CN101892386A - Demulsifying and detoxifying method of gallium extracting system - Google Patents
Demulsifying and detoxifying method of gallium extracting system Download PDFInfo
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- CN101892386A CN101892386A CN2010101981016A CN201010198101A CN101892386A CN 101892386 A CN101892386 A CN 101892386A CN 2010101981016 A CN2010101981016 A CN 2010101981016A CN 201010198101 A CN201010198101 A CN 201010198101A CN 101892386 A CN101892386 A CN 101892386A
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Abstract
The invention discloses a demulsifying and detoxifying method of a gallium extracting system, which is characterized by comprising the following steps of: A. processing of materials and liquids: the elimination of suspended particles, the preprocessing of a high-iron liquid and the preprocessing of a high-arsenic liquid; B. addition of a thinner and an improver in an extracting agent: adding 20-40 percent by volume of sulfonated kerosene as the thinner to reduce the viscosity of a load extracting agent, reducing emulsification and accelerating layering; adding 0.5-1 percent by volume of tributyl phosphate as the improver which can effectively inhabit the emulsification of a gallium extracting agent; and C. demulsification and detoxification in the extracting process: extracting by using a container or a pool, and inhabiting emulsification and accelerating detoxification by flexibly controlling and adopting the proper balance time and intensity of extraction, washing and reverse extraction. According to the operation of the method, the emulsifying and poisoning phenomena of the extracting agent in the gallium extracting process can be completely eliminated.
Description
Technical field:
The present invention relates to a kind of deemulsification and detoxification of gallium extracting system.
Background technology:
In order to realize extraction process, must make profit two-phase thorough mixing, and then the clarification phase-splitting, promptly should make the liquid of a phase high dispersing form milk sap mutually in another, make this milk sap instability again, can very fast phase-splitting after leaving standstill.Therefore, extraction process itself promptly is the formation and the destructive process of milk sap, but because a variety of causes, the milk sap of Sheng Chenging is very stable sometimes, can not phase-splitting in the clarification stage, or phase-splitting is chronic, promptly causes emulsification.The balance of extraction agent then is that the multiple metal ion that needs to make collection go into extraction agent under the different condition of control can enter water in the complete back extraction of another stage, makes extraction agent obtain regeneration.If regenerative process is bad, make one or more ion back extractions not exclusively in extraction agent, accumulate to reach and to a certain degree cause percentage extraction to decline to a great extent, be extraction agent and poison.
The applicant generally adopts butylacetate to extract gallium under hydrochloric acid system.The silica gel that the dust that machinery is brought in the extraction process, material slag and reaction generate etc. can cause that all emulsification, extraction process are difficult to continue; And ferric iron, trivalent arsenic etc. and gallium synchronously collection go into extraction agent, excessive concentration or regenerate extraction agent emulsification and poisoning when not enough, the gallium percentage extraction descends, deterioration in quality.
Summary of the invention:
At the deficiencies in the prior art, the present invention proposes a kind of like this scheme:
A kind of deemulsification of gallium extracting system and detoxification is characterized in that:
The pre-treatment of steps A, material, feed liquid:
Steps A-1 suspended particle is eliminated: add elder generation's amine of the poly-third second moon of polymeric flocculant by the 0.1-0.5Kg/ cubic meter in containing the gallium feed liquid, make suspended particle flocking settlings such as silica gel;
The pre-treatment of steps A-2 high ferro feed liquid: in relative encloses container, in containing the gallium feed liquid, feed sulfur dioxide gas or add S-WAT and reach capacity, so that ferric iron as much as possible in the solution is reduced to divalence;
The pre-treatment of the high arsenic feed liquid of steps A-3: in containing the gallium feed liquid, add clorox in container or pond and carry out oxidation operation, so that trivalent arsenic as much as possible in the solution is oxidized to pentavalent arsenic;
The interpolation of dilution, activator in step B, the extraction agent: press the 20-40% volume and add sulfonated kerosene, reduce emulsification, quicken layering as the viscosity of thinner with reduction load extraction agent; Add tributyl phosphate as activator can effectively suppress the to come together emulsification of gallium extraction agent by the 0.5-1% volume;
Breakdown of emulsion and detoxifcation in step C, the extraction process use container or pond to extract, and can control flexibly and adopt suitable extraction, washing, back extraction starting time, intensity to suppress emulsification, quicken to detoxify:
Step C-1 extraction section: the HF solution that finishes in abstraction pool, to pour into rapidly simultaneously the concentration 50% that accounts for extraction liquids 0.5-2% bulk specific gravity in extraction;
Step C-2 washing section: enter washing section after the extraction, preparation acidity 6N hydrochloric acid soln is compared oil: water=3-5: 1;
Step C-3 stripping section: the HF solution that in back extraction hydrochloric acid, adds the concentration 50% of 0.5-1% left and right sides volume.
