CN103014338A - Method for processing poor organic phase after solvent extraction indium extracting - Google Patents
Method for processing poor organic phase after solvent extraction indium extracting Download PDFInfo
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Abstract
Disclosed is a method for processing a poor organic phase after solvent extraction indium extracting. The method includes: A, poor organic phase regeneration, namely, mixing the poor organic phase after solvent extraction indium extracting with regenerant, standing for layering, and separating to obtain a regenerated organic phase, wherein the regenerant is a mixture of oxalic acid and hydrofluoric acid; B, dechlorinating, namely, mixing the regenerated organic phase with water, standing for layering, and separating to obtain a dechlorinated organic phase; and C, acid pickling, namely, mixing the dechlorinated organic phase with pickling agent sulfuric acid solution for acid pickling, standing for layering, and separating to obtain a purified organic phase. By the method, the poor organic phase is continuously purified and regenerated, so that impurities such as iron, arsenic, tin, silicon dioxide, antimony, chlorine entrained in the organic phase are eliminated, and the service life of the organic phase is prolonged. In addition, by the method, the rate of removal of chlorine in the poor organic phase is higher than 85wt%, and a condition for subsequent recovery of zinc in indium extracting residual liquid is provided.
Description
Technical field
The present invention relates to the recovery method of valuable metal in a kind of Zinc hydrometallurgy process, particularly a kind of extracting treating method that from contain the indium material, reclaims indium.
Background technology
At present, the general technology flow process that reclaims indium from contain the indium material is: contain indium material → enrichment → leaching → purification → extraction → back extraction → displacement → founding anode → electrolysis → indium ingot, wherein, common extraction agent and thinner is respectively P204(two (2-ethylhexyl phosphoric acid) during extraction) and sulfonated kerosene.Day by day poor along with the indium resource, it is more and more higher to contain in the indium material impurity such as iron, arsenic, bismuth, tin, silicon, antimony, and during Enrichment Indium, impurity is also along with indium enters the enrichment slag together.When the enrichment slag leaches, these impurity major parts all change in the leach liquor, although leach liquor has been taked purification and impurity removal, but still there is partial impurities to continue to remain in the scavenging solution, when indium is carried in follow-up extraction, above-mentioned impurity also in various degree by organic extractant phase, affect organic phase extraction indium effect, more can cause emulsifying and ageing of organic phase, extraction can't be carried out.
The organic phase that indium is carried in extraction is called as rich organic phase, rich organic phase obtains indium strip liquor and lean organic phase after the hydrochloric acid back extraction of 6～7mol/L, in the prior art, generally after indium is carried in extraction, rich organic phase is carried out pickling, as to adopt concentration be that the hydrochloric acid of 6～7mol/L is to being entrained in the iron in the rich organic phase, tin, silicon-dioxide, the impurity such as antimony carry out pickling, and then back extraction, but pickling is to tin, silicon-dioxide, the impurity such as antimony are almost without elute effect, washed metal efficient is also relatively low, so that still contain a large amount of impurity in the lean organic phase that obtains after the back extraction, decrease the organic phase life cycle.Simultaneously, prior art is because carrying chlorine secretly in the organic phase, causes after recycling that cl content significantly rises in the indium-raffinate, has a strong impact on the recovery of zinc in the indium-raffinate.
Therefore, how to find a kind of method of effective processing solvent extraction process lean organic phase, prolong the life cycle of organic phase, a difficult problem that reduces cl content in the indium-raffinate remains further to be explored.
Summary of the invention
The invention solves the solvent extraction that exists in the prior art carry contain in the indium lean organic phase that a large amount of impurity cause that its life cycle is short, cl content is high causes the technical problem that cl content also raises in the indium-raffinate, provides a kind of solvent extraction to put forward the treatment process of the lean organic phase of indium.
Particularly, technical scheme of the present invention is:
The treatment process of the lean organic phase of indium is put forward in a kind of solvent extraction, may further comprise the steps:
A, lean organic phase regeneration: the lean organic phase of solvent extraction being carried indium mixes with regenerator, and then standing demix obtains regenerated liquid, regeneration organic phase after the separation; Described regenerator is the mixed solution of oxalic acid and hydrofluoric acid;
B, dechlorination: the regeneration organic phase that steps A obtains is mixed with dechlorinating agent, and standing demix obtains rich chlorine water solution, dechlorination organic phase after the separation; Described dechlorinating agent is water;
C, pickling: the dechlorination organic phase that step B is obtained is mixed with pickling agent and is carried out pickling, and standing demix obtains pickle solution, purifies organic phase after the separation; Described pickling agent is sulphuric acid soln.
