CN1477172A - High-temp, resistant organic silicon adhesive and its preparation method - Google Patents
High-temp, resistant organic silicon adhesive and its preparation method Download PDFInfo
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- CN1477172A CN1477172A CNA031416063A CN03141606A CN1477172A CN 1477172 A CN1477172 A CN 1477172A CN A031416063 A CNA031416063 A CN A031416063A CN 03141606 A CN03141606 A CN 03141606A CN 1477172 A CN1477172 A CN 1477172A
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Abstract
The present invention relates to a high-temp. resistant organic silicon adhesive and its preparation method. It uses the water glass as raw material, and prepares the MQ resin and hydroxy terminated silicon rubber, then uses them as raw material and uses alkali as catalyst to prepare the invented high temp. resistant organic silicon adhesive, and its peeling strength at 180 deg.C can be up to above 20N/25cm, and it can be used for a long period below 200 deg.C, and can not be damaged.
Description
Technical field
The present invention relates to a kind of high temperature resistant silicone adhesive.The invention further relates to the preparation method of this high temperature resistant silicone adhesive.
Background technology
In today of rapid economic development, all require to use high-temperature-resistant adhesive in building, boats and ships, machinery, aerospace, the communications facility.
So-called high-temperature-resistant adhesive is meant the tackiness agent that can bear 200 ℃ of left and right sides temperature under the long term operation condition.Present most of high-temperature-resistant adhesive is to be that body material makes with silicone resin (MQ resin) and hydroxy-end capped silicon rubber.Be characterized in: (1) all has good adhesivity to high energy and low-energy surface material, especially some difficult sticking materials such as tetrafluoroethylene, polyimide, polycarbonate etc. is all had adhesive property preferably; (2) have outstanding high and low temperature resistance, can be between-73 ℃～296 ℃ life-time service, and under high temperature and low temperature, still keep its bonding strength and snappiness; (3) have good unreactiveness, long service life has outstanding wet fastness and electrical insulation capability simultaneously.
Early stage high-temperature-resistant adhesive is generally natural resins such as shellac, pitch, has developed vibrin afterwards, as thermosetting adhesives such as Synolac and unsaturated polyesters.But because the high thermal resistance of above-mentioned tackiness agent can satisfy requirement of actual application, substituted by epoxy resin binder again afterwards, because epoxy resin binder has better comprehensive performance, satisfies the service requirements of F class B insulation, therefore obtained certain application.The back charing easily but Resins, epoxy is heated for a long time, therefore after the 1980's, the high-temperature resistant organic silicon resin tackiness agent of low carbon content begins to be developed application.
The MQ silicone resin is a kind of organo-siloxane end-blocking chain link R by simple function group (M group)
3SiO
1/2And the organo-siloxane chain link SiO of four-functional group (Q group)
4/2The polysiloxane that the performance that hydrolytic condensation forms is special.Because of the difference of M/Q ratio, make the MQ resin have different molecular weight, present the state from the viscous fluid to the pulverulent solids, its physical properties comprises that density, transparency, viscosity, softening temperature, tackifying and amphipathic property etc. all can change thereupon.
The MQ resin is mainly used in to cooperate with silicon rubber makes silicone adhesive, has the effect of reinforcement and tackify.Along with the variation of MQ resin demand, can be made into the high temperature resistant pressure sensitive adhesive of each tool characteristic.
The MQ resin as the characteristics of the maximum of rubber tackifier is: raise with the embrittlement temperature that can not make rubber after the silicon rubber blend, thereby make the low temperature adhesivity of pressure sensitive adhesive fabulous.General pressure-sensitive adhesive just loses pressure-sensitive adhesivity when being lower than second-order transition temperature, and the pressure sensitive adhesive that is formed by MQ resin tackify silicon rubber also maintains good pressure-sensitive adhesivity when liquid nitrogen (196 ℃) temperature.
At present, producing the MQ resin both at home and abroad, mainly to adopt tetraethyl silicate be raw material, though product property is good, costs an arm and a leg, and limited its application to a certain extent.
Summary of the invention
The objective of the invention is to prepare the high temperature resistant silicone adhesive that a kind of price is low, performance is good.
High temperature resistant silicone adhesive of the present invention is to be reacted in the presence of alkaline catalysts by MQ resin and hydroxy-end capped silicon rubber to form, and it is as follows specifically to form proportioning:
Amounts of components is 100 weight parts in toluene
MQ resin 10～15
Hydroxy-end capped silicon rubber 10～15
Alkaline catalysts 0.0100～0.0125
Deionized water 2
Isopropylcarbinol 1.25
Toluene 100
Mineral alkali and organic basess such as alkaline catalysts such as NaOH, KOH, Tetramethylammonium hydroxide.
