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Method for synthesizing soluble ZrC ceramic precursor polymer

A technology of ceramic precursors and synthesis methods, which is applied in the field of synthesis of soluble ZrC ceramic precursor polymers, can solve the problems of uneven distribution of metal elements, low ceramic yield, high oxygen content of products, etc., to reduce the ceramicization temperature, Improvement of ceramic productivity and easy availability of raw materials

Active Publication Date: 2016-06-22
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide a synthetic method of a soluble ZrC ceramic precursor polymer, which solves the technical problems of low ceramic yield, uneven distribution of metal elements in the product, and high oxygen content in the product in the prior art

Method used

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  • Method for synthesizing soluble ZrC ceramic precursor polymer
  • Method for synthesizing soluble ZrC ceramic precursor polymer
  • Method for synthesizing soluble ZrC ceramic precursor polymer

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preparation example Construction

[0027] The preparation method provided by the invention uses zirconium dichloride (Cp 2 ZrCl 2 ) or trichlorozirconocene (CpZrCl 3 ) as a zirconium source, using Grignard reagents containing double bonds such as allyl Grignard reagents and 3-butene Grignard reagents as carbon sources, and reacting with anhydrous xylene as a solvent below -5°C for 4-12 hours . Adding an initiator with a mass fraction of 3wt%-8wt% to the obtained monomer, raising the temperature to 100-130° C. and refluxing for 6-48 hours to obtain a soluble ZrC ceramic precursor.

[0028] Reacting in this way can reduce the oxygen element introduced into the reaction system, and further ensure that the obtained ceramic product has lower porosity and high ceramic yield. Moreover, the precursor prepared by the method can be dissolved in organic solvents such as xylene and toluene, and has good solubility.

[0029] More preferably, the initiator is dicumyl peroxide. Using this as an initiator can effectively ...

Embodiment 1

[0044] (1) Add a magnetic stirrer to the dried 250ml three-necked flask, and install a constant pressure dropping funnel, a gas outlet piston, and a rubber stopper, and replace it with high-purity nitrogen three times;

[0045] (2) 3g of zirconocene dichloride was added to a three-necked flask, and 10ml of anhydrous xylene was used as a solvent, and the reaction device was cooled to -20°C;

[0046] (3) Allylmagnesium chloride Grignard reagent is added to the reaction system through a constant pressure dropping funnel at a molar ratio of Grignard reagent: zirconium source=2: 1; after the addition, keep the low temperature and stir for 4 hours;

[0047] (4) After the above reaction system was reacted at room temperature for 24 hours, the inorganic salt was filtered out to obtain the active monomer, and dicumyl peroxide was added as an initiator relative to the active monomer mass fraction of 5 wt %; heated to 130° C. Reflux for 20 hours;

[0048] (5) After the reflux was comple...

Embodiment 2

[0053] (1) Add a magnetic stirrer to the dried 250ml three-necked flask, and install a constant pressure dropping funnel, a gas outlet piston, and a rubber stopper, and replace it with high-purity nitrogen three times;

[0054] (2) 3g of zirconocene dichloride was added to a three-necked flask, and 10ml of anhydrous xylene was used as a solvent, and the reaction device was cooled to -5°C;

[0055] (3) 3-butenylmagnesium chloride Grignard reagent is added to the reaction system through a constant pressure dropping funnel at a molar ratio of Grignard reagent: zirconium source=2: 1; after the addition, keep the low temperature and stir for 8 hours ;

[0056] (4) After the above reaction system was reacted at room temperature for 18 hours, the inorganic salt was filtered out to obtain the active monomer, and dicumyl peroxide was added as an initiator relative to the active monomer mass fraction of 3wt%; heated to 100° C. Reflux for 18 hours;

[0057] (5) After the reflux was com...

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Abstract

The invention provides a method for synthesizing a soluble ZrC ceramic precursor polymer. According to the method, Cp2ZrCl2 or CpZrCl3 is taken as the zirconium source, a double-bond Grignard reagent such as the allyl Grignard reagent and 3-butene Grignard reagent is taken as the carbon source, and an activated monomer obtained through reaction of the zirconium source and the carbon source is polymerized through a proper initiator to obtain a soluble ZrC ceramic precursor. A ZrC superhigh temperature ceramic material can be obtained through high-temperature pyrolysis of the prepared ZrC ceramic precursor.

Description

technical field [0001] The invention relates to the technical field of ceramic preparation, in particular to a synthesis method of a soluble ZrC ceramic precursor polymer. Background technique [0002] ZrC ceramics have the characteristics of high hardness, high melting point (>3000°C) and high temperature resistance, and are important ultra-high temperature materials. At present, the preparation methods of ZrC ceramics mainly include high-temperature carbothermal reduction method, sol-gel method and precursor conversion method. [0003] The high-temperature carbothermal reduction method refers to the preparation of ZrC ceramic powder at a high temperature above 1600°C by placing zirconia or zirconium powder in carbon powder and mixing it (MaitreA, LefortP.Solidstatereactionofzirconiawithcarbon[J].SolidStateIonics,1997,104(1 ):109-122; Tsuchida T, Yamamoto S. Mechanical activation assisted self-propagating high-temperature synthesis of ZrCandZrB 2 inairfromZr / B / Cpowderm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F130/04C04B35/56
CPCC04B35/5622C04B2235/48C08F130/04
Inventor 龙鑫王军邵长伟王浩简科王小宙
Owner NAT UNIV OF DEFENSE TECH
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