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Polysiloxazane and preparation method thereof

A technology for polysiloxazane and silazane, which is applied in the field of polysiloxsilazane and its preparation, can solve the problems of tediousness, difficulty in realizing polymer structure regulation, affecting high temperature performance, etc., and achieves high purity and high yield. High rate and good thermal stability

Active Publication Date: 2019-07-09
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods are cumbersome and require the preparation of highly active silicon nitrogen lithium salt, or the use of highly corrosive bromine water and sodium hydroxide
Or require the use of expensive noble metal catalysts that are difficult to remove from the system, compromising high temperature performance
In addition, it is difficult to achieve the regulation of polymer structure

Method used

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  • Polysiloxazane and preparation method thereof
  • Polysiloxazane and preparation method thereof
  • Polysiloxazane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] 10L three-necked flask, after nitrogen replacement, add 5000ml toluene, add methylhydrogen dichlorosilane (CH 3 SiHCl 2 ) 460g, methylvinyldichlorosilane 56g, methyltrichlorosilane 1000g, under mechanical stirring, feed ammonia gas into the reaction solution until the system pH≥10. Filtrate under the protection of nitrogen, remove the ammonium chloride produced by the reaction, and remove the solvent in the solution by rotary evaporation to obtain 630 g of Si-H polysilazane (coded as PSN1), the structure of which is as follows:

[0061]

[0062] The above structure was verified by NMR and infrared detection.

Embodiment 2

[0064] 10L three-necked flask, after nitrogen replacement, add 5000ml toluene, add methylhydrogen dichlorosilane (CH 3 SiHCl 2 ) 100g, dimethyldichlorosilane 400g, methyltrichlorosilane 1000g, under mechanical stirring, feed ammonia gas into the reaction solution until the system pH≥10. Filtrate under the protection of nitrogen, remove the ammonium chloride produced by the reaction, and remove the solvent in the solution by rotary evaporation to obtain 607g of Si-H polysilazane (coded as PSN2), the structure is as follows:

[0065]

[0066] The above structure was verified by NMR and infrared detection.

Embodiment 3

[0068] 10L three-necked flask, after nitrogen replacement, add 5000ml toluene, add methylhydrogen dichlorosilane (CH 3 SiHCl 2 ) 460g, methylvinyldichlorosilane 800g, under mechanical stirring, feed ammonia gas into the reaction solution until the system pH ≥ 10. Filtrate under the protection of nitrogen, remove the ammonium chloride produced by the reaction, and remove the solvent in the solution by rotary evaporation to obtain 456g of Si-H polysilazane (coded as PSN3), the structure is as follows:

[0069]

[0070] Wherein, x and y are natural numbers greater than 1.

[0071] The above structure has been verified by nuclear magnetic and infrared detection, and as an exemplary illustration, the corresponding drawings are provided in the accompanying drawings of the description. figure 1 is PSN3 29 Si NMR spectrum, figure 2 is the infrared spectrum of PSN3.

[0072] Synthesis of Polysiloxazane

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Abstract

The invention belongs to the field of high polymer materials, and relates to polysiloxazane. The polysiloxazane is composed of a structural unit I represented by a formula (a) or / and a formula (b) anda structural unit II represented by a formula (c) or / and a formula (d), wherein R1 and R2 are the same or different and are selected from hydrogen, C1-C20 alkyl, vinyl, phenyl, allyl or trifluoropropyl, R3 and R4 are selected from hydrogen and C1-C20 alkyl, vinyl, phenyl, allyl or trifluoropropyl, R3 and R4 are not hydrogen at the same time, R5 and R6 are selected from H, methyl, ethyl, propyl orphenyl, m, n, p and q are integers from 1 to 1000, and the values of m, n, p and q are the same or different.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a polysiloxysilazane and a preparation method thereof. Background technique [0002] Polysiloxane is a polymer with Si-O bond as the main chain. According to its product form, it is divided into silicone oil, silicone rubber, and silicone resin. It is widely used in many fields such as electronics, food hygiene, and aerospace. . Polysilazane is a polymer with Si-N bond as the main chain. The particularity of its molecular structure endows it with special properties different from the general high molecular polymer with C-C bond as the main chain, and the main chain is Si-O The polysiloxane bond is also very different. It is often used as a precursor of silicon nitride-based ceramics or a high-temperature-resistant resin matrix to prepare high-temperature-resistant composite materials. It can also be used as an improvement for epoxy resin, silicone resin, an...

Claims

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Application Information

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IPC IPC(8): C08G77/452C08G77/62C08G77/54
CPCC08G77/452C08G77/54C08G77/62C08G77/80
Inventor 徐彩虹罗永明艾丽青潘振雪刘伟曹腊梅
Owner INST OF CHEM CHINESE ACAD OF SCI
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