The present invention is performed such: at first prepare MQ resin and hydroxy-end capped silicon rubber, in the presence of catalyzer MQ resin and the reaction of hydroxy-end capped silicon rubber are made high temperature resistant silicone adhesive then.The preparation of one .MQ resin
MQ resin formula of the present invention is as follows:
Amounts of components (is 100 weight parts in toluene)
Water glass, solid content 10%, modulus 3.6 60～80
Hexamethyldisiloxane, MM 10～20
Ethanol 15～30
Hydrochloric acid, 36%～38% 30～40
Toluene 100
The following method of synthetic employing of MQ resin:
With MM and water glass 60～70 ℃ of cohydrolysis 1～1.5 hour in hydrochloric acid and ethanol, add toluene then, refluxed 2～4 hours down at 70～80 ℃.Isolate the upper strata organic layer after static, be washed with water to neutrality, add Calcium Chloride Powder Anhydrous and soak to eliminate moisture, toluene is removed in distillation at last, obtains pale yellow powder shape MQ resin two. the preparation of hydroxy-end capped silicon rubber
Hydroxy-end capped silicone rubber formulations of the present invention is as follows:
Amounts of components is (with D
4Be 100 weight part meters)
Octamethylcyclotetrasiloxane, D
4100
The vinyl cyclotetrasiloxane, D
4 v0.25～0.26
Hydroxy silicon oil, viscosity are 40～60mPas 0.08
Tetramethylammonium hydroxide silicon alkoxide 0.3～0.5
The synthetic method of hydroxy-end capped silicon rubber is as follows:
Above-mentioned raw materials is added in the reaction flask, vacuumized 0.5～1 hour under 50～60 ℃, logical then nitrogen is warming up to 80～90 ℃, reacts 1～3 hour.Be warming up to 110～120 ℃, continue reaction 1～3 hour.Be warming up to 150～180 ℃ and vacuumize about 0.5 hour and get final product again.The molecular weight of products therefrom is about 500,000.Three. the preparation of high temperature resistant silicone adhesive
High temperature resistant silicone adhesive prescription of the present invention is as follows:
Amounts of components (is 100 weight parts in toluene)
MQ resin 10～15
Hydroxy-end capped silicon rubber 10～15
Alkali 0.0100～0.0125
Deionized water 2
Isopropylcarbinol 1.25
Toluene 100
The synthetic method of high temperature resistant silicone adhesive is as follows:
Silicon rubber and toluene are added in the reaction flask, be warming up to 80～100 ℃ under stirring, silicon rubber is dissolved fully.Stop heating, be cooled to room temperature.Alkali is dissolved in deionized water and isopropylcarbinol, and adds in the above-mentioned silicone rubber solution, 100～115 ℃ of reflux 2～3 hours with the MQ resin.Vacuumize then to remove as far as possible and desolvate, promptly get desired product.
Among the present invention during the MQ resins cohydrolysis mode MM and ethanol can be added in the hydrochloric acid, 60～70 ℃ are stirred hydrolysis 20～30 minutes down, add water glass again and continue cohydrolysis 20～40 minutes.
Above-mentioned cohydrolysis mode also can be heated to hydrochloric acid 60～70 ℃, adds water glass, MM and ethanol then successively, cohydrolysis 20～40 minutes.
Tackiness agent solidifying agent of the present invention is a dibenzoyl peroxide, and consumption is advisable with 0.5～1.5% of tackiness agent total amount, and solidification value is suitable at 110～130 ℃.
Tackiness agent of the present invention is based on MQ resin and hydroxy-end capped silicon rubber, has that price is low, adhesive property good, resistant to elevated temperatures characteristics.It is raw material that the MQ resin adopts water glass and hexamethyldisiloxane, and its performance and prior art are basic identical with the product of tetraethyl silicate method preparation, but much cheap, and the preparation condition gentleness, and be simple to operate; The preparation method of hydroxy-end capped silicon rubber has above-mentioned advantage equally, makes product of the present invention possess good application and popularization value.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is further described.
Embodiment 1
The preparation prescription of MQ resin is consulted table 1.At first, press the proportioning weighing of MQ resin 1 in the table 1.Earlier ethanol and MM are added in the hydrochloric acid, 60 ℃ are stirred hydrolysis 30min down.Add water glass, continue cohydrolysis 30min.Add toluene, at 70 ℃ of following backflow 4h.Isolate the upper strata organic layer after static, be washed with water to neutrality.Add Calcium Chloride Powder Anhydrous and soak 3h to eliminate moisture, toluene is removed in distillation at last, obtains pale yellow powder shape MQ resin.
