CN105255441B - A kind of preparation method of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive - Google Patents
A kind of preparation method of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive Download PDFInfo
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- CN105255441B CN105255441B CN201510679811.3A CN201510679811A CN105255441B CN 105255441 B CN105255441 B CN 105255441B CN 201510679811 A CN201510679811 A CN 201510679811A CN 105255441 B CN105255441 B CN 105255441B
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Abstract
A kind of preparation method of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive, it is related to a kind of preparation method of adhesive.It will solve the problems, such as that existing modified Polycarbosilane viscosity is high, molecular weight distribution it is wide cause to be difficult to embedding, unstable properties, manufacturability poor.Method：First, dimethyldichlorosilane, trim,ethylchlorosilane, sodium and dimethylbenzene are mixed, low-molecular polysilane is obtained after reaction；2nd, silicon carbide is prepared；3rd, Polycarbosilane and t etram-ethyltetravinylcyclotetrasiloxane are dissolved in dimethylbenzene/tetrahydrofuran mixed solvent, addition obtains Polycarbosilane based high-temp-resistant embedding adhesive with chloroplatinic acid, after reaction.Method of the present invention method reduces the viscosity of Polycarbosilane, reduces molecular weight distribution, prepares the Polycarbosilane based high-temp-resistant embedding adhesive that a kind of viscosity is 1000 4000mPas, stable performance, it is easy to embedding and prepare face coat.
Description
Technical field
The present invention relates to a kind of preparation method of adhesive.
Background technology
With the development of Aeronautics and Astronautics technology, people propose higher and higher requirement to material, for example：Rocket, lead
Metal, ceramic material and composite that the fields such as bullet, space shuttle, atomic power device use, require and use high-temperature plastic
Stick is bonded and embedding.It is gluing that current high-temperature resistance adhesive is broadly divided into organic high-temperature resistance adhesive, inorganic high-temperature resistant
Agent, organosilicon fire-resistant adhesive.Organic high-temperature resistance adhesive mainly includes epoxy resin series, novolac systems, gathers
Benzimidazole series and polyimides series, its epoxy resin and novolac systems heatproof are usually no more than 600 DEG C；Polyphenyl
And imidazoles series is due to preparation technology and uses the extremely harsh limitation of technique, it is impossible to produce in enormous quantities；Polyimides series is solid
Change that temperature is high, rigidity is big after solidification, limits its range of application.Inorganic high-temperature resistant adhesive temperature in use is high, reported
Phosphate adhesive can be widely used to high temperature resistant bonding field, but inorganic high-temperature resistant adhesive in 1700 DEG C of long-term uses
Porous material is, its application in embedding adhesive area is limited.Organosilicon fire-resistant adhesive has good sealing
Property and can be applied in the range of -100~1200 DEG C, but organosilicon fire-resistant adhesive adhesive strength is low, limits its application
Scope.
Polycarbosilane is a kind of matrix resin of fire-resistant high-performance composite, in the national defence such as space flight, aviation tip skill
Art field has broad application prospects.It is modified using the Si -- H of high activity in Polycarbosilane, modified poly- carbon
Silane can be applied in adhesive area, but modified Polycarbosilane is generally solid, and liquid modifying Polycarbosilane viscosity is high, technique
Property is poor, limits Polycarbosilane in embedding and the application in face seal field.
The content of the invention
The invention aims to solve that existing modified Polycarbosilane viscosity is high, molecular weight distribution it is wide cause be difficult to fill
Envelope, unstable properties, the problem of manufacturability difference, and a kind of preparation of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive is provided
Method.
