Preparation method of zirconium tetrachloride

A technology of zirconium tetrachloride and zirconium oxide, which is applied in the direction of zirconium halide, etc., can solve the problems of shortening the process flow, impact on product yield and purity, and large difference in product quality, so as to achieve short process flow, shorten production process flow, and improve The effect of recovery

Inactive Publication Date: 2007-10-03
CHAOYANG BAISHENG TITANIUM IND CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The advantage of this method is that it saves the ball coking process, shortens the process flow, and saves electric energy; but the disadvantage is that under the above process conditions, the

Method used

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  • Preparation method of zirconium tetrachloride
  • Preparation method of zirconium tetrachloride

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Experimental program
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Embodiment 1

[0030] The method for producing zirconium tetrachloride with boiling furnace, first zircon sand (ZrSiO 4 ) is desiliconized in an electric arc furnace in advance, the weight percentage of desiliconized zirconia is greater than 92%, and SiO in zirconia 2 The content should be less than 0.5% by weight. Desiliconized zirconium is crushed into 160-325 mesh fine powder, mixed with 100-200 mesh petroleum coke to increase uniformity, and the weight ratio is 100:18; desiliconized zirconia and petroleum coke fine powder are pre-heated at a temperature of 80-200°C Dehydration treatment for 1-2 hours; when the furnace temperature rises to 900±5°C, add the dehydrated material into the fluidized furnace at a feeding rate of 100-150kg / hour, and feed chlorine at a rate of 0.67M 3 / hour, and react at a temperature of 900~1100±5°C for 20~21 hours. The reacted material is cooled to 200±10°C for 8-10 hours, and then continued to cool to 20±5°C for 3-5 hours. The finally discharged hydrochlori...

Embodiment 2

[0032] The raw materials after dehydration treatment are ready for use. Raise the boiling furnace temperature from 0 to 900°C for 2 to 3 hours. When the furnace temperature reaches 900°C, add the dehydrated material at a feeding rate of 150kg / hour, and feed chlorine gas at the same time. The rate of chlorine gas is 0.85M 3 / hour, react at 900-1100±5°C for 20-21 hours, and the zirconium tetrachloride produced is condensed by a condenser to obtain the product. Other conditions are with embodiment 1.

Embodiment 3

[0034] Dehydrate the desiliconized zirconia and petroleum coke powder at 150-200°C for 1.5 hours; raise the boiling furnace temperature to 0-900°C for 2-3 hours, add the dehydrated materials when the furnace temperature rises to 900°C, and the feeding speed It is 120kg / hour, feed chlorine gas at the same time, the flow rate is 0.8M 3 / hour, reacted at 900~1100±5°C for 20~21 hours, and other conditions were the same as in Implementation 1.

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Abstract

A process for preparing ZrCl4 includes such steps as proportionally mixing fine desiliconized zirconium oxide powder with petroleum coke powder, dewatering, loading the mixture into boiling furnace at 900 +/- 5 deg.C while filling chlorine gas, chlorinating reaction at 900-1100 +/- 5 deg.C for 20-21 hr, cooling to 200 +/- 10 deg.C for 8-10 hr, and cooling to 20 +/- 5 deg.C for 3-5 hr.

Description

technical field [0001] The invention relates to a method for preparing zirconium tetrachloride by boiling chlorination, in particular to a method for preparing zirconium tetrachloride by electromelting desilication of zirconia. Background technique [0002] Zirconium is a rare metal, and its compounds have many unique properties, such as the nucleation properties of zirconium, the strong affinity of zirconium atoms to oxidation, low ignition point and high combustion temperature of sponge zirconium, and easy reaction with gas to form stable compounds. Some are used in the nuclear industry, rocket missiles, alloy additives, getters, magnetic fluid power generation and optical fiber communications, and are also widely used in ceramics, papermaking, refractories and other industries. The existing method for producing zirconium tetrachloride is to produce zircon sand and petroleum coke through carbonization, and the chemical reaction in this process is:...

Claims

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Application Information

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IPC IPC(8): C01G25/04
Inventor 刘远清
Owner CHAOYANG BAISHENG TITANIUM IND CO LTD
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