Embodiment 2
Press the formulation MQ resin 2 of table 1.At first, press the proportioning weighing of MQ resin 1 in the table 1.Hydrochloric acid is heated to 70 ℃, adds water glass, MM and ethanol successively, cohydrolysis 20min.Add toluene, at 80 ℃ of following backflow 2h.Isolate the upper strata organic layer after static, be washed with water to neutrality.Add Calcium Chloride Powder Anhydrous and soak 3h to eliminate moisture, toluene is removed in distillation at last, obtains pale yellow powder shape MQ resin.
Embodiment 3
The preparation prescription of hydroxy-end capped silicon rubber is consulted table 2.At first, press hydroxy-end capped silicon rubber 1 formulation of table 2.Raw material is added in the reaction flask, vacuumize 0.5h under 60 ℃, logical then nitrogen is warming up to 80 ℃, reaction 3h.Be warming up to 120 ℃, continue reaction 1h.Be warming up to 150 ℃ and vacuumize 0.5h.The molecular weight of products therefrom is 550,000.
Embodiment 4
Press the hydroxy-end capped silicon rubber 2 of formulation of table 2, raw material is added in the reaction flask, vacuumize 0.5h under 60 ℃, logical then nitrogen is warming up to 90 ℃, reaction 1h.Be warming up to 110 ℃, continue reaction 3h.Be warming up to 180 ℃ and vacuumize 0.5h again.The molecular weight of product be 450,000.
Embodiment 5
See also 3 high temperature resistant silicone adhesive prescriptions of the present invention that table 3 exemplifies.At first, press prescription 1 preparation in the table 3.Silicon rubber and toluene are added in the reaction flask, be warming up to 80 ℃ under stirring, silicon rubber is dissolved fully.Stop heating, be cooled to room temperature.NaOH is dissolved in deionized water and isopropylcarbinol, and adds in the above-mentioned silicone rubber solution, reflux 2h (controlled temperature is 110 ℃) with the MQ resin.Vacuumize then to remove as far as possible and desolvate, promptly get desired product.
Embodiment 6
Press and fill a prescription 2 in the table 3, be warming up to 95 ℃ under stirring, silicon rubber is dissolved fully in silicon rubber and the toluene adding reaction flask.Stop heating, be cooled to room temperature.KOH is dissolved in deionized water and isopropylcarbinol, and adds in the above-mentioned silicone rubber solution, reflux 3h (controlled temperature is 100 ℃) with the MQ resin.Vacuumize then to remove as far as possible and desolvate, promptly get desired product.
Comparative example
Press in the table 3 the comparative example prescription silicon rubber and toluene are added in the reaction flask, be warming up to 90 ℃ under stirring, silicon rubber is dissolved fully.Stop heating, be cooled to room temperature.Tetramethylammonium hydroxide is dissolved in deionized water and isopropylcarbinol, and adds in the above-mentioned silicone rubber solution, reflux 2.5h (controlled temperature is 110 ℃) with the MQ resin.Vacuumize then to remove as far as possible and desolvate, promptly get desired product.
The performance of above-mentioned each routine product sees Table 4 (be selected from Best Curing, 1% dibenzoyl peroxide that all adds the tackiness agent total amount is as solidifying agent, 120 ℃ of solidification values).
| Material name | Proportioning (wt%) | |
| MQ resin 1 | MQ resin 2 | |
| Water glass (solid content 10%, modulus 3.6) | ????60 | ????80 |
| Hexamethyldisiloxane (MM) | ????20 | ????10 |
| Ethanol | ????20 | ????20 |
| Hydrochloric acid (36%～38%) | ????35 | ????35 |
| Toluene | ????100 | ????100 |
Table 1
| Material name | Proportioning (wt%) | |
| Hydroxy-end capped silicon rubber 1 | Hydroxy-end capped silicon rubber 2 | |
| Octamethylcyclotetrasiloxane (D 4) | ????100 | ????100 |
| Vinyl cyclotetrasiloxane (D 4 v) | ????0.25 | ????0.26 |
| Hydroxy silicon oil | ????0.05 | ????0.08 |
| Tetramethyl-oxyammonia silicon alkoxide | ????0.3 | ????0.5 |
Table 2
| Material name | Proportioning (wt%) | |||
| Prescription 1 | Prescription 2 | Prescription 3 | Comparative example | |
| MQ resin of the present invention | ??10 | ??12 | ??15 | ??- |
| Commercially available MQ resin with the tetraethyl silicate preparation | ??- | ??- | ??- | ??15 |
| Hydroxy-end capped silicon rubber | ??15 | ??13 | ??10 | ??10 |
| Alkaline catalysts | ??0.0100 | ??0.0120 | ??0.0125 | ??0.0125 |
| Deionized water | ??2 | ??2 | ??2 | ??2 |
| Isopropylcarbinol | ??1.25 | ??1.25 | ??1.25 | ??1.25 |
| Toluene | ??100 | ??100 | ??100 | ??100 |
Table 3
| Performance project | Prescription 1 | Prescription 2 | Prescription 3 | Comparative example |
| Time of drying (s) | 15 | 15 | ????13 | ??15 |