A kind of preparation method of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive, realizes according to the following steps：
First, by dimethyldichlorosilane, trim,ethylchlorosilane, sodium and dimethylbenzene mix, at 100-130 DEG C react 1~
4h, it is the low-molecular polysilane of 1500~5000mPas, decentralization less than 2 that viscosity is obtained after purification；Wherein dimethyl dichloro
Silane is 1 with the mol ratio of trim,ethylchlorosilane:(0.1~0.75), dimethyldichlorosilane is 1 with the mol ratio of sodium:(1.25
~2.0), dimethyldichlorosilane is 1 with the volume ratio of dimethylbenzene:(1.25~2.75)；
2nd, by low-molecular polysilane, 1~5h is reacted under 250~400 DEG C, 5~15MPa, inert gas shielding, is obtained
Viscosity is the silicon carbide of 1500~6000mPas, decentralization less than 2；
3rd, gained Polycarbosilane and t etram-ethyltetravinylcyclotetrasiloxane in step 2 are dissolved in dimethylbenzene/tetrahydrochysene furan
Mutter in mixed solvent, add chloroplatinic acid, 0.5~4h is reacted at room temperature, it is 1000~4000mPas's that viscosity is obtained after purification
Polycarbosilane based high-temp-resistant embedding adhesive；Wherein Polycarbosilane and the mol ratio of t etram-ethyltetravinylcyclotetrasiloxane is 1:
(0.1~2.0), Polycarbosilane is 1 with the mass ratio of chloroplatinic acid:(0~0.1), dimethylbenzene is 1 with the volume ratio of tetrahydrofuran:
(0.5~2).
The present invention solves that existing modified Polycarbosilane viscosity is high, molecular weight distribution it is wide cause be difficult to embedding, performance not
The problem of stabilization, manufacturability difference, using the viscosity present approach reduces Polycarbosilane, reduces molecular weight distribution, prepares one
Plant the Polycarbosilane based high-temp-resistant embedding adhesive that viscosity is 1000~4000mPas, stable performance, it is easy to embedding and preparation
Face coat, after 180 DEG C of solidifications, 1000 DEG C of thermal weight losses (nitrogen atmosphere) are less than 10%, are bonded refractory metal, 1000 DEG C of bondings
Intensity rate of descent is less than 50%.
Brief description of the drawings
Fig. 1 is after 180 DEG C of solidification 2h of gained low viscosity Polycarbosilane based high-temp-resistant embedding adhesive are prepared in embodiment 1
TG spectrograms.
Specific embodiment
Technical solution of the present invention is not limited to act specific embodiment set forth below, also including between each specific embodiment
Any combination.
Specific embodiment one：The preparation method of present embodiment low viscosity Polycarbosilane based high-temp-resistant embedding adhesive,
Realize according to the following steps：
First, by dimethyldichlorosilane, trim,ethylchlorosilane, sodium and dimethylbenzene mix, at 100-130 DEG C react 1~
4h, it is the low-molecular polysilane of 1500~5000mPas, decentralization less than 2 that viscosity is obtained after purification；Wherein dimethyl dichloro
Silane is 1 with the mol ratio of trim,ethylchlorosilane:(0.1~0.75), dimethyldichlorosilane is 1 with the mol ratio of sodium:(1.25
~2.0), dimethyldichlorosilane is 1 with the volume ratio of dimethylbenzene:(1.25~2.75)；
2nd, by low-molecular polysilane, 1~5h is reacted under 250~400 DEG C, 5-15MPa, inert gas shielding, is glued
Spend the silicon carbide less than 2 for 1500~6000mPas, decentralization；
3rd, gained Polycarbosilane and t etram-ethyltetravinylcyclotetrasiloxane in step 2 are dissolved in dimethylbenzene/tetrahydrochysene furan
Mutter in mixed solvent, add chloroplatinic acid, 0.5~4h is reacted at room temperature, it is 1000~4000mPas's that viscosity is obtained after purification
Polycarbosilane based high-temp-resistant embedding adhesive；Wherein Polycarbosilane and the mol ratio of t etram-ethyltetravinylcyclotetrasiloxane is 1:
(0.1~2.0), Polycarbosilane is 1 with the mass ratio of chloroplatinic acid:(0~0.1), dimethylbenzene is 1 with the volume ratio of tetrahydrofuran:
(0.5~2).
In present embodiment step one dimethyldichlorosilane be raw material, trim,ethylchlorosilane be molecular weight regulator, sodium
For catalyst, dimethylbenzene are solvent.
