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Method for producing high-purity zirconium oxychloride and co-producing silicon tetrachloride through zircon sand boiling chlorination method

A technology of boiling chlorination and pure zirconium oxychloride, which is applied in the direction of zirconium halide, silicon halide compound, halosilane, etc., can solve the problem of high production cost, increased production cost, and product quality that cannot reach high-purity zirconium oxychloride Quality standards and other issues to achieve the effect of low production cost and good product quality

Active Publication Date: 2015-08-05
赤峰盛森硅业科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Zirconium oxychloride products are widely used and are the basic raw materials of zirconium chemical industry. The market demand is large. In 2014, it reached 240,000 tons. However, domestic zirconium oxychloride is produced by "alkali fusion method". Pollution control is very difficult, and the product quality cannot meet the quality standards of high-purity zirconia oxychloride. High-grade zirconia enterprises need to extract or recrystallize the purchased zirconia oxychloride to reduce the impurity content before proceeding with production, resulting in The production cost increases, and the national zirconium oxychloride enterprises are also actively carrying out technological innovation to reduce production costs, improve product quality, and improve environmental quality

Method used

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  • Method for producing high-purity zirconium oxychloride and co-producing silicon tetrachloride through zircon sand boiling chlorination method
  • Method for producing high-purity zirconium oxychloride and co-producing silicon tetrachloride through zircon sand boiling chlorination method
  • Method for producing high-purity zirconium oxychloride and co-producing silicon tetrachloride through zircon sand boiling chlorination method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Process route see figure 1 , specifically prepared as:

[0042] 1) Chlorination reaction

[0043] The raw material zircon sand, calcined petroleum coke and silicon carbide are added to the mixer according to the mass ratio of zircon sand: calcined coke: silicon carbide = 1:0.22:0.34, and the materials are mixed, and then added to the front of the furnace The silo is continuously fed into the chlorination furnace through a screw conveyor.

[0044]Chlorine gas is fed into the bottom of the chlorination furnace, and the weight of the feed is zircon sand: chlorine gas = 1: 2.78. The chlorine gas enters the reaction section through the distributor to react with the raw materials. The reaction temperature is controlled at 1170 °C, and the furnace pressure is controlled within 3000 Pa. At the same time Determine the slag removal time of the chlorination furnace according to the furnace pressure, and control the chlorine flow rate at 0.009m / s, so that the reaction can proceed...

Embodiment 2

[0081] In Example 1, the silicon tetrachloride-containing tail gas obtained by the cooling treatment of the quencher enters the gas-solid separation of the gas, and the solid obtained is a zirconium tetrachloride solid, which enters the purifier for purification, then enters the hydrolysis tank through a screw conveyor, and adds Pure water, evaporating acid, and washing liquid are used for hydrolysis, and the amount of material added is zirconium tetrachloride

[0082] Solid: pure water: evaporating acid: washing liquid is 0.91:2.35:0.72:1.00 (weight ratio), control the hydrolysis temperature at 40-50°C, the speed of the mixer in the hydrolysis tank is 100r / min, and the concentration of zirconium in the hydrolysis solution is 100±10g / l, use a pump to send it into a chamber filter press to filter out the entrained solids to obtain a purified zirconium oxychloride solution, and the washing solution during hydrolysis can be recycled and reused. Wherein, the evaporating acid is 2...

Embodiment 3

[0095] The primary mother liquor prepared in the above-mentioned embodiment 1 or embodiment 2 is subjected to pressurized evaporation, and the primary crystallization mother liquor enters a double-heating external circulation graphite evaporator, uses steam to heat the mother liquor, and uses the secondary steam of the evaporator as a heat source to preheat the mother liquor solution , control the vapor pressure at 0.3MPa-0.7MPa, and the secondary pressure at 0.2MPa-0.3MPa, so that the concentration of hydrochloric acid in the evaporating liquid is 17-19%, and the concentration of zirconia is 190±10g / l. Crystallization tank, crystallization at 25°C for 20h, the crystallized oxychlorination solution is filtered through a belt filter, and the filtered crystals are washed with 18% hydrochloric acid to obtain zirconium oxychloride, and the obtained filtrate is the secondary mother liquor.

[0096] The obtained zirconium oxychloride crystals are re-dissolved as crystal seeds, and t...

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Abstract

The present invention relates to a high-purity zirconium oxychloride production method, specifically to a method for producing high-purity zirconium oxychloride and co-producing silicon tetrachloride through a zircon sand boiling chlorination method. The method comprises: adopting zircon sand, a reducing agent and a stabilizer, introducing chlorine gas into a chlorination furnace at a gas velocity of 0.07-0.12 m / s, carrying out a boiling chlorination reaction at a temperature of 1150-1200 DEG C to generate zirconium tetrachloride and silicon tetrachloride, carrying out gas-solid separation, and carrying out hydrolysis and purification on the separated solid and carrying out evaporation, crystallization and separation on the zirconium oxychloride solution so as to obtain the high-purity zirconium oxychloride and the co-produced product silicon tetrachloride, wherein a mass ratio of the zircon sand to the reducing agent to the stabilizer to the chlorine gas is 0.9-1.1:0.2-0.3:0.3-0.4:2.7-2.8. The product produced through the method of the present invention has characteristics of good quality, low production cost, and no polluting.

Description

technical field [0001] The invention relates to a production method of high-purity zirconium oxychloride, in particular to a method for producing high-purity zirconium oxychloride and co-production of silicon tetrachloride by boiling chlorination of zircon sand. Background technique [0002] Zirconium oxychloride products are widely used and are the basic raw materials of zirconium chemical industry. The market demand is large. In 2014, it reached 240,000 tons. However, domestic zirconium oxychloride is produced by "alkali fusion method". Pollution control is very difficult, and the product quality cannot meet the quality standards of high-purity zirconia oxychloride. High-grade zirconia enterprises need to extract or recrystallize the purchased zirconia oxychloride to reduce the impurity content before proceeding with production, resulting in With the increase of production cost, zirconium oxychloride enterprises across the country are also actively carrying out technologic...

Claims

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Application Information

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IPC IPC(8): C01G25/04C01B33/107
Inventor 郭志斌李宏彬李毅南董法强
Owner 赤峰盛森硅业科技发展有限公司
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