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Preparation method of zirconium fluoride

A technology of zirconium fluoride and zirconium tetrafluoride, which is applied in the field of preparation of zirconium fluoride, can solve the problems of high raw material cost and complicated process, and achieve the effect of simple preparation method, wide sources and low cost

Active Publication Date: 2014-04-09
贵州万方铝化科技开发有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above method has the problems of high cost of raw materials and complicated process

Method used

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  • Preparation method of zirconium fluoride
  • Preparation method of zirconium fluoride
  • Preparation method of zirconium fluoride

Examples

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preparation example Construction

[0025] The embodiment of the present invention provides a preparation method of zirconium fluoride, comprising:

[0026] mixing the zirconium-containing substance with the fluoride to obtain a mixture;

[0027] The mixture is reacted to obtain gaseous zirconium tetrafluoride and solid oxide;

[0028] Gas-solid separation to obtain gaseous zirconium tetrafluoride;

[0029] Wherein, the zirconium-containing substances include: zirconium-containing minerals or zirconium oxide-containing wastes.

[0030] Zirconium-containing substances (including zirconium-containing minerals or zirconium oxide-containing wastes) are used as raw materials, which have a wide range of sources and low cost; the zirconium in these raw materials is a fluorine-friendly substance, and after contacting with fluoride, it preferably reacts with fluorine to generate Zirconium tetrafluoride and other solid oxides can be separated by gas-solid separation to obtain zirconium tetrafluoride. Therefore, the pre...

Embodiment 1

[0059] Example 1: Preparation of high-purity ZrF with zircon sand and NaF as raw materials 4

[0060] The zircon sand and NaF are mixed uniformly, the average particle size of silicon-containing metal oxide or silicon-containing mineral and fluoride is about 0.3 mm, and the mass percentage of NaF in the obtained mixture is 30%. The mixture was calcined at 910 °C for 3 hours to form Na 2 O, SiF 4 and ZrF 4 , SiF 4 , ZrF 4 At high temperature, it is gaseous and escapes from solid. The zirconium tetrafluoride and silicon tetrafluoride generated in the reactor are separated by gas-solid to obtain high-purity zirconium tetrafluoride and silicon tetrafluoride. Zirconium tetrafluoride. The reaction equation is as follows:

[0061] ZrO 2 +4NaF→ZrF 4 +2Na 2 O

[0062] SiO 2 +4NaF→2Na 2 O+SiF 4

Embodiment 2

[0063] Example 2: With baddeleyite and AlF 3 Preparation of high-purity ZrF as raw material 4

[0064] Combining baddeleyite with AlF 3 Mix well, baddeleyite zircon and AlF 3 The average particle size is about 0.9mm, and the AlF in the obtained mixture 3 The mass percentage is 50%. The mixture was calcined at 1000°C for 7 hours to form Al 2 O 3 and ZrF 4 , ZrF 4 It is gaseous at high temperature and escapes from solid. The zirconium tetrafluoride and silicon tetrafluoride generated in the reactor are separated by gas-solid to obtain high-purity zirconium tetrafluoride and silicon tetrafluoride. Zirconium tetrafluoride. The reaction equation is as follows:

[0065] 3ZrO 2 +4AlF 3 ·3H 2 O→2Al 2 O 3 +3ZrF 4 +12H 2 O

[0066] 3SiO 2 +4AlF 3 ·3H 2 O→2Al 2 O 3 +3SiF 4 +12H 2 O

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Abstract

The invention relates to the field of chemical industry and specifically relates to a preparation method of zirconium fluoride. The preparation method of zirconium fluoride comprises the following steps: mixing a zirconium-containing substance with a fluoride to obtain a mixture; reacting the mixture to obtain gaseous zirconium tetrafluoride and a solid oxide; carrying out gas-solid separation to obtain gaseous zirconium tetrafluoride, wherein the zirconium-containing substance comprises zirconium-containing minerals or scrap materials containing zirconium oxide. The preparation method of zirconium fluoride provided by the embodiment of the invention is low in cost and is simple.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of zirconium fluoride. Background technique [0002] Zirconium fluoride is a white solid, slightly soluble in water, easily soluble in HF, hydrated zirconium fluoride monohydrate and zirconium fluoride trihydrate. There are two crystal forms of zirconium tetrafluoride: α-type and β-type, and those synthesized at temperatures below 450 °C are α-ZrF 4 , when the temperature reaches above 450℃, it will transform into β~ZrF 4 . It sublimates at high temperature, with a sublimation temperature of 905°C. [0003] The preparation methods of anhydrous zirconium tetrafluoride mainly include ammonium fluorozirconate decomposition method, zirconium dioxide, ammonium hydrogen fluoride calcination method and hydrated zirconium tetrafluoride dehydration method. Decomposition of ammonium fluorozirconate with ZrOCl 2 ·8H 2 O is the raw material, and ammonia water is ad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/04
Inventor 龚亚云林乐洪章林李丹阳刘瑞
Owner 贵州万方铝化科技开发有限公司
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