Chloroplatinic acid is catalyst in present embodiment step 3.
Specific embodiment two：Present embodiment from unlike specific embodiment one, it is anti-at 12 DEG C in step one
2h is answered, low-molecular polysilane of the viscosity for 3000mPas, decentralization less than 2 is obtained after purification.Its step and parameter with it is specific
Implementation method one is identical.
Specific embodiment three：Present embodiment from unlike specific embodiment one or two, dimethyl in step one
Dichlorosilane is 1 with the mol ratio of trim,ethylchlorosilane:0.5.Other steps and parameter are identical with specific embodiment one or two.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three, two in step one
Dimethyl dichlorosilane (DMCS) is 1 with the mol ratio of sodium:1.5.Other steps and parameter are identical with one of specific embodiment one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four, two in step one
Dimethyl dichlorosilane (DMCS) is 1 with the volume ratio of dimethylbenzene:2.Other steps and parameter are identical with one of specific embodiment one to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five, in step 2
300 DEG C, 10MPa, react 2h under inert gas shielding, obtain low molecular weight polycaprolactone carbon of the viscosity for 3000mPas, decentralization less than 2
Silane.Other steps and parameter are identical with one of specific embodiment one to five.
Specific embodiment seven：It is lazy in step 2 unlike one of present embodiment and specific embodiment one to six
Property gas purity be 99.999%.Other steps and parameter are identical with one of specific embodiment one to six.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven, room in step 3
The lower reaction 2h of temperature, obtains the Polycarbosilane based high-temp-resistant embedding adhesive that viscosity is 2000mPas after purification.Other steps and
Parameter is identical with one of specific embodiment one to seven.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight, gather in step 3
Carbon silane is 1 with the mol ratio of t etram-ethyltetravinylcyclotetrasiloxane:1.Other steps and parameter and specific embodiment one
It is identical to one of eight.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine, gather in step 3
Carbon silane is 1 with the mass ratio of chloroplatinic acid:0.05.Other steps and parameter are identical with one of specific embodiment one to nine.
Specific embodiment 11：Unlike one of present embodiment and specific embodiment one to ten, in step 3
Dimethylbenzene is 1 with the volume ratio of tetrahydrofuran:1.5.Other steps and parameter are identical with one of specific embodiment one to ten.
Beneficial effects of the present invention are verified using following examples：
Embodiment 1：
The preparation method of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive, realizes according to the following steps：
First, by dimethyldichlorosilane, trim,ethylchlorosilane, sodium and dimethylbenzene mix, at 100~130 DEG C react 1~
4h, obtains low-molecular polysilane of the viscosity for 2000mPas, decentralization less than 2 after purification；Wherein dimethyldichlorosilane with
The mol ratio of trim,ethylchlorosilane is 1:0.4, dimethyldichlorosilane is 1 with the mol ratio of sodium:1.6, dimethyldichlorosilane
It is 1 with the volume ratio of dimethylbenzene:2；
2nd, by low-molecular polysilane, 2h is reacted under 300 DEG C, 10MPa, inert gas shielding, obtaining viscosity is
The silicon carbide of 3000mPas, decentralization less than 2；
3rd, gained Polycarbosilane and t etram-ethyltetravinylcyclotetrasiloxane in step 2 are dissolved in dimethylbenzene/tetrahydrochysene furan
Mutter in mixed solvent, 3h is reacted at room temperature, the Polycarbosilane based high-temp-resistant casting glue that viscosity is 2000mPas is obtained after purification
Stick；Wherein Polycarbosilane and the mol ratio of t etram-ethyltetravinylcyclotetrasiloxane is 1:1, the body of dimethylbenzene and tetrahydrofuran
Product is than being 1:1.
Gained low viscosity Polycarbosilane based high-temp-resistant embedding adhesive is prepared in this implementation, after solidifying 2h at 180 DEG C, is carried out
Detection, as a result as shown in figure 1,1000 DEG C of thermal weight losses are 9.7%.
