market is swift and violent with Japan, Korea S, Taiwan and China, TFT-LCD will capture audiovisual market fast, and the driving transformer that is complementary with liquid-crystal display begins to produce in China.Because the output terminal of the driving transformer that is complementary with liquid-crystal display is high frequency, high pressure, therefore need encapsulate with silica gel, increase creepage distance, prevent to puncture, play insulation and dampproof effect.
Main what adopt is that the single-component de-alcoholized silica gel of self cure seals to liquid-crystal display with the sealing of the output terminal of driving transformer, the type silica gel at room temperature absorbs airborne moisture afterreaction sulfuration, the methyl alcohol that sulfuration is emitted does not have corrosion to the fine copper wire of transformer, and the type silica gel requires to have good fire retardant performance simultaneously.Single-component de-alcoholized silica gel is normally with α, and alpha, omega-dihydroxy polydimethyl siloxane is a base-material, and it is linking agent that methyltrimethoxy silane etc. contain Polymethoxylated silane coupling agent, and organic titanate and inner complex thereof are that catalyzer and filler are formulated.In the process of preparation seal gum, the affiliation that adds of titanate ester catalyzer makes sizing material that the process of a thickening be arranged, and this brings certain trouble to production, and simultaneously, micro-moisture in the sizing material and free hydroxyl influence the package stability of seal gum.The flame retardant properties general method of seal gum is to add halogen flame retardant and inorganic combustion inhibitor realization.Because the requirement of electron trade Halogen and the obnoxious flavour that the halogen flame retardant discharges in fire-retardant process make the halogen flame retardant be restricted in the application of electron trade; And needing to add very big quantity in seal gum, inorganic combustion inhibitor could arrive the good flame effect, the heavy addition inorganic combustion inhibitor can make the hardness of seal gum higher, mechanical properties decrease, simultaneously, some inorganic combustion inhibitor of heavy addition, as the inorganic hydrogen aluminum oxide, can have a strong impact on the electrical property of seal gum.
Summary of the invention
In order to solve the deficiencies in the prior art, the invention provides a kind of employing α, fire-retardant single-component de-alcoholized silicone rubber sealant of the self cure of ω-divinyl polydimethylsiloxane end blocking method and preparation method.
In order to realize above-mentioned technical purpose, technical characterictic of the present invention is: this silicone rubber sealant comprises following (A)-(J) component, and each component is as follows by weight:
(A) α, ω-divinyl polydimethylsiloxane 40-60 part
(B) end group is polydimethylsiloxane 5-15 part of hydrogen base
(C) vinyltrimethoxy silane 1-5 part
(D) platinum catalyst 1-5 part
(E) thermal silica 1-10 part
(F) inorganic combustion inhibitor aluminium hydroxide 15-30 part
(G) linking agent 5-10 part
(H) titanate catalyst 2-8 part
(I) silane coupling agent 1-5 part
(J) hydroxyl and moisture scavenger 1-3 part
(A) component of the above is α, ω-divinyl polydimethylsiloxane, and its molecular structural formula is CH
2=CH-Si (CH3)
2O[(CH3)
2SiO]
n(CH3)
2Si-CH=CH
2, n=300～1400.
Above-mentioned (B) component is that end group is the polydimethylsiloxane of hydrogen base, and its molecular structural formula is H-Si (CH3)
2O[(CH3)
2SiO]
m(CH3)
2Si-H, m=10～50.
Above-mentioned (D) component platinum catalyst is a kind of in the diethyl phthalate solution of the tetrahydrofuran solution of aqueous isopropanol, Platinic chloride of vinylsiloxane inner complex, the Platinic chloride of Platinic chloride or Platinic chloride.
A kind of in above-mentioned (G) component linking agent methyltrimethoxy silane and the vinyltrimethoxy silane.
Above-mentioned (H) component titanate catalyst is selected one or more mixing in tetrabutyl titanate ester, four isobutyl-titanic acid ester, tetra isopropyl titanate, four (the trimethyl silicane alcoxyl base) titanium for use.
Above-mentioned (I) component silane coupling agent is selected one or more mixing in 3-aminopropyltriethoxywerene werene, N-methyl-3-aminopropyl trimethoxysilane and the diethylenetriamine base propyl trimethoxy silicane for use.
Above-mentioned (J) component hydroxyl and moisture scavenger are selected a kind of in molecular sieve, zeolite, calcium chloride and the magnesium chloride for use.
The preparation method of the fire-retardant single-component de-alcoholized silicone rubber sealant of above-mentioned self cure includes following steps and forms:
The first step with said components (A), (B), (C) at N
2After mixing under the protection, at N
2Add (D) under protection and the condition of stirring and carry out end capping, N
2Protection is after down reaction was finished end capping after 4 hours, vacuum tightness greater than-0.09 condition under de-bubbled 10-30 minute;
Second step added (F) component, (J) component and (E) component successively in above-mentioned end-blocking resin, after vacuum tightness mixes under greater than-0.09 condition, add (G) (H) (I) component react under in vacuum tightness and can make fire-retardant single-component de-alcoholized silicone rubber sealant in 30-60 minute greater than-0.09 condition.
