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Preparation of refined zirconium tetrachloride

A technology of refined zirconium tetrachloride and zirconium tetrachloride, which is applied in the field of halide preparation, can solve the problems of high power consumption of refined zirconium tetrachloride, poor operating environment, low recovery rate, etc., so as to save power consumption , the effect of improving the recovery rate and avoiding pollution

Active Publication Date: 2009-07-22
朝阳东锆新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It solves the problems of high power consumption, low recovery rate, and poor operating environment in which crude zirconium tetrachloride produced by chlorination is purified by a purification furnace to produce refined zirconium tetrachloride in the existing method.

Method used

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  • Preparation of refined zirconium tetrachloride
  • Preparation of refined zirconium tetrachloride

Examples

Experimental program
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Effect test

Embodiment 1

[0025] The preparation method of producing refined zirconium tetrachloride by boiling chlorination method, the desiliconized zirconium is crushed to a 325 mesh screen, the petroleum coke is crushed to a 160 mesh screen, the desiliconized zirconium and the petroleum coke are mixed in a weight ratio of 100:20, and the total material The weight is 1 ton, then joins in the reactor that is housed with concentration and is 6moL / L hydrochloric acid, and the hydrochloric acid volume in the still is 2m 3 , at a temperature of 40 ° C, stirring and reacting for 1 hour; the acid leaching mixture is centrifuged, washed with water to neutrality, and dried in a mixing dryer for 3 hours. In the boiling chlorination furnace of the filter, react with chlorine gas at 850°C for 20 hours, and the flow rate of chlorine gas is 0.7~0.8M 3 / hour, the refined zirconium tetrachloride with a content of 98.9% was obtained.

Embodiment 2

[0027] The preparation method for producing refined zirconium tetrachloride by the boiling chlorination method is to crush the desiliconized zirconium to a 400-mesh sieve, crush the graphite to a 100-mesh sieve powder, and mix the desiliconized zirconium and graphite in a weight ratio of 100:18. The total weight of the material is 1 ton, then join in the reactor that is housed with concentration of 4moL / L sulfuric acid, and the volume of sulfuric acid in the still is 1.5m 3 , at a temperature of 50 ° C, stirring and reacting for 2 hours; the acid leaching mixture is centrifuged by solid-liquid, washed with water to neutrality, and dried in a mixing dryer for 4 hours, and the dried material is continuously added to the nickel skeleton equipped with quartz cloth. In the boiling chlorination furnace of the bag filter, the reaction is carried out with chlorine gas at 820 ° C for 20 hours, and the flow rate of chlorine gas is 0.7 ~ 0.8M 3 / hour, the refined zirconium tetrachloride ...

Embodiment 3

[0029] The preparation method of producing refined zirconium tetrachloride by boiling chlorination method, crushing desiliconized zirconium to 400 mesh sieve, crushing petroleum coke into 200 mesh sieve fine powder, mixing desiliconized zirconium and petroleum coke in a weight ratio of 100:19, the material Gross weight is 1 ton, then joins in the reactor that is housed with concentration and is 4moL / L nitric acid, and the nitric acid volume in the still is 1m 3 , at a temperature of 35 ° C, stirring and reacting for 3 hours; the acid leaching mixture was centrifuged by solid-liquid, washed with water to neutrality, dried in a mixing dryer for 3 hours, and then the dried material was continuously added to the nickel skeleton equipped with quartz cloth In the boiling chlorination furnace of the bag filter, react with chlorine gas at 870 ° C for 24 hours, and the flow rate of chlorine gas is 0.7 ~ 0.8M 3 / hour, the refined zirconium tetrachloride with a content of 99.2% was obtai...

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Abstract

The invention adopts a chemical method to remove impurities in raw materials, and a boiling chlorination method to prepare refined zirconium tetrachloride. The preparation method comprises the steps that: desilicated zirconium is ground into fine powder of 300 meshes to 500 meshes and then mixed with petrol coke or graphite of 50 meshes to 200 meshes according to the weight ratio of 100:16-20; then the mixture is added into a container which holds mineral acid with the use concentration of 3 mol / L to 7 mol / L, and reaction is carried out for 0.5 hour to 5 hours at the temperature ranging from 10 DEG C to 60 DEG C so as to remove the impurities; then, the reaction products are washed with water to be neutral, dried at the temperature of 70 DEG C to 120 DEG C and added into a boiling chlorination furnace which is provided with a filter; when the temperature inside the boiling chlorination furnace reaches 800 DEG C to 900 DEG C, chlorine with the flowing rate of 0.6 M / hour to 1.0 M / hour is led into the boiling chlorination furnace to react for 20 hours to 24 hours; and finally, refined zirconium tetrachloride with the content over 98 percent is obtained. Compared with the prior art, the preparation method has the advantages of eliminating the crude zirconium-tetrachloride purifying process with high energy consumption and low yield, shortening process flows, being beneficial to environmental protection and significantly reducing the production cost.

Description

technical field [0001] The invention belongs to the preparation method of halide of zirconium, and particularly relates to a method for producing refined zirconium tetrachloride by purifying by boiling chlorination method. Background technique [0002] The existing refined zirconium tetrachloride used for the production of sponge zirconium is the crude zirconium tetrachloride produced by chlorination in an electric furnace, through low-temperature degassing (removal of low-boiling SiCl 4 , TiCl 4 , AlCl 3 and other impurities), charged with hydrogen for reduction (with H 2 FeCl 3 Reduction to high boiling point FeCl 2 ), high temperature outgassing (remove AlCl 3 ), condensation (collection of zirconium tetrachloride) and other processes to produce. The disadvantage of this method is that the process flow is long, the power consumption is large, the metal recovery rate is low, and the production cost is high. [0003] The company's application number: 200710010730.X n...

Claims

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Application Information

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IPC IPC(8): C01G25/04
Inventor 刘远清刘忠权孙玉军刘景宇李庆彬
Owner 朝阳东锆新材料有限公司
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