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Novel method for preparing zirconium tungstate powder

A production method, technology of zirconium tungstate, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve the problems of harsh process conditions, long synthesis time, cumbersome steps, etc., and achieve the effect of high purity

Inactive Publication Date: 2011-09-21
SHANGHAI JIAHAN NEW MATERIAL TECH
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Problems solved by technology

Therefore, a single ZrW was synthesized by a solid-phase method 2 o 8 Very difficult
Combustion synthesis method, combustion synthesis method to synthesize ZrW 2 o 8 , the reaction speed is relatively fast, but the product is impure, and harmful nitrogen oxides are released during the reaction process, causing environmental pollution and not suitable for industrial applications
Low temperature synthesis method, low temperature synthesis method refers to low temperature synthesis of ZrW 2 o 8 Although this method avoids high-temperature sintering, its steps are cumbersome, the process conditions are harsh, and its synthesis time is long, so it is not suitable for industrial mass production
Wet chemistry combined with microwave calcination synthesis method, wet chemistry method combined with microwave calcination process to synthesize ZrW 2 o 8 , the reaction time was shortened, but the temperature of the synthesis reaction was only reduced to a certain extent

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Embodiment Construction

[0009] The present invention is described further in conjunction with accompanying drawing, and the manufacturing technology of this device is very clear to those skilled in the art.

[0010] The process steps are: with ZrO 2 and WO 3 As raw material, according to ZrO 2 : WO 3 =1:2 stoichiometric ratio weighing. ZrO 2 and WO 3 Put it into a resin ball mill jar, add absolute ethanol as a solvent, and ball mill in a ball mill for 8 hours. Let it stand for precipitation, pour off the upper layer of clear solvent, dry it in an oven, take it out and grind it into powder. Put the powder in a quartz crucible, heat it at 600°C for 4 hours, take it out, put it in the air to cool down; grind it for 40 minutes; adjust the temperature to 800°C and heat it for 8 hours, take it out and grind it for 40 minutes after cooling in the furnace; then heat it at 900°C for 12 hours, and cool it in the furnace Finally, take it out and grind for 40min; put ZrO in a mold with a diameter of 60mm ...

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Abstract

The invention relates to a novel method for preparing zirconium tungstate powder, which is characterized by comprising the following process steps of: weighing in a stoichiometric ratio of ZrO2 to WO3 of 1:2, putting the ZrO2 and WO3 into a resin ball mill, adding absolute ethanol serving as a solvent, performing ball milling in a ball mill for 8 hours, standing for sedimentation, removing an upper-layer clear solvent, drying in an oven, putting powder into a quartz crucible, heating at 600DEG C for 4 hours, taking out, and cooling in the air; grinding for 40 minutes; regulating the temperature to be 800DEG C, heating for 8 hours, cooling together with a furnace, taking out, and grinding for 40 minutes; heating at 900DEG C for 12 hours, cooling together with a furnace, taking out, and grinding for 40 minutes; and putting ZrO2 and WO3 mixed powder into a mold with the diameter of 60mm, pressing under the pressure of 125MPa into a round sheet, and keeping the temperature of 1,220DEG C for 3 hours. Compared with the prior art, the novel method has the advantages that: the grain size is 0.5-1mu m, the purity is high, and the average coefficient of linear expansion is -5.33*10<-6> / K in a section of 20-700DEG C.

Description

technical field [0001] The invention relates to a novel method for preparing zirconium tungstate powder. Background technique [0002] Currently, ZrW 2 o 8 The production methods of the powder are as follows: oxide direct synthesis method, ZrO 2 and WO 3 Mix according to appropriate proportions, ball mill in a planetary ball mill for 24 hours, place in a sealed platinum kumquat pot and sinter at 1200°C for more than 48 hours, and then quench to obtain ZrW 2 o 8 Powder, the solid state method has a high sintering temperature and takes a long time, and because WO 3 The volatility is strong, usually get ZrW 2 o 8 and WO 3 mixture. Therefore, a single ZrW was synthesized by a solid-phase method 2 o 8 Very difficult. Combustion synthesis method, combustion synthesis method to synthesize ZrW 2 o 8 , the reaction speed is relatively fast, but the product is impure, and harmful nitrogen oxides are released during the reaction process, causing environmental pollution an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00
Inventor 李昊
Owner SHANGHAI JIAHAN NEW MATERIAL TECH
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