The invention has the beneficial effects as follows that the present invention adopts α, the end capped method of ω-divinyl polydimethylsiloxane, concrete end blocking method is under the effect of platinum catalyst, hydrogen base in the end hydrogen base polydimethylsiloxane and α, vinyl generation addition reaction in ω-divinyl polydimethylsiloxane, and another hydrogen base in the end hydrogen base polydimethylsiloxane and the vinyl generation addition reaction in the vinyltrimethoxy silane can to prepare end group be three end capped polydimethylsiloxanes of methoxyl group, simultaneously, catalysis end capping platinum catalyst can cooperate the effect of playing cooperative flame retardant with the inorganic combustion inhibitor aluminium hydroxide that adds in the subsequent preparation technology, can reduce the addition of inorganic combustion inhibitor aluminium hydroxide so greatly.Platinum catalyst mainly plays the catalysis end capping and cooperates the dual function of cooperative flame retardant with inorganic combustion inhibitor aluminium hydroxide among the present invention.
Embodiment
Below in conjunction with specific embodiment the present invention is made and to further specify:
Embodiment 1
Silicon rubber sealant of the present invention comprises (A)-(J) component, and each constituent mass umber is as follows:
(A) α, 50 parts of ω-divinyl polydimethylsiloxane
(B) end group is 7.5 parts of the polydimethylsiloxanes of hydrogen base
(C) vinyltrimethoxy silane is 1.5 parts
(D) platinum catalyst is 2 parts
(E) thermal silica is 4 parts
(F) inorganic combustion inhibitor aluminium hydroxide is 20 parts
(G) linking agent is 6 parts
(H) titanate catalyst is 4 parts
(I) silane coupling agent is 3 parts
(J) hydroxyl and moisture scavenger are 2 parts
The α that 25 ℃ of following viscositys of wherein said (A) component are 10000cps, ω-divinyl polydimethylsiloxane; Described (B) component is that molecular weight is 1000 end hydrogen base silicone oil; Described (C) component is a vinyltrimethoxy silane; (D) component is a platinum catalyst; (E) component is a thermal silica; (F) component is an inorganic combustion inhibitor aluminium hydroxide; (G) component is a methyltrimethoxy silane; (H) component is a tetra isopropyl titanate; (I) component is a diethylenetriamine base propyl trimethoxy silicane; (J) component is pulverous molecular sieve.The α that concrete grammar and step are is 10000cps with 25 ℃ of following viscositys; ω-divinyl polydimethylsiloxane 50; molecular weight is 7.5 parts of 1000 end hydrogen base silicone oil; 1.5 parts of vinyltrimethoxy silanes; stirred 10-30 minute under nitrogen protection, reaction is 4 hours under 2 parts of post-heating to 80 of adding platinum catalyst ℃ following nitrogen protection under nitrogen protection and the condition of stirring.After finishing, end capping adds 4 parts of 20 parts in inorganic combustion inhibitor aluminium hydroxide, 2 parts in pulverous molecular sieve and thermal silicas under greater than 0.085 condition after de-bubbled 10-30 minute in vacuum tightness; adding 6 parts of methyltrimethoxy silanes after vacuum tightness is mixed 30-60 minute under greater than 0.085 condition, the reaction under nitrogen protection of 3 parts of 4 parts of tetra isopropyl titanates and diethylenetriamine base propyl trimethoxy silicanes is stirred after 90 minutes and can be made the fire-retardant single-component de-alcoholized silicone rubber sealant of self cure.
With the fire-retardant single-component de-alcoholized silicone rubber sealant of the self cure for preparing among the embodiment, utilize mould about the about 2mm of thickness to prepare the print of the about 2mm of thickness, under (23 ± 2) ℃, (50 ± 5) % humidity condition, solidified 14 days, be cut into dumbbell shape with special-purpose cut-off knife, press the GB/T531 tested for hardness, press GB/T528 test tensile strength and elongation at break; Utilize the mould of the about 1mm of thickness to prepare the print of the about 1mm of thickness, under (23 ± 2) ℃, (50 ± 5) % humidity condition, solidified 14 days, be cut into the circular print that diameter is 100mm, press GB/T1692 test volume resistivity with special-purpose cut-off knife; Utilize the mould of the about 3mm of thickness to prepare the print of the about 3mm of thickness, under (23 ± 2) ℃, (50 ± 5) % humidity condition, solidified 14 days, be cut into the print of 125mm * 13.0mm, press GB/T 13488-1992 mensuration vertical combustion performance with special-purpose cut-off knife.
