Novel liquid polycarbosilane and preparation method thereof

A technology of polycarbosilane and liquid state, which is applied in the field of new liquid polycarbosilane and its preparation, which can solve the problems of poor impregnation effect, solvent residue, and low ceramic yield, and achieve high impregnation efficiency and the effect of not being prone to air bubbles

Inactive Publication Date: 2019-03-15
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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Problems solved by technology

[0005] The purpose of the present invention is to provide a novel liquid polycarbosilane and a preparation method thereof. The process of the novel liquid polycarbosilane with adjustable viscosity, adjustable silicon-carbon ratio and high ceramic yield has a wide application range and solves the problems of the prior art. The ceramic precursor polycarbosilane encountered problems such as low ceramic yield, poor impregnation effect, and solvent residue in the PIP process

Method used

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  • Novel liquid polycarbosilane and preparation method thereof
  • Novel liquid polycarbosilane and preparation method thereof
  • Novel liquid polycarbosilane and preparation method thereof

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preparation example Construction

[0051] The embodiment of the present invention also provides a method for preparing a liquid polycarbosilane, which is used to prepare a novel liquid polycarbosilane, the method comprising the following steps:

[0052] a. Prepare liquid polycarbosilane by Grignard coupling agent method, and prepare cyclosilane by pyrolysis method;

[0053] Specifically, in the embodiment of the present invention, liquid polycarbosilane can be prepared by a conventional format coupling agent method, and cyclosilane can be prepared by a conventional pyrolysis method; wherein, such as Figure 7 As shown, the mass ratio of liquid polycarbosilane to cyclosilane is preferably 1:0.1 to 1.5, more preferably 1:0.1 to 0.9, Figure 7 The middle abscissa is the mass ratio of liquid polycarbosilane and cyclosilane, and the ordinate is the viscosity.

[0054] b. Rearranging the cyclosilane and the liquid polycarbosilane to obtain a novel liquid polycarbosilane, the chemical structure of which is shown in f...

example 1

[0071] (1) Add 4.8g of magnesium metal into a three-necked flask reactor with stirring, constant pressure funnel, and reflux device, repeatedly vacuumize and fill dry inert gas at least three times to get rid of air and moisture therein, and pre-heat the reactor. Cool to 20°C;

[0072] (2) Take 100 ml of tetrahydrofuran solvent and inject it into the three-necked flask protected by dry nitrogen in step (1). Inject 144g of tetrahydrofuran, 5.5g of allyl chloride and 22g of chloromethyldichlorosilane into a constant pressure funnel with a syringe, and slowly add the mixture into a three-necked flask while stirring. The temperature was slowly raised to 70°C at a rate of 0.5°C / min, and kept at 70°C for 36 hours to obtain the Grignard reagent.

[0073] (3) Lower the temperature of the reactor to 20°C, add 19g of reducing agent lithium aluminum hydride at this temperature, slowly raise the temperature to 70°C at a rate of 0.5°C / min, and keep the temperature at 70°C for 24h.

[007...

example 2

[0078] (1) Add 4.8g of magnesium metal into a three-necked flask reactor with stirring, constant pressure funnel, and reflux device, repeatedly vacuumize and fill dry inert gas at least three times to get rid of air and moisture therein, and pre-heat the reactor. Cool to 20°C;

[0079] (2) Take 50ml of tetrahydrofuran solvent and inject it into the three-necked flask protected by dry nitrogen in step (1). Use a syringe to inject 210ml of tetrahydrofuran, 7g of allyl chloride and 42g of chloromethyldichlorosilane into a constant pressure funnel, and slowly add the mixture into a three-necked flask while stirring. The temperature was slowly raised to 70°C at a rate of °C / min, and kept at 70°C for 36 hours to obtain the Grignard reagent.

[0080] (3) Lower the temperature of the reactor to 20°C, add 19g of reducing agent lithium aluminum hydride at this temperature, slowly raise the temperature to 70°C at a rate of 0.5°C / min, and keep the temperature at 70°C for 20h.

[0081] (...

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Abstract

The invention relates to novel liquid polycarbosilane and a preparation method thereof, and belongs to the technical field of ceramic material synthesis. The novel liquid polycarbosilane has a chemical structural formula as follows: as shown in the specification, wherein m1, m2, m3 and m4 are all positive integers and more than or equal to 1. The novel liquid polycarbosilane provided by the embodiment of the invention can be adjusted in the viscosity from 10 to 1,000 cP, does not need to be used in combination with a solvent, has a certain degree of cross-linking between molecules, does not generate bubbles easily, is high in impregnation efficiency, and has a ceramic yield up to 81 percent.

Description

technical field [0001] The invention belongs to the technical field of synthesis of high-performance ceramic materials, and specifically relates to a novel liquid polycarbosilane with high ceramic yield, adjustable viscosity and adjustable silicon-carbon ratio and a preparation method thereof. Background technique [0002] High-performance ceramic materials have extremely high temperature resistance, oxidation resistance, wear resistance and anti-corrosion properties. It is a high-tech new material that is difficult for general metal materials and polymer materials. Applications in related fields have great application potential. [0003] Precursor impregnation-pyrolysis process (PIP) is a high-performance ceramic composite preparation process that has developed extremely rapidly in the past decade. Inorganic ceramics are obtained through the cracking and transformation of organic precursors at high temperatures, and special-shaped components with complex shapes can be prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C04B35/571
CPCC04B35/571C08G77/60
Inventor 冯志海李媛胡继东陶孟李军平
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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