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High temperature resistant organosilicon adhesive, special silicon nitrogen polymer therefore and preparation

A silicon-nitrogen polymer, high temperature resistant technology, used in non-polymer adhesive additives, adhesives, adhesive additives, etc., can solve the problems of high price, material corrosion, increased brittleness, etc. The effect of excellent temperature and good toughness

Inactive Publication Date: 2009-03-04
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of heat-resistant resin is expensive, and as the degree of crosslinking increases, the brittleness also increases
Inorganic adhesives have the highest heat-resistant temperature, but they are more brittle and cause certain corrosion to materials

Method used

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  • High temperature resistant organosilicon adhesive, special silicon nitrogen polymer therefore and preparation
  • High temperature resistant organosilicon adhesive, special silicon nitrogen polymer therefore and preparation
  • High temperature resistant organosilicon adhesive, special silicon nitrogen polymer therefore and preparation

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preparation example Construction

[0025] Preparation of the first part of silicon nitrogen polymer

[0026] The structural formula of silicon nitrogen polymer of the present invention is:

[0027]

[0028] In the structural formula: R 1 , R 2 Respectively hydrogen, methyl, phenyl, vinyl and other groups; m, n are 0, 1 or 2, and m+n=1 or 2; x is 50-200.

[0029] Its synthetic method is: add R in the there-necked bottle 1 SiCl 3 , R 1 R 2 SiCl 2 and organic solvents, start to feed NH under stirring and cooling in a water bath 3 , until the ammonia is no longer absorbed, reduce the flow of NH 3 Velocity, Repass NH 3 After about 1 to 2 hours, stop the reaction, remove the ammonium chloride by filtration, wash the ammonium chloride with an organic solvent for 3 to 4 times, and remove the solvent and oligomers by distillation and vacuum distillation to obtain a silicon nitrogen polymer.

[0030] Wherein, the concrete condition of above-mentioned polymerization reaction is: R 1 SiCl 3 , R 1 R 2 SiCl ...

Embodiment 1

[0034] Add 53g (0.5mol) of HSiCl in the three-neck flask 3 , 82g (0.5mol) of Me 2 SiCl 2 and 500ml of toluene, NH was introduced under stirring and cooling 3 , 50~70ml / min, to NH 3 no longer absorbed, lowering NH 3 The flow rate is 10-20ml / min, continue to pass for 1-2 hours, stop the reaction, filter to remove ammonium chloride, and wash with toluene 3 times, remove the solvent and oligomers by decompression method, and obtain 60g of silicon nitrogen polymer , yield 72%. By coulometric titration, the measured nitrogen content was 28.91%, and the calculated value was 30.52%. Its number average molecular weight is 600, and molecular weight distribution is 1.58, and silicon spectrogram is as follows figure 1 shown.

Embodiment 2

[0036] Add 269.1g (1.8mol) of MeSiCl in the three-necked flask 3 , 141g (1mol) of MeViSiCl 2 And the THF of 1500ml, carry out reaction and process by the operation and reaction condition of example 1, obtain the silicon nitrogen polymer of 199.4g, productive rate 73%, nitrogen content 24.31%, calculated value 25.52%. Its number average molecular weight was 1000, and its molecular weight distribution was 1.85.

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Abstract

The invention discloses a high temperature resistant organic silicon binding agent, as well as a dedicated silicon nitrogen polymer thereof and a preparation method. The structure of the provided silicon nitrogen polymer is shown as the formula I, wherein, R<1> and R<2> are H, methyl, phenyl or vinyl respectively; m and n are 0, 1 or 2, m plus n is equal to 1 or 2; and x is an integer between 50 to 200. The invention develops the novel silicon nitrogen polymer and takes the silicon nitrogen polymer as a toughening agent for preparing the high temperature resistant organic silicon binding agent. Compared with phenolic resin and polyimide, the binding agent can be cured at room temperature, the binding agent further has good toughness after the room temperature curing; furthermore, the binding agent has high temperature resistant performance as the binding agent and still has considerable shear strength at 550 DEG C. The binding agent has the advantages of better thermal stability, mechanical performance and binding performance; the temperature resistance is better than silicon rubber, epoxy resin and modified epoxy resin; and compared with the inorganic binding agent, the binding agent has great toughness.

Description

technical field [0001] The invention relates to a high temperature resistant organic silicon adhesive, a silicon nitrogen polymer used in the adhesive and a preparation method. Background technique [0002] At present, high temperature resistant adhesives include silicone rubber, silicone resin, phenolic, polyimide, epoxy resin, etc. Generally, thermosetting resins have higher temperature resistance than linear thermoplastic resins, while thermoplastic resins with crystalline structures are more resistant to random structures. The resin is heat resistant. For phenolic, polyimide or other aromatic resins, these binders have many excellent properties and are widely used in aviation, aerospace and other fields. The molecular main chain structure of silicone resin is composed of silicon-oxygen bonds with high bond energy, which is much higher in heat resistance than the molecular structure of carbon chains, and is a good main component of heat-resistant adhesives. [0003] How...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/54C09J183/16C09J11/06C09J183/04
Inventor 罗永明徐彩虹郑知敏梅雪凝
Owner INST OF CHEM CHINESE ACAD OF SCI