Embodiment 2：
The preparation method of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive, realizes according to the following steps：
First, by dimethyldichlorosilane, trim,ethylchlorosilane, sodium and dimethylbenzene mix, at 100~130 DEG C react 1~
4h, obtains low-molecular polysilane of the viscosity for 3000mPas, decentralization less than 2 after purification；Wherein dimethyldichlorosilane with
The mol ratio of trim,ethylchlorosilane is 1:0.2, dimethyldichlorosilane is 1 with the mol ratio of sodium:1.7, dimethyldichlorosilane
It is 1 with the volume ratio of dimethylbenzene:2.3；
2nd, by low-molecular polysilane, 3h is reacted under 350 DEG C, 9MPa, inert gas shielding, obtaining viscosity is
The silicon carbide of 4000mPas, decentralization less than 2；
3rd, gained Polycarbosilane and t etram-ethyltetravinylcyclotetrasiloxane in step 2 are dissolved in dimethylbenzene/tetrahydrochysene furan
Mutter in mixed solvent, add chloroplatinic acid, 1h is reacted at room temperature, the Polycarbosilane base that viscosity is 1500mPas is obtained after purification resistance to
High temperature embedding adhesive；Wherein Polycarbosilane and the mol ratio of t etram-ethyltetravinylcyclotetrasiloxane is 1:1.5, Polycarbosilane
It is 1 with the mass ratio of chloroplatinic acid:0.05, dimethylbenzene is 1 with the volume ratio of tetrahydrofuran:1.2.
Gained low viscosity Polycarbosilane based high-temp-resistant embedding adhesive, performance detection, as a result such as the He of table 1 are prepared in this implementation
Shown in table 2, it is seen then that gained low viscosity Polycarbosilane based high-temp-resistant embedding adhesive is prepared in this implementation, 25 DEG C of viscosity are
2000mPas, is bonded refractory metal, and after 180 DEG C of solidification 2h, 1000 DEG C of shear strength rates of descent are less than 50%.
The shear strength of the Polycarbosilane based high-temp-resistant embedding adhesive of table 1
| Test temperature (DEG C) | Normal temperature | 200 | 500 | 800 | 1000 |
| Shear strength * (MPa) | 2.2 | 2.2 | 2.1 | 1.3 | 1.2 |
Note：* it is refractory metal by viscous material, curing process is 180 DEG C, solidifies 2h
The agent viscosity of the Polycarbosilane based high-temp-resistant embedding adhesive of table 2
| Test temperature (DEG C) | 20 | 25 | 30 | 35 |
| Viscosity (mPas) | 2500 | 2000 | 1750 | 1300 |
Claims (9)
1. a kind of preparation method of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive, it is characterised in that it is real according to the following steps
It is existing：
First, dimethyldichlorosilane, trim,ethylchlorosilane, sodium and dimethylbenzene are mixed, 1~4h are reacted at 100~130 DEG C,
It is the low-molecular polysilane of 1500~5000mPas, decentralization less than 2 that viscosity is obtained after purification；Wherein dimethyldichlorosilane
It is 1 with the mol ratio of trim,ethylchlorosilane: (0.1~0.75), dimethyldichlorosilane is 1 with the mol ratio of sodium: (1.25~
2.0), dimethyldichlorosilane and the volume ratio of dimethylbenzene are 1: (1.25~2.75)；
2nd, by low-molecular polysilane, 1~5h is reacted under 250~400 DEG C, 5~15MPa, inert gas shielding, obtains viscosity
Silicon carbide for 1500-6000mPas, decentralization less than 2；
3rd, gained Polycarbosilane and t etram-ethyltetravinylcyclotetrasiloxane in step 2 are dissolved in dimethylbenzene/tetrahydrofuran and are mixed
In bonding solvent, chloroplatinic acid is added, 0.5~4h is reacted at room temperature, the poly- carbon that viscosity is 1000~4000mPas is obtained after purification
Silane based high-temp-resistant casting glue stick；Wherein Polycarbosilane and the mol ratio of t etram-ethyltetravinylcyclotetrasiloxane is 1: (0.1
~2.0), Polycarbosilane is 1 with the mass ratio of chloroplatinic acid: (0~0.1), dimethylbenzene is 1: (0.5 with the volume ratio of tetrahydrofuran
~2).
