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Method of synthesizing zirconium silicate powder at low temperature by unhydrolyzed sol-gel method

A technology of zirconium silicate and gel method, applied in the field of low temperature synthesis of zirconium silicate powder, can solve the problems of high price, difficult industrial production, difficult to obtain, etc., and achieves the effects of low cost, reduced synthesis temperature and easy operation.

Inactive Publication Date: 2007-10-17
JINGDEZHEN CERAMIC INSTITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In U.S. Patent US005656328, although the synthesis temperature was reduced to 900°C by adding NaF and NaCl, the Zr(OPr n ) 4 and Si(OAc) 4 The price is expensive and not easy to obtain, so it is difficult to apply to industrial production

Method used

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  • Method of synthesizing zirconium silicate powder at low temperature by unhydrolyzed sol-gel method
  • Method of synthesizing zirconium silicate powder at low temperature by unhydrolyzed sol-gel method
  • Method of synthesizing zirconium silicate powder at low temperature by unhydrolyzed sol-gel method

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Experimental program
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Embodiment 1

[0019] Si(OC 2 h 5 ) 4 (chemically pure), anhydrous ZrCl 4 (industrial pure) is the precursor, LiF (chemically pure) is the mineralizer, and dichloromethane is the solvent (CH 2 Cl 2 , chemically pure), 0.036molSi(OC 2 h 5 ) 4 , 0.0108molLiF uniformly mixed at room temperature, 0.03mol anhydrous ZrCl 4 with 30mlCH 2 Cl 2 Mix evenly at room temperature, then mix the two mixtures with each other, stir on a magnetic stirrer at room temperature for 10 minutes, continue heating and stirring at 65°C for 20 minutes, and then place them in an oil bath at 110°C for 12 hours under reflux to obtain a transparent precursor sol. Dry the sol in an oven at 35°C to obtain dry glue, and finally crush and calcinate the dry glue. The calcination system is: before the solvent is evaporated at 350°C, the heating rate is 4°C / min, and then it is raised to 700°C at 8°C / min , heat preservation 60min, the synthesized zirconium silicate powder is shown in accompanying drawing 1.

Embodiment 2

[0021] Si(OC 2 h 5 ) 4 (chemically pure), anhydrous ZrCl 4 (industrial pure) is a precursor, and LiF (chemically pure) is a mineralizer. The consumption of each raw material is the same as that of the preparation process and Example 1, but the solvent used is ethanol (chemically pure), and the drying temperature is 80 ° C. Synthetic See accompanying drawing 2 for zirconium silicate powder.

Embodiment 3

[0023] Si(OC 2 h 5 ) 4 (chemically pure), anhydrous ZrCl 4 (industrial pure) is the precursor, LiF (chemically pure) is the mineralizer, and 0.036molSi(OC 2 h 5 ) 4 Mix evenly with 0.0108mol LiF, then add 0.03mol anhydrous ZrCl 4 Add Si(OC 2 h 5 ) 4 and LiF in a mixed solution, placed on a magnetic stirrer at room temperature and stirred for 10 minutes to obtain a sol, and the sol was heated and stirred at 65°C for 20 minutes, and then placed in an oil bath at 110°C for reflux heating for 12 hours to obtain a dry glue, and finally The dry rubber was crushed and calcined, and the calcining system was as follows: the heating rate was 4°C / min before 350°C, and then raised to 700°C at 8°C / min, and kept for 30 minutes. The synthesized zirconium silicate powder is shown in Figure 3.

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Abstract

The invention discloses a method for synthesizing zirconium silicate powder in low temperature with a non-hydrolytic sol-gel method. Commercially pure non-aqueous zirconium chloride and orthosilicate ethyl ester are used as the raw materials of the precursor, LiF or MgF2 is the mineralizer and dichloromethane or ethanol is added in as the solvent. The precursor raw materials, the mineralizer and the solvent are prepared in proportion to form a precursor sol, which is back washed and dried to produce zirconium silicate dry gel which is further smashed and calcined to form the zirconium silicate powder at the low temperature of 700 to 850 degree. Compared with the current techniques, the invention is characterized in lower temperature for forming the zirconium silicate powder, simpler process, convenient operation and the using the commercially pure zirconium chloride as the raw material is more suitable for industrialization production.

Description

technical field [0001] The invention relates to a method for synthesizing zirconium silicate powder at low temperature by a non-hydrolytic sol-gel method. Background technique [0002] Zirconium silicate is an important high-temperature inorganic non-metallic material with many excellent properties. Such as good thermal stability, low thermal conductivity, small expansion coefficient, and its strength does not decay at a high temperature of 1400 ° C. At the same time, sintered zirconium silicate has better thermal shock resistance than mullite and zirconia. These properties make Zirconium silicate has become an important candidate material for high-temperature structural ceramics. In the traditional ceramic industry, zirconium silicate can not only be used as an opacifying agent and whitening agent to improve the opacifying effect and whiteness of ceramics, but also as a matrix material for zirconium-based pigments. Due to the super stability of z...

Claims

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Application Information

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IPC IPC(8): C01B33/20C04B35/16C04B35/48C04B35/624
Inventor 江伟辉周艳华周健儿魏恒勇顾幸勇朱小平
Owner JINGDEZHEN CERAMIC INSTITUTE
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