| Outward appearance | Water white transparency | Water white transparency | Water white transparency | Water white transparency |
| 180 ° of stripping strengths (N/25cm) | 22 | 23.2 | ????20.8 | ??22.4 |
| Thermotolerance (200 ℃, 500h) | Do not have and destroy | Do not have and destroy | Do not have and destroy, slightly jaundice | Do not have and destroy |
Table 4
Claims (5)
1. high temperature resistant silicone adhesive is reacted in the presence of catalyzer by MQ resin and hydroxy-end capped silicon rubber and to form, and it is as follows to it is characterized in that specifically forming proportioning:
Amounts of components is 100 weight parts in toluene
MQ resin 10～15
Hydroxy-end capped silicon rubber 10～15
Alkaline catalysts 0.0100～0.0125
Deionized water 2
Isopropylcarbinol 1.25
Toluene 100
2. the preparation method of high temperature resistant silicone adhesive according to claim 1 is characterized in that: preparation divides following three steps:
(1) preparation of MQ resin, its preparation process is: at first by following component concentration weighing:
Amounts of components is 100 weight parts in toluene
Water glass, solid content 10%, modulus 3.6 60～80
Hexamethyldisiloxane, MM 10～20
Ethanol 15～30
Hydrochloric acid, 36%～38% 30～40
Toluene 100
MQ resin synthetic as follows:
With MM and water glass 60～70 ℃ of cohydrolysis 1～1.5 hour in hydrochloric acid and ethanol, add toluene then, refluxed 2～4 hours down at 70～80 ℃, isolate the upper strata organic layer after static, be washed with water to neutrality, add Calcium Chloride Powder Anhydrous and soak to eliminate moisture, toluene is removed in distillation at last, obtains pale yellow powder shape MQ resin;
(2) preparation of hydroxy-end capped silicone adhesive, its preparation process is: at first by following component concentration weighing:
Component concentration is with D
4Be 100 weight part meters
Octamethylcyclotetrasiloxane, D
4100
The vinyl cyclotetrasiloxane, D
4 v0.25～0.26
Hydroxy silicon oil, viscosity are 40～60mPas 0.08
Tetramethylammonium hydroxide silicon alkoxide 0.3～0.5
The synthetic method of hydroxy-end capped silicon rubber is as follows:
Above-mentioned raw materials is added in the reaction flask, vacuumize, logical then nitrogen is warming up to 80～90 ℃, react 1～3 hour, is warming up to 110～120 ℃, continues to react 1～3 hour, is warming up to 150～180 ℃ and vacuumize again;
(3) preparation of high temperature resistant silicone adhesive: at first weighing is good respectively by each amounts of components of aforesaid right requirement 1 described high temperature resistant silicone adhesive, then silicon rubber and toluene are added in the reaction flask, be warming up to 80～100 ℃ under stirring, silicon rubber is dissolved fully; Stop heating, be cooled to room temperature; Alkali is dissolved in deionized water and isopropylcarbinol, and adds in the above-mentioned silicone rubber solution with the MQ resin, 100～115 ℃ of following reflux 2～3 hours vacuumizing then to remove as far as possible and desolvating, and promptly get desired product.
3. the preparation method of high temperature resistant silicone adhesive according to claim 2 adds MM and ethanol in the hydrochloric acid earlier when it is characterized in that cohydrolysis, and 60～70 ℃ are stirred hydrolysis 20～30 minutes down, added the water glass cohydrolysis again 20～40 minutes.
4. the preparation method of high temperature resistant silicone adhesive according to claim 2 is heated to 60～70 ℃ with hydrochloric acid earlier when it is characterized in that cohydrolysis, adds water glass, MM and ethanol successively, cohydrolysis 20～40 minutes.
5. the preparation method of high temperature resistant silicone adhesive according to claim 2 is characterized in that its solidifying agent adopts dibenzoyl peroxide, and consumption is 0.5～1.5% of a tackiness agent total amount, and solidification value is 110～130 ℃.
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| CN103242746B (en) * | 2013-05-22 | 2014-06-18 | 苏州市丛岭胶粘剂有限公司 | Modified fireproof adhesive and preparation method thereof |
| CN103242746A (en) * | 2013-05-22 | 2013-08-14 | 苏州市丛岭胶粘剂有限公司 | Modified fireproof adhesive and preparation method thereof |
| CN103440903A (en) * | 2013-08-16 | 2013-12-11 | 卢儒 | Silicon resin composition for nuclear motor mica tape and application thereof |
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| CN110734739A (en) * | 2019-09-19 | 2020-01-31 | 宜宾天原集团股份有限公司 | Preparation method of organic silicon pressure-sensitive adhesives |
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