As to further improvement of the present invention, in the steps A, described regenerator is the mixed solution that the hydrofluoric acid of the oxalic acid of mass percentage concentration 3～10% and mass percentage concentration 1～10% forms.
As to further improvement of the present invention, in the steps A, the volume ratio of described lean organic phase and regenerator is 10:1～60:1, and mixing time is 3～10 minutes, and temperature is 20～50 ℃, and settling time is more than 3 minutes.
As to further improvement of the present invention, among the step B, the volume ratio of regeneration organic phase and dechlorinating agent is 10:1～60:1, and mixing time is 3～10 minutes, and temperature is 20～50 ℃, and settling time is more than 3 minutes.
As to further improvement of the present invention, among the step C, the concentration of sulfuric acid is 50～300g/L in the described pickling agent.
As to further improvement of the present invention, among the step C, the volume ratio of dechlorination organic phase and sour Xian's agent is 10:1～60:1, and pickling time is 3～10 minutes, and temperature is 20～50 ℃, and settling time is more than 3 minutes.
As a further improvement on the present invention, steps A, B, C all carry out in extraction box.
Beneficial effect of the present invention is:
The treatment process of indium lean organic phase is put forward in solvent extraction provided by the invention, step by lean organic phase regeneration, dechlorination and pickling, make lean organic phase obtain continuous purification and regeneration, eliminate the impurity such as entrained iron, arsenic, tin, silicon-dioxide, antimony, chlorine in the organic phase and affected the possibility of extraction efficiency, thereby effectively solve emulsification and the problem of aging of extraction process organic phase, significantly prolong the life cycle of organic phase, realize that organic phase recycles.Simultaneously, adopt treatment process provided by the invention, can make that the decreasing ratio of chlorine reaches more than the 85wt% in the lean organic phase, effectively reduce the cl content in the indium-raffinate, for the recovery of zinc in the follow-up indium-raffinate provides condition.In addition, treatment process provided by the invention, technique is simple, workable, running cost is low.
Embodiment
As indicating without special, among the present invention, the lean organic phase that indium is carried in solvent extraction refers in extraction box rich indium organic phase after the back extraction operation is processed, and enters the organic phase of the impurity such as entrained iron in the regenerative mixed groove, arsenic, tin, silicon-dioxide, antimony, chlorine.
The invention provides a kind of solvent extraction and put forward the treatment process of the lean organic phase of indium, may further comprise the steps:
A, lean organic phase regeneration: the lean organic phase of solvent extraction being carried indium mixes with regenerator, and then standing demix obtains regenerated liquid, regeneration organic phase after the separation; Described regenerator is the mixed solution of oxalic acid and hydrofluoric acid;
B, dechlorination: the regeneration organic phase that steps A obtains is mixed with dechlorinating agent, and standing demix obtains rich chlorine water solution, dechlorination organic phase after the separation; Described dechlorinating agent is water;
C, pickling: the dechlorination organic phase that step B is obtained is mixed with pickling agent and is carried out pickling, and standing demix obtains pickle solution, purifies organic phase after the separation; Described pickling agent is sulphuric acid soln.
As previously mentioned, generally only the rich organic phase after the extraction is carried out pickling in the prior art, in fact still be entrained with a large amount of impurity such as iron, arsenic, tin, silicon-dioxide, antimony, chlorine in the lean organic phase, cause its life cycle shorter, at present generally speaking this organic phase circular flow after 7～10 days just need to change lean organic phase in the equipment such as groove tank and concentrate removal of impurities to process with sodium hydroxide.Therefore, if want to realize recycling of organic phase, must remove the impurity in the lean organic phase.And the present inventor finds by great many of experiments just, adopt treatment process provided by the invention can eliminate the impurity such as entrained iron in the organic phase, arsenic, tin, silicon-dioxide, antimony, chlorine and affect the possibility of extraction efficiency, thereby effectively solve emulsification and the problem of aging of extraction process organic phase, significantly prolong the life cycle of organic phase, the realization organic phase recycles, reduce simultaneously the cl content in the indium-raffinate, for the recovery of zinc in the follow-up indium-raffinate provides condition.
