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Method utilizing hydrogen chloride gas method to prepare zirconium oxychloride

A technology of hydrogen chloride gas and zirconium oxychloride, applied in chemical instruments and methods, inorganic chemistry, zirconium compounds, etc., can solve problems such as time-consuming, loss of concentration equipment, large steam, etc., to reduce costs, reduce production costs, and save effect of steam

Inactive Publication Date: 2016-08-03
LOMON BILLIONS GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a kind of method for preparing zirconium oxychloride with hydrogen chloride gas method for above-mentioned defective of prior art, overcome the method of prior art to consume a large amount of steam, evaporation process takes too much time, and equipment utilization rate is low , The defect of serious loss of concentration equipment under high temperature and high acidity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Measure 1500 mL of zirconium oxychloride leach solution with zirconium dioxide content of 70 g / L and acidity of 3.6 mol / L. Under mechanical stirring, feed hydrogen chloride gas until the acidity of the solution is 5.0mol / L, then stop passing hydrogen chloride gas; heat the material to a temperature of 60°C until it is completely dissolved; reduce it to 25°C at a rate of 0.3°C / min; Filter; rinse with 6.0mol / L dilute hydrochloric acid to obtain 338.04 g of zirconium oxychloride crystals, with a crystallization rate of 75.12%.

Embodiment 2

[0025] Measure 1500 mL of zirconium oxychloride leach solution with zirconium dioxide content of 88 g / L and acidity of 3.9 mol / L. Under mechanical stirring, feed hydrogen chloride gas until the acidity of the liquid is 5.2mol / L, stop passing hydrogen chloride gas, and heat the material to a temperature of 90°C until it is completely dissolved; reduce it to 15°C at a rate of 0.3°C / min; Filter; rinse with 5.9mol / L dilute hydrochloric acid to obtain 352.39g of zirconium oxychloride crystals, with a crystallization rate of 78.53%.

Embodiment 3

[0027] Measure 1500 mL of zirconium oxychloride leach solution with zirconium dioxide content of 98 g / L and acidity of 4.5 mol / L. Under mechanical stirring, feed hydrogen chloride gas until the acidity of the liquid is 5.4mol / L, then stop passing hydrogen chloride gas; heat the material to a temperature of 70°C until it is completely dissolved; reduce it to 20°C at a rate of 0.2°C / min; Filter; rinse with 5.8mol / L dilute hydrochloric acid to obtain 363.24g of zirconium oxychloride crystals, with a crystallization rate of 80.72%.

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Abstract

The invention discloses a method for preparing zirconium oxychloride by a hydrogen chloride gas method. The process steps of the method are: S1, taking zirconium oxychloride leaching solution and putting it into a reaction kettle; When the acidity of the zirconia leaching solution increases to a set value, stop feeding the hydrogen chloride gas; S3, heat to dissolve the crystallization material completely, and when the temperature drops to the set temperature, suction filter; S4, rinse with dilute hydrochloric acid to obtain zirconium oxychloride crystals. The beneficial effects of the present invention are: 1) The hydrogen chloride gas is passed into the zirconium oxychloride solution to increase the acidity of the solution to achieve the purpose of crystallization, and at the same time reduce the increase in the amount of liquid in the system and reduce the amount of waste acid; at the same time, it improves the utilization of equipment 2) The concentration process, an important part of the current zirconium oxychloride production process, is omitted, and a large amount of steam is no longer consumed. A single ton of zirconium oxychloride crystals saves about 6 tons of steam, effectively reducing production costs.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for preparing zirconium oxychloride by a hydrogen chloride gas method. Background technique [0002] At present, most domestic manufacturers use the method of concentrated crystallization to produce zirconium oxychloride, and ZrO 2 The zirconium oxychloride solution whose zirconium content is 70-120g / L and acidity is 3.6-4.5mol / L is evaporated with superheated steam, and then concentrated to ZrO 2 A zirconium oxychloride solution with a zirconium content of 180-220g / L and an acidity of 6.0-7.5mol / L. Then cool down to crystallize and pickle to obtain qualified products. The disadvantages of this process are firstly that a large amount of steam is consumed, secondly that the evaporation process takes too much time and the utilization rate of equipment is low, and thirdly that the loss of concentration equipment is serious under high temperature and high acidity...

Claims

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Application Information

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IPC IPC(8): C01G25/00
CPCC01G25/00
Inventor 陈建立申朝春付凌杰李景娜豆君于文军
Owner LOMON BILLIONS GRP CO LTD
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