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Zirconium tetrachloride purification method

A purification method and technology of zirconium tetrachloride, applied in zirconium halide and other directions, can solve the problems of low production capacity, dangerous hydrogen storage and use, low recovery rate, etc.

Active Publication Date: 2010-10-27
LIAONING HUAGAO NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problems of the above method are: 1. There is a certain risk in the storage and use of hydrogen. 2. It is difficult to separate the low boiling point impurities and adjust the output quality by manual deflation adjustment. 3. It cannot be continuously produced and the production capacity is very low. In addition to impurities, the recovery rate is low, only 90%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] First 6000kg crude ZrCl 4 Mix it with 1000kgNaCl and 1000kgKCl and add it into the molten salt furnace, heat it to 290°C to form 8 tons of eutectic molten salt with a low melting point;

[0013] Add 100kg of crude zirconium tetrachloride to the melt every hour, and continuously feed;

[0014] After the addition, pump 2200kg of molten salt into the evaporation furnace, and control the temperature of the evaporation furnace at 500-550°C to make the ZrCl 4 Evaporation is condensed and collected in the condenser;

[0015] Change the molten salt intermittently, return 220kg of molten salt from the evaporation furnace to the molten salt furnace every hour, and then use the pump to replenish 220kg of molten salt into the evaporation furnace, repeat this process, continuous evaporation in the evaporation furnace, continuous discharge, and the output reaches 770kg per 8 hours .

Embodiment 2

[0017] First 6400kg crude ZrCl 4 Mix it with 800kgNaCl and 800kgKCl and add it into the molten salt furnace, and heat it to 330°C to form 8 tons of eutectic molten salt with a low melting point;

[0018] Add 180kg of crude zirconium tetrachloride to the melt per hour, and continuously feed;

[0019] After the addition, pump 2000kg of melt into the evaporation furnace continuously, and the temperature of the evaporation furnace is controlled at 600-650°C to make the ZrCl 4 Evaporation is condensed and collected in the condenser;

[0020] Change the molten salt intermittently, return 360kg of molten salt from the evaporation furnace to the molten salt furnace every hour, and then use the pump to replenish 360kg of molten salt into the evaporation furnace. Repeat this process, continuous evaporation in the evaporation furnace, continuous discharge, and the output reaches 1380kg per shift of 8 hours.

Embodiment 3

[0022] First 6800kg crude ZrCl 4 Mix it with 600kgNaCl and 600kgKCl and add it into the molten salt furnace, heat it to 350°C to form 8 tons of eutectic molten salt with a low melting point;

[0023] Add 150 kg of crude zirconium tetrachloride to the melt per hour, and continuously feed;

[0024] After the addition, pump 1800kg of melt continuously into the evaporation furnace. The temperature of the evaporation furnace is controlled at 550-600°C to make the 4 Evaporation is condensed and collected in the condenser;

[0025] Change the molten salt intermittently, return 280kg of molten salt from the evaporation furnace to the molten salt furnace every hour, and then use the pump to replenish 280kg of molten salt into the evaporation furnace, and repeat this process, continuous evaporation in the evaporation furnace, continuous discharge, and the output reaches 1160kg per shift of 8 hours .

[0026] The result that the zirconium tetrachloride that embodiment 1~embodiment 3 p...

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Abstract

The invention relates to a zirconium tetrachloride purification method solving the problems that the prior purification method has a certain risk, hardly ensures the yield and the quality due to manual discharge adjustment when separating impurities with low boiling points and has continuous production incapability, very low productivity and low recovery rate. The method comprises the following steps: firstly, mixing crude ZrCl4 as well as NaCl and KCl to a molten salt furnace; heating to 290-350 DEG C to form eutectic molten salt with a low boiling point; continuously and additionally addingZrCl4 to the molten salt furnace, wherein the weight ratio of the ZrCl4 to the molten salt every hour is from 1:44 to 1:88; pumping 20-30 percent of molten salt by total weight into an evaporation furnace by a pump; controlling the furnace temperature at 500-650 DEG C to evaporate and condense the ZrCl4; intermittently exchanging the molten salt by returning 10-20 percent of added molten salt by total weight from the evaporation furnace to the molten salt furnace; adding new molten salt by the pump according to the amount of the returned molten salt; and repeating the steps to continuously discharge. The purification method is riskless, ensures the safe production and has simple process for removing the product impurities, stable quality, continuous production, high productivity and high recovery rate without high-temperature and low-temperature discharge links.

Description

technical field [0001] The invention relates to a method for purifying zirconium tetrachloride. Background technique [0002] Crude zirconium tetrachloride contains Si≤0.1, Al≤0.1, Fe≤0.1, Ti≤0.1, purified ZrCl 4 Containing Fe≤0.02, Si≤0.003, Al≤0.005, Ti≤0.003, these four impurities are present in zirconium tetrachloride as chlorides. Purification of zirconium tetrachloride is mainly to separate Si, Al, Fe, Ti impurities in zirconium tetrachloride from zirconium tetrachloride, so as to improve the quality of zirconium tetrachloride products. At present, the purification of zirconium tetrachloride is mainly realized by means of low-temperature degassing, high-temperature degassing, hydrogenation reduction, etc., and through the evaporation and condensation process of zirconium tetrachloride. Specifically: hydrogenation purification of crude ZrCl 4 , put 1 to 1.2 tons of crude zirconium tetrachloride into the purification furnace and seal it for heating, degassing, hydroge...

Claims

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Application Information

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IPC IPC(8): C01G25/04
Inventor 石政君
Owner LIAONING HUAGAO NEW MATERIAL CO LTD