Particularly, among the present invention, the lean organic phase of first indium being carried in solvent extraction carries out manipulation of regeneration, concrete steps are mixed with regenerator for the lean organic phase of solvent extraction being carried indium, be the impurity generation chemical reactions such as the regenerators such as oxalic acid and hydrofluoric acid and iron, arsenic, tin, silicon-dioxide, antimony, chlorine, making above-mentioned impurity form precipitation enters in the regenerated liquid, make the impurity such as iron, tin and silicon-dioxide of carrying secretly in the lean organic phase change solution over to, then by standing demix, will separate with the regeneration organic phase with the solution (being regenerated liquid) of impurity.Among the present invention, described regenerator is the mixed solution of oxalic acid and hydrofluoric acid.Under the preferable case, described regenerator is that mass percentage concentration is that 3～10% oxalic acid and mass percentage concentration are the mixed solution that 1%～10% hydrofluoric acid forms.
The consumption of described regenerator fully changes in the solution impurity such as iron, tin and silicon-dioxide in the lean organic phase over to and gets final product.Under the preferable case, in the steps A, the volume ratio of described lean organic phase and regenerator is 10:1～60:1.In this steps A, thoroughly enter in the solution for guaranteeing the impurity such as iron, tin and silicon-dioxide in the lean organic phase, under the preferable case, mixing time (being the recovery time) is 3～10 minutes, and temperature is 20～50 ℃, and settling time is more than 3 minutes.Among the present invention, settling time refers to the time of repose of standing demix.
Obtain regenerated liquid and regeneration organic phase after separating in the steps A, the organic phase of wherein regenerating can be sent subsequent processing---dechlorination.The step of described dechlorination comprises: the organic phase of will regenerating is mixed with dechlorinating agent, and the chlorine of carrying secretly in the regeneration organic phase is changed in the aqueous solution, and then standing demix obtains rich chlorine water solution and dechlorination organic phase after the separation.Among the present invention, described dechlorinating agent is water.Under the preferable case, the volume ratio of regeneration organic phase and dechlorinating agent is 10:1～60:1.Among this step B, can thoroughly enter in the solution for guaranteeing the chlorine in the regeneration organic phase, under the preferable case, mixing time (being the dechlorination time) is 3～10 minutes, and temperature is 20～50 ℃, and settling time is more than 3 minutes.Among the present invention, described water also can adopt the production water poorer and more cheap than distilled water and tap water quality, reduces process costs.
Step B separates the dechlorination organic phase that obtains low chlorine content, then it is carried out pickling.The step of described pickling comprises mixes the dechlorination organic phase with pickling agent, make the impurity such as part iron residual in the dechlorination organic phase, arsenic, antimony, chlorine change pickle solution over to, and then standing demix, obtain organic phase (namely purifying organic phase) after pickle solution and the pickling after the separation, this purification organic phase can be returned extraction box and recycle.Among the present invention, described pickling agent is sulphuric acid soln.Under the preferable case, the concentration of sulfuric acid is 50～300g/L in the described pickling agent.
Under the preferable case, among the step C, during pickling, the volume ratio of dechlorination organic phase and pickling agent is 10:1～60:1.Described pickling time is 3～10 minutes, and temperature is 20～50 ℃, and settling time is more than 3 minutes.
As a kind of preferred implementation of the present invention, steps A, B, C all carry out in extraction box, be that steps A-C carries out continuously, prevent the consumption of organic phase in transfer process and the introducing of other impurity, further guarantee the treatment effect of described lean organic phase.
Among the present invention, for improving the effect of regeneration, dechlorination and pickling, the mixing step among steps A, B, the C all carries out under agitation condition.
Adopt treatment process provided by the invention, solvent extraction is carried the lean organic phase of indium and processed, after regeneration, dechlorination and cleanup acid treatment, organic phase is purified and regenerates, and wherein the decreasing ratio of chlorine is more than 85%, realizes recycling of organic phase.Simultaneously, treatment process provided by the invention, technique is simple, workable, running cost is low.
