A method for removing impurities and preparing chromium oxide in a potassium-based sub-molten salt solution

A sub-molten salt and chromium oxide technology is applied in the field of solution crystal liquid removal and chromium oxide preparation after the reaction of chromium salt production sub-molten salt. problems such as long aging time, to achieve the effect of easy filtration and washing, low chromium band loss, and coarse particles

Active Publication Date: 2016-04-06
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patent US3899568 uses sodium dichromate to neutralize and add seeds, but the time for neutralization and heat preservation is as long as 9 to 12 hours
Chinese patent CN1070892 adopts chromium-containing sodium bisulfate as a neutralizing agent, which contains AlPO under stirring 4 and CrPO 4 One of sodium phosphate and phosphoric acid is added to the bottom liquid of the seed crystal at the same time, so that the aluminum in the solution and the trivalent chromium in the chromium-containing sodium bisulfate are converted into AlPO 4 -CrPO 4 It is difficult to solve the problem of high chromium strip loss while consuming sulfuric acid
For example (GuangyeWei, 2012, International Journal of Minerals, Metallurgy and Materials), in the presence of a large amount of carbonate, basic sodium chromium carbonate is formed. This intermediate product can also generate chromium oxide during high-temperature calcination, as shown in the following formula, but at the same time it generates High levels of chromate, reducing overall recovery in the redox process

Method used

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  • A method for removing impurities and preparing chromium oxide in a potassium-based sub-molten salt solution
  • A method for removing impurities and preparing chromium oxide in a potassium-based sub-molten salt solution
  • A method for removing impurities and preparing chromium oxide in a potassium-based sub-molten salt solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Choose potassium sub-molten salt solution from a chromium salt factory

[0038]

[0039] The alkaline solution obtained from the potassium-based sub-molten salt solution crystal solution is pumped into the storage tank, and the temperature is controlled to 60°C. Access to CO 2 (High purity CO 2 Mix with air, volume fraction 55%), neutralize potassium hydroxide for 0.4h; then add aluminum hydroxide seed crystals with a seed crystal coefficient of 0.5, neutralize and remove aluminum. The cumulative decomposition time is 2h. The removal rate of carbon and aluminum is 99.9%, and the removal rate of silicon is 98.5%. The aluminum hydroxide filter cake was washed countercurrently for 4 times, the temperature was 80°C, and the time was 30 minutes. After carbon content, the filter cake loses part of the water-soluble chromium, K in the filtrate 2 CO 3 Slightly reduced (90g / L), K 2 CO 3 :150g / L; KHCO 3 : 62g / L. The filtrate is pre-carbonized, the pressure is 0.8MPa, and the time...

Embodiment 2

[0041] Choose sodium chromate alkaline solution from a chromium salt factory

[0042]

[0043] The alkaline solution obtained from the potassium-based sub-molten salt solution crystal solution is pumped into the storage tank, and the temperature is controlled at 70°C. Access to CO 2 (High purity CO 2 Mix with air, volume fraction 36%), neutralize potassium hydroxide for 1.0h; then add aluminum hydroxide seed crystals with a seed crystal coefficient of 1.0, neutralize and remove aluminum. The cumulative decomposition time is 3h. The removal rate of carbon and aluminum is 99.5%, and the removal rate of silicon is 98.5%. The aluminum hydroxide filter cake was washed 4 times in countercurrent, at a temperature of 90°C, and a time of 15 minutes. After carbon content, the filter cake loses part of the water-soluble chromium, K in the filtrate 2 CO 3 Slightly reduced (190g / L), K 2 CO 3 :190g / L; KHCO 3 : 86g / L. The filtrate is pre-carbonized, the pressure is 0.6MPa, and the time is 1....

Embodiment 3

[0045] Choose sodium chromate alkaline solution from a chromium salt factory

[0046]

[0047] The alkaline solution obtained from the potassium-based sub-molten salt solution crystal solution is pumped into the storage tank, and the temperature is controlled to 60°C. Access to CO 2 (High purity CO 2 Mix with air, volume fraction 20%), neutralize potassium hydroxide for 0.5h; then add aluminum hydroxide seed crystals with a seed crystal coefficient of 0.6, neutralize and remove aluminum. The cumulative decomposition time is 2h. The removal rate of carbon and aluminum is 99.1%, and the removal rate of silicon is 98.0%. The aluminum hydroxide filter cake was washed countercurrently for 4 times, the temperature was 80°C, and the time was 20 minutes. After carbon content, the filter cake loses part of the water-soluble chromium, K in the filtrate 2 CO 3 Slightly reduced (280g / L), K 2 CO 3 :80g / L; KHCO 3 : 29g / L. The filtrate is pre-carbonized, the pressure is 0.4MPa, and the time ...

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Abstract

The invention discloses a method for decontaminating potassium sub-molten salt soluble crystal liquid and preparing chromic oxide. The method comprises the following steps: (1) introducing CO2 to potassium sub-molten salt soluble crystal liquid, neutralizing potassium hydroxide in the solution, then adding seed crystals, controlling the temperature of the solution at 30-90 DEG C and removing aluminum and silicon; (2) introducing CO2 to the solution obtained in the step (1) to carry out room-temperature pre-carbonation; (3) adding a reducing agent to pre-carbonated feed liquid obtained in the step (2), heating to 120-170 DEG C, and carrying out heat preservation and solid-liquid separation after reaction is ended, so as to obtain a chromium hydroxide filter cake; and (4) drying and calcining the chromium hydroxide filter cake obtained in the step (3), so as to obtain a chromium sesquioxide product. By adopting a pre-acidification mode, the reducing agent is not added in pre-carbonation; no CO2 is introduced after the pre-carbonated feed liquid and the reducing agent are mixed; the method is high in conversion rate of hydrothermal reduction, fewer in intermediate products, high in total yield of chrome, high in purity of the sintered chromic oxide and fewer in impurities by controlling a proper pre-carbonation condition.

Description

Technical field [0001] The invention relates to the field of chromium salt production, in particular to a new method for removing impurities from a solution crystal solution and preparing chromium oxide after the reaction of chromium salt production sub-molten salt. Background technique [0002] The current production methods of chromium salts are divided into calcium roasting, calcium-free roasting and liquid phase oxidation. Some calcium roasting technologies will gradually be eliminated due to low conversion rate and large slag discharge. At present, the main methods of chromium salt production in my country are calcium-free roasting and sub-molten salt liquid phase oxidation. The main purpose is to reduce the discharge of harmful chromium slag and reduce the environmental pollution of the chromium salt production industry. [0003] The sub-molten salt liquid-phase oxidation method has a high conversion rate, which can convert 99% of chromium into chromate into the leaching sol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G37/033
Inventor 曲景奎齐涛魏广叶余志辉张培育李玉杰
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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