Preparation method of chromium trichloride

A technology of chromium chloride and chromium hydroxide, applied in the field of chemistry, can solve the problems of low yield, high production cost, unenvironmental protection, etc., and achieve the effects of improving output and yield, low cost and reducing pollution

Inactive Publication Date: 2016-08-24
山西国润制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

3. Control the basic aging process
Although the process route is relatively short and easy to operate, a large amount of organic solvents are used in the process, the production cost is high, the yield is low, and it is not environmentally friendly.

Method used

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  • Preparation method of chromium trichloride

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Experimental program
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Effect test

Embodiment 1

[0028] The preparation of embodiment 1 chromium chloride

[0029] 1) At room temperature, add 50kg of chromium sulfate and 150kg of purified water into the glass-lined tank, stir to dissolve. Slowly add 320L of 8% sodium hydroxide solution dropwise to undergo a neutralization reaction for 1 hour. After filtering, vacuum-dry the filter cake at 70-80°C to obtain 15.45kg of chromium hydroxide.

[0030] 2) At room temperature, add 15.45kg of chromium hydroxide obtained in the previous step into the glass-lined tank, add 77.25kg of purified water and stir to dissolve. 30.9 kg of concentrated hydrochloric acid was added dropwise for reaction, and the dropwise addition was completed in 30 minutes, and reacted at 90° C. for 2 hours to obtain 112 L of reaction solution.

[0031] 3) Concentrate the reaction solution to 56L at 80°C to 85°C with a vacuum degree not greater than -0.08mp, add 0.75kg into activated carbon for decolorization for 30 minutes, and keep the feed liquid at 50-60°...

Embodiment 2

[0033] The preparation (best scheme) of embodiment 2 chromium chlorides

[0034] 1) At room temperature, add 50kg of chromium sulfate and 150kg of purified water into the glass-lined tank, stir to dissolve. Slowly add 250 L of 10% sodium hydroxide solution dropwise to undergo a neutralization reaction for 1 hour, and after filtration, vacuum-dry the filter cake at 70-80 degrees to obtain 16.15 kg of chromium hydroxide.

[0035] 2) At room temperature, add 16.15kg of chromium hydroxide obtained in the previous step into the glass-lined tank, add 80.75kg of purified water and stir to dissolve. 32.3 kg of concentrated hydrochloric acid was added dropwise for reaction, and the dropwise addition was completed in 30 minutes, and reacted at 90° C. for 2 hours to obtain 118 L of reaction solution.

[0036] 3) Concentrate the reaction solution to 59L at 80°C to 85°C and the vacuum degree is not greater than -0.08mp, then add 0.8kg into activated carbon for decolorization for 30min, ke...

Embodiment 3

[0038] The preparation of embodiment 3 chromium chlorides

[0039] 1) At room temperature, add 50kg of chromium sulfate and 150kg of purified water into the glass-lined tank, stir to dissolve. Slowly add 166.7L of 15% sodium hydroxide solution dropwise to undergo a neutralization reaction for 1 hour. After filtration, vacuum-dry the filter cake at 70-80°C to obtain 16.10kg of chromium hydroxide.

[0040] 2) At room temperature, add 16.10 kg of chromium hydroxide obtained in the previous step into the glass-lined tank, add 80.5 kg of purified water and stir to dissolve. 32.2 kg of concentrated hydrochloric acid was added dropwise for reaction, and the dropwise addition was completed in 30 minutes, and reacted at 90° C. for 2 hours to obtain 115 L of reaction solution.

[0041] 3) Concentrate the reaction solution to 55.5L at 80°C to 85°C and the vacuum degree is not greater than -0.08mp, add 0.8kg into activated carbon for decolorization for 30min, keep the feed liquid at 50-6...

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Abstract

The invention discloses a preparation method of chromium trichloride. The preparation method includes the following steps: 1) neutralizing chromium sulfate and a 8-15% sodium hydroxide solution to obtain chromium hydroxide; 2) performing a reaction to the chromium hydroxide with 2-2.5 times of hydrochloric acid to obtain a reaction liquid; 3) concentrating the reaction liquid, adding activated carbon, and filtering the reaction liquid through three stages: one activated carbon and two filter membranes, with temperature maintained at 50-60 DEG C to obtain a filtrate; and 4) spray-drying the filtrate to obtain the chromium trichloride. The preparation method increases yield and reduces content of impurities through selection and optimization on reaction liquid concentration and material proportion. In a drying method of a crystallization machine, the spray-drying method is employed preferably to replace a conventional organic solvent crystallization and vacuum drying method, so that the preparation method is environment-friendly, saves working time, reduces energy consumption and effectively controls water content. The preparation method is short in process, is low in cost, is short in time, is high in yield and content, is low in environment pollution and is very suitable for industrial production. The method aims to provide high-quality raw materials for chromium (III) medicine preparations.

Description

technical field [0001] The invention relates to a new method for preparing chromium chloride, which belongs to the field of chemistry. Background technique [0002] Chromium chloride, chemical formula: CrCl3·6H2O, is green or dark green crystalline powder, soluble in water, soluble in ethanol, insoluble in ether. It turns into a green solution after boiling with water for a long time. It turns into chromium trioxide when heated in the air. It can be sublimated in chlorine gas flow, and co-heated with carbon tetrachloride at 400 ° C to obtain kinetically inert purple anhydrous. There are three variants of hexahydrate, dark green, light green and purple, all of which turn into a mixture of dark green and purple in aqueous solution, but appear dark green in organic solvents such as DMSO, DMF, and ethanol. It is used in chromium salt making, chrome plating and as mordant. Used as a mordant in the printing and dyeing industry; used in chrome plating in the electroplating indu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G37/04
Inventor 杨立志杨育平
Owner 山西国润制药有限公司
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