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with specific embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.The raw material that adopts all is commercially available among the embodiment.
Embodiment 1
Step 1: be that the mixed solution that forms of the hydrofluoric acid of the oxalic acid of 3wt% and 1wt% is as the regenerator of present embodiment with the concentration for preparing.Lean organic phase and regenerator are carried out mixed regeneration in the regenerative mixed groove in extraction box, wherein the volume ratio of lean organic phase and regenerator is 10:1, recovery time is 3 minutes, temperature is 20 ℃, settling time 3 minutes, obtain regenerated liquid and regeneration organic phase after the separation, the regeneration organic phase is sent subsequent processing;
Step 2: under the condition that constantly stirs, add regeneration organic phase and the dechlorinating agent water that step 1 obtains in the dechlorination tempering tank in the extraction box, mix dechlorination, the volume ratio of the organic phase of wherein regenerating and dechlorinating agent water is 10:1, the dechlorination time is 3 minutes, and temperature is 20 ℃, settling time 3 minutes, obtain rich chlorine water solution and dechlorination organic phase after the separation, the dechlorination organic phase is sent subsequent processing;
Step 3: under the condition that constantly stirs, mix in the dechlorination organic phase that step 2 is obtained and the pickling tempering tank of pickling agent (sulphuric acid soln of 50g/L) in extraction box and carry out pickling, wherein, the volume ratio of dechlorination organic phase and pickling agent is 10:1, pickling time is 3 minutes, and temperature is 20 ℃, settling time 3 minutes, obtain pickle solution after the separation and purify organic phase (its dechlorination rate is 89%), this purification organic phase is returned extraction box and is recycled.
Embodiment 2
Step 1: be that the mixed solution that forms of the hydrofluoric acid of the oxalic acid of 6wt% and 5wt% is as the regenerator of present embodiment with the concentration for preparing.Lean organic phase and regenerator are carried out mixed regeneration in the regenerative mixed groove in extraction box, wherein the volume ratio of lean organic phase and regenerator is 40:1, recovery time is 6 minutes, temperature is 40 ℃, settling time 5 minutes, obtain regenerated liquid and regeneration organic phase after the separation, the regeneration organic phase is sent subsequent processing;
Step 2: under the condition that constantly stirs, add regeneration organic phase and the dechlorinating agent that step 1 obtains in the dechlorination tempering tank in the extraction box, mix dechlorination, the volume ratio of the organic phase of wherein regenerating and dechlorinating agent water is 30:1, the dechlorination time is 5 minutes, and temperature is 30 ℃, settling time 5 minutes, obtain rich chlorine water solution and dechlorination organic phase after the separation, the dechlorination organic phase is sent subsequent processing;
Step 3: under the condition that constantly stirs, mix in the dechlorination organic phase that step 2 is obtained and the pickling tempering tank of pickling agent (sulphuric acid soln of 180g/L) in extraction box and carry out pickling, wherein, the volume ratio of dechlorination organic phase and pickling agent is 40:1, pickling time is 6 minutes, and temperature is 40 ℃, settling time 6 minutes, obtain pickle solution after the separation and purify organic phase (its dechlorination rate is 87%), this purification organic phase is returned extraction box and is recycled.
Embodiment 3
Step 1: be that the mixed solution that forms of the hydrofluoric acid of the oxalic acid of 10wt% and 10wt% is as the regenerator of present embodiment with the concentration for preparing.Lean organic phase and regenerator are carried out mixed regeneration in the regenerative mixed groove in extraction box, wherein the volume ratio of lean organic phase and regenerator is 60:1, recovery time is 10 minutes, temperature is 50 ℃, settling time 8 minutes, obtain regenerated liquid and regeneration organic phase after the separation, the regeneration organic phase is sent subsequent processing;
Step 2: under the condition that constantly stirs, add regeneration organic phase and the dechlorinating agent water that step 1 obtains in the dechlorination tempering tank in the extraction box, mix dechlorination, the volume ratio of the organic phase of wherein regenerating and dechlorinating agent water is 60:1, the dechlorination time is 10 minutes, and temperature is 50 ℃, settling time 8 minutes, obtain rich chlorine water solution and dechlorination organic phase after the separation, the dechlorination organic phase is sent subsequent processing;
Step 3: under the condition that constantly stirs, mix in the dechlorination organic phase that step 2 is obtained and the pickling tempering tank of pickling agent (sulphuric acid soln of 300g/L) in extraction box and carry out pickling, wherein, the volume ratio of dechlorination organic phase and pickling agent is 60:1, pickling time is 10 minutes, and temperature is 50 ℃, settling time 8 minutes, obtain pickle solution after the separation and purify organic phase (its dechlorination rate is 86%), this purification organic phase is returned extraction box and is recycled.
