Preparation method of SiBCN ceramic precursor containing borazine structure

A technology of ceramic precursor and borazane, which is applied in the field of preparation of SiBCN ceramic precursor, can solve the problems of difficult process control, difficulty in mass preparation, and difficulty in wide application of SiBCN ceramic matrix composite materials, and achieves low cost of raw materials , Excellent thermal stability, and the effect of large-scale preparation

Inactive Publication Date: 2015-10-14
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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  • Abstract
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  • Application Information

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Problems solved by technology

However, this synthetic route has problems such as difficult process control and large-scale p

Method used

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  • Preparation method of SiBCN ceramic precursor containing borazine structure
  • Preparation method of SiBCN ceramic precursor containing borazine structure

Examples

Experimental program
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Example Embodiment

[0032] Example 1

[0033] 1) In an anhydrous and oxygen-free environment, put the pre-activated magnesium chips into a Schlenk reaction flask. Under the protection of nitrogen, add 15mL tetrahydrofuran and 1.3g chloromethylmethylsilane. When the tetrahydrofuran is refluxed, place it in an ice bath. Add dropwise a mixed solution of 20.5g of chloromethylmethylsilane and 30mL of tetrahydrofuran, and then reflux at 60°C for 8 hours to obtain a Grignard reagent;

[0034] 2) In an anhydrous and oxygen-free environment, add dropwise a mixed solution of 12.9 g of trichloroborazine and 50 mL of toluene to the Grignard reagent obtained in step 1) under an ice bath, and then stir at room temperature for 8 hours, Remove the solvent and by-products to obtain the small molecule product containing the borazine structure; use a nuclear magnetic analyzer to characterize its H spectrum and C spectrum, such as figure 1 with 2 Shown.

Example Embodiment

[0035] Example 2

[0036] 1) In an anhydrous and oxygen-free environment, put the pre-activated magnesium chips into a Schlenk reaction flask. Under the protection of nitrogen, add 15 mL of ether and 1.5 g of chloromethyl methyl dichlorosilane. When the ether is refluxed, Add dropwise a mixed solution of 30.5g chloromethylmethyldichlorosilane and 50mL ether under an ice bath, and then reflux at 80°C for 6 hours to obtain a Grignard reagent;

[0037] 2) In an anhydrous and oxygen-free environment, add dropwise a mixed solution of 14.9 g of dichloroborazine and 50 mL of toluene to the Grignard reagent obtained in step 1) under an ice bath, and then stir at room temperature for 8 hours, Remove the solvent and by-products to obtain small molecular products containing borazine structure;

[0038] 3) In an anhydrous and oxygen-free environment, pass ammonia gas into the small molecule product in step 2) at -30°C until the system shows basicity. At this time, the amount of ammonia gas is a...

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Abstract

A preparation method of a SiBCN ceramic precursor containing a borazine structure belongs to the field of inorganic non-metal materials. The preparation method comprises the following steps of: firstly, preparing methylchlorosilane into a Grignard reagent, and taking the Grignard reagent to react with chlorine-containing borazine to obtain a micro-molecular structure containing the borazine structure; and furthermore, carrying out aminolysis on a micro-molecular product containing a Si-CI group to obtain a corresponding polymer product. A micro-molecule and a polymer are SiBCN ceramic precursors. The problems of an existing preparation method that a process is difficult to control, the product is difficult to prepare in batches and the like are solved. According to the preparation method provided by the invention, the cost of raw materials is low, the product with higher purity is easy to obtain and the product can be prepared in batches.

Description

Technical field [0001] The invention belongs to the field of inorganic non-metallic materials, and relates to a preparation method of a SiBCN ceramic precursor containing a borazine structure. Background technique: [0002] Continuous fiber reinforced ceramic matrix composites not only have the advantages of traditional ceramics such as high temperature resistance, corrosion resistance, wear resistance, and excellent mechanical properties, but also overcome the shortcomings of traditional ceramics themselves such as brittleness and catastrophic damage, showing excellent toughness and reliability It has broad application prospects in the fields of energy, aviation and aerospace. [0003] Among the preparation methods of various ceramic matrix composite materials, the precursor immersion cracking process has attracted wide attention from researchers due to its advantages such as low equipment requirements, convenient operation, strong designability of ceramic matrix, and easy prepara...

Claims

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Application Information

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IPC IPC(8): C08G79/08C04B35/58C07F5/02
Inventor 刘伟曹腊梅益小苏谭僖李麒
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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