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Method for separating and regenerating organic phase of invalid gallium and germanium extracting agent

A technology of organic phase and extractant, which is applied in the field of organic phase separation and regeneration of invalid gallium germanium extractant, can solve the problems of loss of extraction capacity, collapse of extraction system, and impact on economic benefits, so as to avoid environmental pollution and waste of resources, and reduce consumption Effect

Active Publication Date: 2021-12-14
SHENZHEN ZHONGJIN LINGNAN NONFEMET COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Therefore, through the long-term operation of the extraction organic system, the extraction organic phase based on alkylhydroxamic acid+acidic phosphate type extractant+diluent gradually becomes the one of fatty acid+acidic phosphate type extractant+diluent The extraction system, if things go on like this, will cause the extraction system to collapse and eventually lose the extraction ability
[0008] On the other hand, the continuous supplementary cost of alkyl hydroxamic acid is very high, which is an important cost in production and seriously affects economic benefits.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] S1. Take 200ml of degradation and failure extractant and put it into a 500ml airtight bottle, add 200ml of 300g / L dilute sulfuric acid, put it in a shaker, and react for 0.5 hours;

[0051] S2. After the reaction is completed, add 200ml of clear water to the organic phase and oscillate evenly, separate the organic phase and the water phase with a separatory funnel, repeatedly mix and oscillate and wash 5 times, and measure the pH value of the last washing water to be 6 to obtain 190ml of the organic phase;

[0052] S3. Add 190ml of organic phase to 200ml of 100g / L sodium hydroxide solution, stir and react at room temperature for 60 minutes, and let stand for 6 hours. It can be observed that there is obvious stratification, and the upper layer is light yellow diluent and saponified P204, measuring cylinder weighed to obtain 115ml, separated and acidified and regenerated for secondary use, based on phosphate extractant, the recovery rate was 95.8%; the lower layer was brow...

Embodiment 2

[0057] S1. Take 200ml of degradation and failure extractant and put it into a 500ml airtight bottle, add 200ml of 180g / L dilute hydrochloric acid, put it in a shaker, and react for 0.5 hours;

[0058] S2. After the reaction is completed, add 200ml of clear water to the organic phase and oscillate evenly, separate the organic phase and the water phase with a separatory funnel, repeatedly mix and oscillate and wash for 5 times, and the pH value of the last washing water is 6 to obtain 188ml of the organic phase;

[0059] S3. 188ml organic phase is added in the 150g / L sodium hydroxide solution of 200ml, stirring and reacting at normal temperature for 90 minutes, standing for 6 hours, it can be observed that there is obvious stratification, and the upper layer is light yellow diluent and saponified P204, weighed by a measuring cylinder to obtain 114ml, separated and acidified, regenerated and used for secondary use, calculated as a phosphate extractant, the recovery rate was 95.5%;...

Embodiment 3

[0064] S1. Take 200ml of degradation and failure extraction agent and put it into a 500ml airtight bottle, add 100ml of 100g / L oxalic acid solution, put it in a shaker, and react for 1 hour;

[0065] S2. After the reaction is completed, add 200ml of clear water to the organic phase and oscillate evenly, separate the organic phase and the water phase with a separatory funnel, repeatedly mix and oscillate and wash for 5 times, and the pH value of the last washing water is 6 to obtain 184ml of the organic phase;

[0066] S3. 184ml organic phase is added in the 160g / L sodium hydroxide solution of 200ml, stirring and reacting at normal temperature for 60 minutes, standing for 6 hours, it can be observed that there is obvious stratification phenomenon, and the upper layer is light yellow diluent and saponified P204, weighed by a measuring cylinder to obtain 113ml, separated and acidified, regenerated and used for secondary use, calculated as a phosphate ester extractant, the recovery...

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Abstract

The invention discloses a method for separating and regenerating an organic phase of an invalid gallium and germanium extracting agent. The method comprises the steps that according to an extraction agent compounded by an acidic phosphate type extraction agent and alkyl hydroximic acid, the degraded extraction agent is used for implementing purification component separation, and organic phase accumulated metal ions are reversely extracted by adopting acid so as to eliminate the influence of metal ions on the subsequent oximation reaction; the diluent and the acid phosphate type extraction agent of the organic phase part are separated out, the diluent and the acid phosphate type extraction agent obtained through separation can be recycled, and the recovery rate is 95% or above; and the separated fatty acid is used as a raw material for synthesizing the alkyl hydroxamic acid for product synthesis, and after synthesis, the effective component is greater than 80%. According to the method for separating and regenerating the organic phase of the invalid gallium and germanium extracting agent, the invalid waste extraction agent is reused, so that on the one hand, the consumption of the purchase cost is reduced, and on the other hand, environmental pollution and resource waste caused by treating the invalid waste extraction agent are avoided.

Description

technical field [0001] The invention belongs to the field of comprehensive utilization of waste extractants, and in particular relates to a method for organic phase separation and regeneration of spent gallium-germanium extractants. Background technique [0002] The extractant compounded by acidic phosphate ester extractant and hydroxamic acid is an extractant for efficiently extracting gallium germanium in a sulfuric acid system. Related products include alkyl hydroxamic acid, octyl hydroxamic acid, acetyl hydroxamic acid, etc., among which alkyl hydroxamic acid is a kind of high-efficiency beneficiation agent, and has the performance of efficient extraction of gallium germanium, usually with acid phosphate type The extraction agent is compounded to obtain a co-extraction system. On the one hand, the compound extraction agent can reduce the amount of reagents used. On the other hand, the co-extraction system has a better extraction effect than the alkyl hydroxamic acid inde...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B3/40C22B41/00C22B58/00
CPCC22B7/006C22B7/009C22B41/00C22B58/00Y02P10/20
Inventor 张伟宫晓丹吴才贵张登凯周科华张俊峰骆昌运高艳芬郑莉莉黄青孙昱邓磊
Owner SHENZHEN ZHONGJIN LINGNAN NONFEMET COMPANY
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