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A kind of synthesis method of zr-si-c ceramic precursor at normal temperature and pressure

A ceramic precursor and atmospheric pressure synthesis technology, applied in the field of normal temperature and pressure synthesis of Zr-Si-C ceramic precursors, can solve the problems of poor designability, complex process, low zirconium content of ceramic products, etc., and achieve less control conditions , simple equipment and improved safety

Active Publication Date: 2019-03-29
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, the existing synthetic methods all require at least one of harsh reaction conditions such as high temperature, low temperature, high pressure, and electrification, the process is complex, the designability is poor, and the content of zirconium in ceramic products is low.

Method used

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  • A kind of synthesis method of zr-si-c ceramic precursor at normal temperature and pressure
  • A kind of synthesis method of zr-si-c ceramic precursor at normal temperature and pressure
  • A kind of synthesis method of zr-si-c ceramic precursor at normal temperature and pressure

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Experimental program
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Effect test

Embodiment 1

[0035] This embodiment includes the following steps:

[0036](1) Under normal temperature, normal pressure, and nitrogen protection, place 10.0g (39.8mmol) dimethyl zirconocene in a three-necked flask, stir and add 90mL of anhydrous and oxygen-free tetrahydrofuran to dissolve, drop in 8.8mL of TMEDA and 96.0mmol n-butyllithium (commercially available 2.4mol / L n-butyllithium n-hexane solution 40.0mL), reacted for 11 hours, and vacuum dried to obtain active zirconocene lithium salt;

[0037] (2) Dissolve 5 g (14.7 mmol) of the active lithium zirconocene salt prepared in step (1) in 50.0 mL of anhydrous and oxygen-free tetrahydrofuran under normal temperature, normal pressure, and nitrogen protection. Dilute 2.1ml (17.4mmol) of dimethyldichlorosilane in 45.0mL of anhydrous and oxygen-free tetrahydrofuran, and drop into the solution of active zirconocene lithium salt, and stir for 13 hours to generate figure 1 Shown polymerization, drop 2.0mL of methanol to terminate the reaction...

Embodiment 2

[0042] This embodiment includes the following steps:

[0043] (1) At normal temperature, normal pressure, under the protection of argon, put 10.0g (39.8mmol) dimethyl zirconocene in a Schlenk bottle, stir and add 80mL of anhydrous and oxygen-free tetrahydrofuran to dissolve, drop in 8.8mL of TMEDA and 96.0mmol n-butyllithium (commercially available 2.4mol / L n-butyllithium n-hexane solution 40.0mL), reacted for 12 hours, and vacuum dried to obtain active zirconocene lithium salt;

[0044] (2) Dissolve 5 g (14.7 mmol) of the active lithium zirconocene salt prepared in step (1) in 40.0 mL of anhydrous and oxygen-free tetrahydrofuran at normal temperature, normal pressure, and under the protection of argon. Dilute 1.4ml (11.9mmol) of methyltrichlorosilane in 40mL of anhydrous and oxygen-free tetrahydrofuran, and drop into the solution of active zirconocene lithium salt, and stir for 11 hours to generate figure 2 For the indicated polymerization, 1.5 mL of absolute ethanol was ad...

Embodiment 3

[0047] This embodiment includes the following steps:

[0048] (1) At normal temperature, normal pressure, and under the protection of argon, put 10.0g (39.8mmol) dimethyl zirconocene in a three-necked flask, stir and add 90mL of anhydrous and oxygen-free tetrahydrofuran to dissolve, and drop into 8.8mL of TMEDA And 96.0mmol n-butyllithium (commercially available 2.4mol / L n-butyllithium n-hexane solution 40.0mL), reacted for 10 hours, and vacuum dried to obtain active zirconocene lithium salt;

[0049] (2) Dissolve 5 g (14.7 mmol) of the active lithium zirconocene salt prepared in step (1) in 50.0 mL of anhydrous and oxygen-free tetrahydrofuran under normal temperature, normal pressure, and nitrogen protection. Dilute 2.3ml (17.6mmol) of methyl vinyl dichlorosilane in 30.0mL of anhydrous anoxygen-free tetrahydrofuran, and drop into the solution of active lithium zirconocene salt, stir for 12 hours to generate image 3 Shown polymerization, drop 1.0mL of methanol to terminate t...

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Abstract

The invention relates to a normal-temperature and normal-pressure synthesizing method of a Zr-Si-C ceramic precursor. The normal-temperature and normal-pressure synthesizing method includes the steps of firstly, dissolving dimethyl zirconium dicyclopentadiene in an organic solvent under inert gas atmosphere protection, stirring, adding an organic lithium compound and a ligand compound, and drying to obtain active zirconium dicyclopentadiene lithium salt; secondly, dissolving the active zirconium dicyclopentadiene lithium salt with an organic solvent under inert gas atmosphere protection, stirring, adding halogenated silane monomer, performing polymerization reaction, dropwise adding a terminating agent to terminate the reaction, filtering, concentrating, purifying, and drying to obtain the Zr-Si-C ceramic precursor. The normal-temperature and normal-pressure synthesizing method has the advantages that conditions such as high temperature, low temperature, high pressure and energizing are not needed, the reaction can be performed under normal temperature and normal pressure, the dimethyl zirconium dicyclopentadiene high in activity and cheap and safe n-butyl lithium are used to have reaction with the halogenated silane monomer so as to prepare the Zr-Si-C ceramic precursor through a two-step method, and the preparation method is simple, scientific and reasonable; the Zr-Si-C ceramic precursor synthesized by the method is diversified and can be used for prepared various kinds of Zr-Si-C ceramics.

Description

technical field [0001] The invention relates to a synthesis method of a ceramic precursor, in particular to a synthesis method of a Zr-Si-C ceramic precursor at normal temperature and pressure. Background technique [0002] ZrO 2 / SiC,ZrSiO 4 / ZrC,SiO 2 A series of Zr-Si-C ceramics represented by / ZrC have different excellent characteristics such as high melting point, high hardness, high resistivity, and high refractive index. Materials, ceramic opacifiers and other fields have huge potential application value, so they have attracted much attention. Organic precursor conversion method is an important method for preparing Zr-Si-C ceramic materials. This method is easy to shape, has high product purity and high production efficiency. For example, Japan's Yamamura, Ishikawa et al. used zirconium acetylacetonate to react with the Si-H bond on polycarbosilane, and prepared the chemical formula SiC under the protection of nitrogen at 300 °C. 2.08 h 5.8 o 0.13 Zr 0.03 The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/56
CPCC04B35/56C04B2235/48
Inventor 苟燕子张千策王亦菲王浩简科王军邵长伟
Owner NAT UNIV OF DEFENSE TECH
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