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Preparation of refined zirconium tetrachloride

A technology of refined zirconium tetrachloride and chlorine gas, applied in zirconium halide and other directions, can solve the problems of poor operating environment, low recovery rate, high power consumption of refined zirconium tetrachloride, improve recovery rate, avoid pollution and save energy The effect of power consumption

Active Publication Date: 2011-08-24
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
  • 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 under the 325 mesh sieve, the petroleum coke is crushed under the 160 mesh sieve, the desiliconized zirconium and petroleum coke are mixed in a weight ratio of 100:20, and the total material The weight is 1 ton, and then it is added into a reaction kettle with a concentration of 6moL / L hydrochloric acid, and the volume of hydrochloric acid in the kettle is 2m 3 , at a temperature of 40°C, stirring and reacting for 1 hour; the acid leaching mixture was centrifuged, washed with water until neutral, and dried in a mixing dryer for 3 hours, and then the dry material was continuously added to a bag type bag equipped with a quartz cloth nickel skeleton. In the boiling chlorination furnace with 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 obtained content is 98.9% refined...

Embodiment 2

[0027] The boiling chlorination method produces the preparation method of refined zirconium tetrachloride, and the desiliconized zirconium is crushed under the 400 mesh sieve, and the graphite is crushed to the 100 mesh sieve powder, and the desiliconized zirconium and the graphite are mixed in a weight ratio of 100:18, and the total weight of the material is 1 ton, and then added to the reaction kettle with a concentration of 4moL / L sulfuric acid, the volume of sulfuric acid in the kettle is 1.5m 3 , at a temperature of 50°C, stirring and reacting for 2 hours; the acid leaching mixture was separated by solid-liquid centrifugation, washed with water until neutral, and dried in a mixing dryer for 4 hours, and then the dry material was continuously added to the nickel skeleton equipped with quartz cloth React with chlorine gas at 820°C for 20 hours in the boiling chlorination furnace of bag filter, and the flow rate of chlorine gas is 0.7-0.8M 3 / hour, the obtained content is 9...

Embodiment 3

[0029] The preparation method of producing refined zirconium tetrachloride by boiling chlorination method, crushing desiliconized zirconium under 400 mesh sieve, crushing petroleum coke into fine powder of 200 mesh sieve, mixing desiliconized zirconium and petroleum coke in a weight ratio of 100:19, and the material The total weight is 1 ton, and then it is added into a reaction kettle with a concentration of 4moL / L nitric acid, and the volume of nitric acid in the kettle is 1m 3 , at 35°C, stirring and reacting for 3 hours; the acid leaching mixture was centrifuged from solid to liquid, washed with water until neutral, dried in a mixing dryer for 3 hours, and then the dry 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 for 24 hours at 870°C, and the flow rate of chlorine gas is 0.7-0.8M 3 / hour, the obtained content is 99.2% refined zirconium tetrachloride.

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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<3> / hour to 1.0 M<3> / 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 zirconium halide, in particular to the method for purifying and producing refined zirconium tetrachloride by boiling chlorination. Background technique [0002] The existing refined zirconium tetrachloride used to produce sponge zirconium is the crude zirconium tetrachloride produced by chlorination in an electric furnace, through low-temperature degassing (removing low-boiling SiCl 4 、TiCl 4 , AlCl 3 and other impurities), hydrogen reduction (with H 2 FeCl 3 Reduction to FeCl with high boiling point 2 ), high temperature degassing (remove AlCl 3 ), condensation (collecting zirconium tetrachloride) and other processes to produce. The disadvantages of this method are long process flow, high power consumption, low metal recovery rate and high production cost. [0003] The company's application number: 200710010730.X name: "a preparation method of zirconium tetrachloride" patent application, is to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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