Above embodiment is preferred implementation of the present invention only, should be pointed out that to those skilled in the art, and under the prerequisite that does not break away from the principle of the invention, some improvement of having done also should be considered as protection scope of the present invention.
Claims (7)
1. the treatment process of the lean organic phase of indium is put forward in a solvent extraction, it is characterized in that, may further comprise the steps:
A, lean organic phase regeneration: the lean organic phase of solvent extraction being carried indium mixes with regenerator, and then standing demix obtains regenerated liquid, regeneration organic phase after the separation; Described regenerator is the mixed solution of oxalic acid and hydrofluoric acid;
B, dechlorination: the regeneration organic phase that steps A obtains is mixed with dechlorinating agent, and standing demix obtains rich chlorine water solution, dechlorination organic phase after the separation; Described dechlorinating agent is water;
C, pickling: the dechlorination organic phase that step B is obtained is mixed with pickling agent and is carried out pickling, and standing demix obtains pickle solution, purifies organic phase after the separation; Described pickling agent is sulphuric acid soln.
2. treatment process according to claim 1 is characterized in that, in the steps A, described regenerator is that mass percentage concentration is that 3～10% oxalic acid and mass percentage concentration are the mixed solution that 1～10% hydrofluoric acid forms.
3. treatment process according to claim 1 and 2 is characterized in that, in the steps A, the volume ratio of described lean organic phase and regenerator is 10:1～60:1, and mixing time is 3～10 minutes, and temperature is 20～50 ℃, and settling time is more than 3 minutes.
4. treatment process according to claim 1 is characterized in that, among the step B, the volume ratio of regeneration organic phase and dechlorinating agent is 10:1～60:1, and mixing time is 3～10 minutes, and temperature is 20～50 ℃, and settling time is more than 3 minutes.
5. treatment process according to claim 1 is characterized in that, among the step C, the concentration of sulfuric acid is 50～300g/L in the described pickling agent.
6. treatment process according to claim 1 or 5 is characterized in that among the step C, the volume ratio of dechlorination organic phase and pickling agent is 10:1～60:1, and pickling time is 3～10 minutes, and temperature is 20～50 ℃, and settling time is more than 3 minutes.
7. treatment process according to claim 1 is characterized in that, steps A, B, C all carry out in extraction box.
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Cited By (5)
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| CN103233134A (en) * | 2013-05-10 | 2013-08-07 | 桃江瑞龙金属新材料有限责任公司 | Recycling method of organic phase used for extracting scandium |
| CN104711421A (en) * | 2015-03-04 | 2015-06-17 | 贵州宏达环保科技有限公司 | Regenerating method of poisoning P204 extraction agent |
| CN105506313A (en) * | 2015-12-25 | 2016-04-20 | 河南豫光锌业有限公司 | Dechlorination method of organic phase in indium extracting process |
| CN107641722A (en) * | 2017-09-28 | 2018-01-30 | 新邵辰州锑业有限责任公司 | A kind of method for removing iron ion in antimony electrolyte |
| CN107858508A (en) * | 2017-11-09 | 2018-03-30 | 合山锌业科技有限公司 | The method of extraction of indium tin in solution of zinc sulfate |
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| CN105506313A (en) * | 2015-12-25 | 2016-04-20 | 河南豫光锌业有限公司 | Dechlorination method of organic phase in indium extracting process |
| CN107641722A (en) * | 2017-09-28 | 2018-01-30 | 新邵辰州锑业有限责任公司 | A kind of method for removing iron ion in antimony electrolyte |
| CN107858508A (en) * | 2017-11-09 | 2018-03-30 | 合山锌业科技有限公司 | The method of extraction of indium tin in solution of zinc sulfate |
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Application publication date: 20130403 |