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Method for low-temperature synthesis of zirconium silicate powder through non-hydrolytic sol-gel reaction by using zirconium acetate as zirconium source

A non-hydrolysis, zirconium silicate technology, applied in chemical instruments and methods, silicon compounds, non-metallic elements, etc., can solve problems such as unsatisfactory crystal shape development, high synthesis temperature, obvious agglomeration of zirconium silicate powder, etc., to achieve Perfect crystal development, lower synthesis temperature, and less agglomeration

Inactive Publication Date: 2010-10-27
JINGDEZHEN CERAMIC INSTITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is to use ZrCl 4 As a zirconium source, although zirconium silicate powder was synthesized at low temperature, the synthesis temperature is still high, and the synthesized zirconium silicate powder still has obvious agglomeration phenomenon, and the crystal form development is not ideal, and ZrCl 4 Another disadvantage of making zirconium source is that when using anhydrous low-carbon alcohol as solvent, ZrCl 4 React with low-carbon alcohol to release a large amount of HCl corrosive gas

Method used

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  • Method for low-temperature synthesis of zirconium silicate powder through non-hydrolytic sol-gel reaction by using zirconium acetate as zirconium source
  • Method for low-temperature synthesis of zirconium silicate powder through non-hydrolytic sol-gel reaction by using zirconium acetate as zirconium source
  • Method for low-temperature synthesis of zirconium silicate powder through non-hydrolytic sol-gel reaction by using zirconium acetate as zirconium source

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Experimental program
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Effect test

Embodiment 1

[0024] Si(OC 2 h 5 ) 4 (chemically pure), anhydrous zirconium acetate (chemically pure) as the precursor, LiF (chemically pure) as the mineralizer, dichloromethane as the solvent (CH 2 Cl 2 , chemically pure), 0.036molSi(OC 2 h 5 ) 4 After uniform mixing with 0.008mol LiF at room temperature, add 0.03mol anhydrous zirconium acetate, stir on a magnetic stirrer for 15 minutes to obtain a precursor sol, add 35ml of dichloromethane solvent, stir magnetically for 10 minutes, and then pour into 100ml of the liner to form polytetrafluoroethylene In the pressure bomb of vinyl fluoride, the pressure bomb was placed in a constant temperature oven at 110°C to react for 24 hours. After the reaction was completed, it was naturally cooled to room temperature to obtain a white zirconium silicate solid wet gel. Dry the zirconium silicate solid wet gel in a constant temperature oven at 60°C for 6 hours to obtain off-white zirconium silicate xerogel, and zirconium silicate xerogel is pulv...

Embodiment 2

[0026] With 0.036mol Si(OC 2 h 5 ) 4 (chemically pure), 0.026mol anhydrous zirconium acetate (chemically pure) is the precursor, 0.005mol LiF (chemically pure) is the mineralizer, add 38ml ethanol (CH 3 CH 2 OH, chemically pure) as the solvent, zirconium silicate xerogel was incubated at 650°C for 20min, and other technological processes were the same as in Example 1, and the synthetic zirconium silicate powder was shown in the attached Figure 4 .

Embodiment 3

[0028] With 0.036mol Si(OC 2 h 5 ) 4 (chemically pure), 0.028mol anhydrous zirconium acetate (chemically pure) is the precursor, 0.009mol LiF (chemically pure) is the mineralizer, and 50ml of n-butanol (CH 3 CH 2 CH 2 CH 2 OH, chemically pure) is the solvent, the reaction temperature of the pressure bomb is 130 ℃, and the reaction time is 36h. Other technological processes are the same as in Example 1. The synthetic zirconium silicate powder is shown in the appendix Figure 5 .

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Abstract

The invention discloses a method for the low-temperature synthesis of zirconium silicate powder through non-hydrolytic sol-gel reaction by using zirconium acetate as a zirconium source. The method comprises the following steps of: by using ethyl orthosilicate and anhydrous zirconium acetate as precursors, LiF or MgF2 as a mineralizer, and chloroalkane or anhydrous lower alcohol as a solvent, mixing the precursors, the mineralizer and the solvent in proportion to prepare precursor mixed solution; feeding the solution into a hydrothermal synthesis reactor to perform the thermal treatment to form a zirconium silicate solid wet gel; and drying, grinding and sintering the zirconium silicate solid wet gel at the temperature of 650 DEG C to obtain the zirconium silicate powder with less powder agglomeration and perfect crystal form growth. The method has the advantages of further reducing the synthesis temperature of zirconium silicate and avoiding the emission of HCl corrosive gas along with simple process and convenient operation.

Description

technical field [0001] The invention belongs to the technical field of silicate material manufacture, and relates to a method for synthesizing zirconium silicate powder at low temperature through non-hydrolytic sol-gel reaction using zirconium acetate as a zirconium source. Background technique [0002] Zirconium silicate has high melting point (2500°C), low thermal conductivity (3.5W / m·K at 1000°C) and small expansion coefficient (4.1×10 -6 / °C) and other characteristics, the thermal shock resistance of zirconium silicate ceramics is better than that of mullite and zirconia, and its flexural strength does not decay at 1400°C. Therefore, zirconium silicate is an ideal candidate for the preparation of high-temperature structural ceramics Material. In the traditional ceramic industry, zirconium silicate is used as a high-quality opacifying agent and whitening agent for ceramic glazes due to its high refractive index, and is also used as a ceramic pigment carrier and high-grad...

Claims

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Application Information

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IPC IPC(8): C01B33/20
Inventor 江伟辉张缇朱庆霞刘健敏谭训彦包镇红虞澎澎苗立锋
Owner JINGDEZHEN CERAMIC INSTITUTE
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