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Method of using low-grade witherite to produce high-purity barium chloride

A production method, the technology of barium chloride, applied in the direction of calcium/strontium/barium chloride, calcium/strontium/barium halide, etc., can solve the problem of not being able to directly produce high-purity barium chloride, and achieve low refining cost and excellent process The effect of short process and low equipment investment

Inactive Publication Date: 2017-03-22
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the technical problem that the hydrochloric acid hydrolysis method of low-grade witherite ore cannot directly produce high-purity barium chloride, and provides a method for producing high-purity barium chloride with low-grade witherite
Fe, K, Na, Mg and other impurities are lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1.8Kg of low-grade witherite ore powder (including BaCO 3 The content is 60wt%, CaCO 3 content of 15wt%) into the reaction vessel, add 15wt% hydrochloric acid under the condition of stirring for acidolysis reaction, control the reaction temperature to 45°C, control the pH value of the end of the reaction to be 2~3, until there is no CO 2 Until the bubbles escape, add lime milk to adjust the alkalinity [OHˉ] to 0.4g / L, maintain the alkalinity and temperature and stir for 5 hours, filter it carefully, add 15wt% hydrochloric acid to the filtrate to adjust the pH value to 7, and transfer it to the evaporator Evaporate under medium heating, and when crystallization occurs on the liquid surface, stop heating, cool naturally to 25°C, separate with a centrifuge, take 60mL of centrifuged residue and spray to wash the solid. Wet barium chloride was washed with 700 mL of saturated barium chloride aqueous solution, stirred and washed for 15 minutes, then centrifuged to separate, a...

Embodiment 2

[0029] 180Kg of low-grade witherite ore powder (including BaCO 3 The content is 55wt%, CaCO 3 content of 17wt%) into the reaction vessel, under the condition of stirring, add 3wt% hydrochloric acid for acid hydrolysis reaction, control the reaction temperature to 50°C, control the pH value of the end of the reaction to be 2~3, until there is no CO 2 Until the bubbles escape, add lime milk to adjust the alkalinity [OHˉ] to 0.5g / L, maintain the alkalinity and temperature and stir for 5 hours, filter it carefully, add 15wt% hydrochloric acid to the filtrate to adjust the pH value to 8, and transfer it to the evaporator Evaporate under medium heating, and when crystallization occurs on the liquid surface, stop heating, cool naturally to 30°C, separate with a centrifuge, take 5L of centrifuged residue and spray to wash the solid. Wet barium chloride was washed with 50 L of saturated barium chloride aqueous solution, stirred and washed for 20 minutes, then separated by centrifuge, ...

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Abstract

The invention belongs to the technical field of fine chemical engineering preparation, and particularly relates to a method of using low-grade witherite to produce high-purity barium chloride. The method comprises the steps of adding the low-grade witherite and hydrochloric acid into an acid corrosion resistant reactor to be subject to acid hydrolysis reaction under a condition of stirring, then conducting alkalization, neutralizing, filtration, neutralizing, evaporative crystallization, filtration washing, size mixing washing and filtration washing, and finally drying the material to obtain a barium chloride product. The purity of barium chloride produced through the method is 99.5wt% or above, Ca is less than 10 PPm, Sr is less than 5 PPm, Na is less than 3 PPm, K is less than 2 PPm, Fe is less than 2 PPm, Mg is less than 2 PPm, S can not be detected, and the quality index of high-purity barium chloride is reached.

Description

technical field [0001] The invention belongs to the technical field of fine chemical preparation, in particular to a method for producing high-purity barium chloride by using low-grade witherite. Background technique [0002] Traditional high-purity barium chloride is mainly used to prepare high-purity barium carbonate and high-purity barium titanate materials. There are two traditional production methods of high-purity barium chloride: one is prepared by recrystallization process, that is, barite reduction method. The barite reduction method is to use barium sulfate, that is, barite as a raw material, add a reducing agent, etc., and pass through a high-temperature melting furnace to form barium sulfide, which then reacts with hydrochloric acid to form barium chloride. The product of this process has high purity, but the equipment The investment is large, and hydrogen sulfide gas is discharged, which seriously pollutes the environment; the other is the high-grade witherit...

Claims

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Application Information

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IPC IPC(8): C01F11/28
CPCC01F11/28C01P2006/80
Inventor 杨虎颜超邹伟颜杰陈炯
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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