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Liquid hyperbranched polycarbosilane as well as preparation method and application thereof

A polycarbosilane, liquid technology, applied in the field of preparation, liquid hyperbranched polycarbosilane, can solve problems such as becoming viscous, and achieve the effects of low equipment requirements, reduced risk, and high ceramic yield

Pending Publication Date: 2022-06-03
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the above-mentioned deficiencies of the prior art, to provide a new preparation method of liquid hyperbranched polycarbosilane, to solve various problems caused by the system gradually becoming viscous and sharply rising in temperature, to eliminate the risk of thermal runaway and Improve preparation safety and product yield

Method used

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  • Liquid hyperbranched polycarbosilane as well as preparation method and application thereof
  • Liquid hyperbranched polycarbosilane as well as preparation method and application thereof
  • Liquid hyperbranched polycarbosilane as well as preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The liquid hyperbranched polycarbosilane, the preparation method and the application thereof provided in this embodiment are basically the same as those in the previous embodiment, except that the preparation method includes the following steps:

[0037]The reaction apparatus was dried to remove moisture prior to preparation. A mixed solvent consisting of 0.43 mol of metallic magnesium, 100 ml of toluene and 100 ml of tetrahydrofuran was added to a four-necked flask with a constant pressure dropping funnel, a condensation device, a stirrer and a thermometer. 0.2 mol of chloromethyl(methyl)dichlorosilane, 0.1 mol of chloromethyltrichlorosilane, 0.06 mol of allyl chloride (3-chloropropene) monomer were added to the constant pressure dropping funnel. The reaction device was evacuated, repeated 3-5 times, and then high-purity nitrogen was introduced. Start the stirrer, slowly add the monomer dropwise through the constant pressure dropping funnel, keep the temperature at ro...

Embodiment 2

[0040] The liquid hyperbranched polycarbosilane, the preparation method and the application thereof provided in this embodiment are basically the same as those in the foregoing embodiment 1, except that the preparation method comprises the following steps:

[0041] The reaction apparatus was dried to remove moisture prior to preparation. A mixed solvent consisting of 0.57 mol of metallic magnesium, 100 ml of toluene and 100 ml of tetrahydrofuran was added to a four-necked flask with a constant pressure dropping funnel, a condensation device, a stirrer and a thermometer. 0.2 mol of chloromethyl (methyl) dichlorosilane, 0.2 mol of chloromethyl trichlorosilane, 0.04 mol of allyl chloride (3-chloropropene) monomer were added to the constant pressure dropping funnel. The reaction device was evacuated, repeated 3-5 times, and then high-purity nitrogen was introduced. Start the stirrer, slowly add the monomer dropwise through the constant pressure dropping funnel, keep the temperatu...

Embodiment 3

[0044] The liquid hyperbranched polycarbosilane, the preparation method and the application thereof provided in this embodiment are basically the same as those of the foregoing embodiments 1 and 2, except that the preparation method includes the following steps:

[0045] The reaction apparatus was dried to remove moisture prior to preparation. A mixed solvent consisting of 0.76 mol of metal magnesium, 100 ml of toluene and 100 ml of tetrahydrofuran was added to a four-necked flask with a constant pressure dropping funnel, a condensation device, a stirrer and a thermometer. 0.2 mol of chloromethyl (methyl) dichlorosilane, 0.4 mol of chloromethyl trichlorosilane, 0.116 mol of allyl chloride (3-chloropropene) monomer were added to the constant pressure dropping funnel. The reaction device was evacuated, repeated 3-5 times, and then high-purity nitrogen was introduced. Start the stirrer, slowly add the monomer dropwise through the constant pressure dropping funnel, keep the tempe...

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Abstract

The invention discloses liquid hyperbranched polycarbosilane as well as a preparation method and application thereof. The liquid hyperbranched polycarbosilane is polycarbosilane containing carbon-carbon double bonds, the structural formula of the liquid hyperbranched polycarbosilane is [SiHx (CH3) y (C = CH2) zCH2] n, n is a natural number larger than 0, and x + y + z = 2. According to the preparation method, under the protection of inert gas, chloromethyl trichlorosilane, chloromethyl (methyl) dichlorosilane and magnesium serve as raw materials, tetrahydrofuran and aromatic hydrocarbon serve as a mixed solvent, polycarbosilane is obtained through a one-kettle method, the method is mild in reaction condition, safe and controllable, the problems of reaction failure, thermal runaway and the like easily caused by a traditional single solvent system are solved, and the method is suitable for industrial production. The prepared liquid hyperbranched polycarbosilane is polycarbosilane containing carbon-carbon double bonds, has a relatively high ceramic conversion rate as a precursor, and has a wide prospect in the field of preparation of high-temperature antioxidant ceramics.

Description

Technical field: [0001] The invention relates to the technical field of high polymer manufacturing, in particular to a liquid hyperbranched polycarbosilane, a preparation method and applications thereof. Background technique: [0002] Silicon carbide ceramics have excellent properties such as low density, high modulus, high temperature resistance, and corrosion resistance. Silicon carbide ceramics and their matrix composites play a huge role in high-end fields such as aerospace. Currently. One of the main methods for preparing silicon carbide ceramic materials is the precursor impregnation cracking method, which has a simple preparation process, low heat treatment temperature and low equipment requirements. [0003] In the prior art, the key to the successful preparation of silicon carbide ceramic materials by the precursor impregnation cracking method lies in the precursor polymer, and the liquid hyperbranched polycarbosilane has good room temperature fluidity and high cer...

Claims

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Application Information

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IPC IPC(8): C08G77/60C04B35/571C04B35/622
CPCC08G77/60C04B35/571C04B35/622
Inventor 甄强卢毓鹏陈来
Owner SHANGHAI UNIV
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