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Preparation method of zirconium silicate powder

A technology for zirconium silicate and powder, which is applied in the field of sol-gel-assisted ultrasonic sonochemical method for preparing zirconium silicate powder, can solve the problems of high preparation temperature and short preparation time, and achieves low reaction temperature, short cycle, and high particle size. The effect of narrow diameter distribution

Active Publication Date: 2012-07-11
路亚科消防车辆制造有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Jiang Weihui et al. (Chinese patent 200710108375.X) used commercially pure anhydrous zirconium tetrachloride and ethyl orthosilicate as precursors, and synthesized it by non-hydrolytic sol-gel method at 700°C for 15 minutes by selecting a suitable mineralizer. Zirconium silicate powder, although the preparation time of this method is short, the preparation temperature is relatively high

Method used

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  • Preparation method of zirconium silicate powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1) Separately analyze pure ZrOCl 2 ·8H 2 O, ethyl orthosilicate (CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 ), NaF was added into distilled water and stirred evenly to make ZrOCl 2 The molar concentration is the precursor A of 4mol / L, wherein ZrOCl 2 ·8H 2 O:CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 : The molar ratio of NaF is 2: 7: 1;

[0016] 2) Add hydrochloric acid dropwise to the precursor solution A to adjust the pH value to 1, and keep stirring to form sol B;

[0017] 3) Put sol B into the Erlenmeyer flask, then place the Erlenmeyer flask into an ultrasonic generator with a natural frequency of 80kHz, turn on the ultrasonic generator, and react for 12 hours at 60°C with an ultrasonic power of 300W. cool to room temperature;

[0018] 4) The reactants were taken out, collected by suction filtration through filter paper, washed with deionized water and absolute ethanol respectively, and dried in an electric blast drying oven at 40° C. to obtain zirconium silicate powder.

Embodiment 2

[0020] 1) Separately analyze pure ZrOCl 2 ·8H 2 O, ethyl orthosilicate (CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 ), NaF was added into distilled water and stirred evenly to make ZrOCl 2 The molar concentration is the precursor A of 6mol / L, wherein ZrOCl 2 ·8H 2 O:CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 : The molar ratio of NaF is 4: 4: 2;

[0021] 2) Add hydrochloric acid dropwise to the precursor solution A to adjust the pH value to 4.5, and keep stirring to form sol B;

[0022] 3) Put sol B into the Erlenmeyer flask, then place the Erlenmeyer flask into an ultrasonic generator with a natural frequency of 80kHz, turn on the ultrasonic generator, and react for 8 hours at 80°C with an ultrasonic power of 700W. Natural cooling to room temperature;

[0023] 4) The reactants were taken out, collected by suction filtration through filter paper, washed with deionized water and absolute ethanol respectively, and dried in an electric blast drying oven at 60° C. to obtain zirconium silicate po...

Embodiment 3

[0025] 1) Separately analyze pure ZrOCl 2 ·8H 2 O, ethyl orthosilicate (CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 ), NaF was added into distilled water and stirred evenly to make ZrOCl 2 The molar concentration is the precursor A of 2mol / L, wherein ZrOCl 2 ·8H 2 O:CH 3 CH 2 OSi(OCH 2 CH 3 ) 3 : The molar ratio of NaF is 6: 1: 3;

[0026] 2) Add hydrochloric acid dropwise to the precursor solution A to adjust the pH value to 6.5, and keep stirring to form sol B;

[0027] 3) Put sol B into the Erlenmeyer flask, then place the Erlenmeyer flask into an ultrasonic generator with a natural frequency of 80kHz, turn on the ultrasonic generator, and react for 5 hours at 100°C with an ultrasonic power of 1000W. cool to room temperature;

[0028] 4) The reactants were taken out, collected by suction filtration through filter paper, washed with deionized water and absolute ethanol respectively, and dried in an electric blast drying oven at 80° C. to obtain zirconium silicate powder.

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Abstract

The invention discloses a preparation method of zirconium silicate powder. The preparation method comprises the steps: adding ZrOCl2.8H2O, tetraethyl orthosilicate and NaF into distilled water to obtain a precursor solution A, adding hydrochloric acid into the precursor solution A to regulate a pH value to be 1-6.5 to obtain sol B, placing the sol B into an ultrasonic generator for ultrasonic reaction, and naturally cooling to room temperature after the reaction is finished; and taking out a reactant, leaching and collecting the reactant by using filter paper, then washing the reactant by using deionized water and absolute ethyl alcohol respectively, and drying in an electrothermal blowing dry box to obtain the zirconium silicate powder. According to the invention, the zirconium silicate power with high quality can be prepared by using a sol-gel assisted ultrasonic acoustochemical method. Because the reaction is completed in a liquid phase, annealing crystallization treatment is not needed in a later stage; the preparation method has the advantages of simple technological equipment, low reaction temperature, short period and good repeatability; and the obtained zirconium silicate grains are narrow in grain size distribution and controllable in crystal form.

Description

technical field [0001] The invention belongs to the field of material chemical industry, and in particular relates to a method for preparing zirconium silicate powder by a sol-gel assisted ultrasonic sonochemical method. Background technique [0002] Zirconium silicate (ZrSiO 4 ) belongs to the tetragonal crystal system and is a silicate mineral with an island structure. Zirconium silicate can be used as a high-performance structural material (such as graphite, C / C composite materials and SiC structural ceramics, etc.) due to its high melting point, low thermal conductivity, low expansion coefficient, and excellent chemical and phase stability. High temperature oxidation resistant coating material. [0003] At present, the methods for preparing zirconium silicate crystals mainly include solid-state reaction method, precipitation method, hydrothermal method, and sol-gel method. The above methods generally require high temperature (such as 1300-1600°C for solid-state reacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/20
Inventor 曹丽云刘佳王敦强黄剑锋辛宇吴建鹏
Owner 路亚科消防车辆制造有限公司
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