Table 1
Claims (9)
1. fire-retardant single-component de-alcoholized silicone rubber sealant of self cure, this silicone rubber sealant comprises following (A)-(J) component, each component is as follows by weight:
(A) α, ω-divinyl polydimethylsiloxane 40-60 part
(B) end group is polydimethylsiloxane 5-15 part of hydrogen base
(C) vinyltrimethoxy silane 1-5 part
(D) platinum catalyst 1-5 part
(E) thermal silica 1-10 part
(F) inorganic combustion inhibitor aluminium hydroxide 15-30 part
(G) linking agent 5-10 part
(H) titanate catalyst 2-8 part
(I) silane coupling agent 1-5 part
(J) hydroxyl and moisture scavenger 1-3 part.
2. according to the fire-retardant single-component de-alcoholized silicone rubber sealant of the self cure of claim 1, it is characterized in that: described (A) component is α, ω-divinyl polydimethylsiloxane, and its molecular structural formula is CH
2=CH-Si (CH3)
2O[(CH3)
2SiO]
n(CH3)
2Si-CH=CH
2, n=300～1400.
3. according to the fire-retardant single-component de-alcoholized silicone rubber sealant of the self cure of claim 1, it is characterized in that: described (B) component is that end group is the polydimethylsiloxane of hydrogen base, and its molecular structural formula is H-Si (CH3)
2O[(CH3)
2SiO] m (CH3)
2Si-H, m=10～50.
4. according to the fire-retardant single-component de-alcoholized silicone rubber sealant of the self cure of claim 1, it is characterized in that: described (D) component platinum catalyst is a kind of in the diethyl phthalate solution of the tetrahydrofuran solution of aqueous isopropanol, Platinic chloride of vinylsiloxane inner complex, the Platinic chloride of Platinic chloride or Platinic chloride.
5. according to the fire-retardant single-component de-alcoholized silicone rubber sealant of the self cure of claim 1, it is characterized in that: a kind of in described (G) component linking agent methyltrimethoxy silane and the vinyltrimethoxy silane.
6. according to the fire-retardant single-component de-alcoholized silicone rubber sealant of the self cure of claim 1, it is characterized in that: described (H) component titanate catalyst, select one or more mixing in tetrabutyl titanate ester, four isobutyl-titanic acid ester, tetra isopropyl titanate, four (the trimethyl silicane alcoxyl base) titanium for use.
7. according to the fire-retardant single-component de-alcoholized silicone rubber sealant of the self cure of claim 1, it is characterized in that: described (I) component silane coupling agent, select one or more mixing in 3-aminopropyltriethoxywerene werene, N-methyl-3-aminopropyl trimethoxysilane and the diethylenetriamine base propyl trimethoxy silicane for use.
8. according to the fire-retardant single-component de-alcoholized silicone rubber sealant of the self cure of claim 1, it is characterized in that: described (J) component hydroxyl and moisture scavenger, select a kind of in molecular sieve, zeolite, calcium chloride and the magnesium chloride for use.
9. the preparation method who prepares the fire-retardant single-component de-alcoholized silicone rubber sealant of the described self cure of claim 1 is characterized in that this method includes following steps and forms:
The first step with said components (A), (B), (C) at N
2After mixing under the protection, at N
2Add (D) under protection and the condition of stirring and carry out end capping, N
2Protection is after down reaction was finished end capping after 4 hours, vacuum tightness greater than-0.09 condition under de-bubbled 10-30 minute;
Second step added (F) component, (J) component and (E) component successively in above-mentioned end-blocking resin, after vacuum tightness mixes under greater than-0.09 condition, add (G) (H) (I) component react under in vacuum tightness and can make fire-retardant single-component de-alcoholized silicone rubber sealant in 30-60 minute greater than-0.09 condition.
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|---|---|---|---|
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|---|---|---|---|
| CN2010102656939A CN101942201B (en) | 2010-08-30 | 2010-08-30 | Room-temperature vulcanized antiflaming single-component dealcoholization-type silicone rubber sealant and preparation method thereof |
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| CN101942201B CN101942201B (en) | 2012-05-23 |
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| CN102408719A (en) * | 2011-07-20 | 2012-04-11 | 深圳市宝力科技有限公司 | Room temperature-vulcanized single-component transparent methanol-removing type silicone rubber sealant and preparation method thereof |
| CN102559131A (en) * | 2011-11-25 | 2012-07-11 | 烟台德邦科技有限公司 | Silicon sulfide rubber and preparation method thereof |
| CN102757758A (en) * | 2012-07-09 | 2012-10-31 | 苏州斯迪克新材料科技股份有限公司 | Preparation method of micropore organic silicone adhesive |
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| CN102408719A (en) * | 2011-07-20 | 2012-04-11 | 深圳市宝力科技有限公司 | Room temperature-vulcanized single-component transparent methanol-removing type silicone rubber sealant and preparation method thereof |
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