2. the preparation method of a kind of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive according to claim 1, it is special
Levy is that dimethyldichlorosilane and the mol ratio of trim,ethylchlorosilane are 1: 0.5 in step one.
3. the preparation method of a kind of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive according to claim 1, it is special
Levy is that dimethyldichlorosilane and the mol ratio of sodium are 1: 1.5 in step one.
4. the preparation method of a kind of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive according to claim 1, it is special
Levy is that dimethyldichlorosilane and the volume ratio of dimethylbenzene are 1: 2 in step one.
5. the preparation method of a kind of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive according to claim 1, it is special
It is to react 2h under 300 DEG C, 10MPa, inert gas shielding in step 2 to levy, and obtains viscosity for 3000mPas, decentralization
Silicon carbide less than 2.
6. the preparation method of a kind of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive according to claim 1, it is special
It is to react 2h at room temperature in step 3 to levy, and the Polycarbosilane based high-temp-resistant casting glue that viscosity is 2000mPas is obtained after purification
Stick.
7. the preparation method of a kind of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive according to claim 1, it is special
Levy is that Polycarbosilane and the mol ratio of t etram-ethyltetravinylcyclotetrasiloxane are 1: 1 in step 3.
8. the preparation method of a kind of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive according to claim 1, it is special
Levy is that Polycarbosilane and the mass ratio of chloroplatinic acid are 1: 0.05 in step 3.
9. the preparation method of a kind of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive according to claim 1, it is special
Levy is that dimethylbenzene and the volume ratio of tetrahydrofuran are 1: 1.5 in step 3.
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| CN201510679811.3A CN105255441B (en) | 2015-10-19 | 2015-10-19 | A kind of preparation method of low viscosity Polycarbosilane based high-temp-resistant embedding adhesive |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106349994A (en) * | 2016-08-25 | 2017-01-25 | 安徽大松树脂有限公司 | High-peel-strength heat-resistant aging-resistant adhesive |
| CN106244070A (en) * | 2016-08-25 | 2016-12-21 | 安徽大松树脂有限公司 | A kind of heat-resisting ageing-resisting modified adhesive |
| CN106752938B (en) * | 2016-12-08 | 2019-03-22 | 黑龙江省科学院石油化学研究院 | Ceramic surface seals the preparation method of resistance to 600 DEG C of high temperature coating materials |
| CN110746917A (en) * | 2019-10-18 | 2020-02-04 | 李志兴 | Preparation method of high-temperature-resistant epoxy resin adhesive |
| CN113185921B (en) * | 2021-06-03 | 2022-09-09 | 哈尔滨工程大学 | Preparation method of ceramic precursor modified phosphate adhesive |
| CN114275804A (en) * | 2021-11-26 | 2022-04-05 | 中国电子科技集团公司第十一研究所 | Preparation method of distributed gain suspended particle solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5631082A (en) * | 1988-04-07 | 1997-05-20 | Kanegafuchi Chemical Industry Co., Ltd. | Pressure-sensitive adhesive material |
| CN101045819A (en) * | 2007-04-30 | 2007-10-03 | 东莞市贝特利新材料有限公司 | Organic silicon resin composite |
| CN102250356A (en) * | 2011-06-20 | 2011-11-23 | 厦门大学 | Copolysilane and preparation method thereof |
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2015
- 2015-10-19 CN CN201510679811.3A patent/CN105255441B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5631082A (en) * | 1988-04-07 | 1997-05-20 | Kanegafuchi Chemical Industry Co., Ltd. | Pressure-sensitive adhesive material |
| CN101045819A (en) * | 2007-04-30 | 2007-10-03 | 东莞市贝特利新材料有限公司 | Organic silicon resin composite |
| CN102250356A (en) * | 2011-06-20 | 2011-11-23 | 厦门大学 | Copolysilane and preparation method thereof |
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