The deemulsification of above-mentioned gallium extracting system and detoxification, it is further characterized in that: in steps A-1, the settling time is used the sedimentation of 1-3 level greater than the 24H/ level according to suspended particle size, quantity decision; Correctly select to use negatively charged ion or positively charged ion according to particle charge, negatively charged ion boiling water stirring and dissolving, positively charged ion adds feed liquid after with the normal-temperature water stirring and dissolving.In steps A-3, the temperature that contains the gallium feed liquid is greater than 80 degree.
The deemulsification of above-mentioned gallium extracting system and detoxification, it is further characterized in that: in step C, adopt novel intermittent formula abstraction pool to carry out the intermittent type extraction; Generally be controlled to be extraction about 2-4 minute, washed about 3 minutes, about back extraction 10-30 minute.In step C-3, the temperature that keeps back extraction acid is greater than 25 degree; Adopt the two-stage back extraction, one-level control strip liquor terminal point acidity 2-3N, secondary control strip liquor terminal point acidity 1-2N.
The present invention has following beneficial effect: operate as stated above, can eliminate the emulsification and the intoxicating phenomenon of the extraction agent in the gallium extraction process fully.
The present invention is further detailed explanation below in conjunction with embodiment.Embodiment does not limit the scope of protection of present invention.
Embodiment
The deemulsification of gallium extracting system of the present invention and detoxification and technical process:
The pre-treatment of step 1, material, feed liquid:
1. suspended particle is eliminated: add elder generation's amine (being divided into cloudy positively charged ion) of the poly-third second moon of polymeric flocculant by the 0.1-0.5Kg/ cubic meter in feed liquid, can make suspended particle flocking settlings such as silica gel.The settling time＞the 24H/ level, use the sedimentation of 1-3 level according to suspended particle size, quantity decision; And can correctly select to use negatively charged ion or positively charged ion according to particle charge.Negatively charged ion boiling water stirring and dissolving, positively charged ion add feed liquid after with the normal-temperature water stirring and dissolving.
2. the pre-treatment of high ferro feed liquid: in relative encloses container, in feed liquid, feed sulfur dioxide gas (or adding S-WAT) and reach capacity, ferric iron as much as possible in the solution is reduced to divalence (butylacetate can effectively extract ferric iron, but does not extract ferrous iron).Thereby the collection that significantly reduces extraction process iron is gone into, and alleviates emulsification and poisoning.
The pre-treatment of 3. high arsenic feed liquid adds clorox in container or pond and carries out oxidation operation, trivalent arsenic as much as possible in the solution is oxidized to pentavalent arsenic, (butylacetate can effectively extract trivalent arsenic, but does not extract pentavalent arsenic) in temperature＞80 degree feed liquids.Thereby the collection that significantly reduces extraction process arsenic is gone into, and alleviates emulsification and poisoning.
The interpolation of dilution, activator in step 2, the extraction agent: press the 20-40% volume and add sulfonated kerosene, reduce emulsification, quicken layering as the viscosity of thinner with reduction load extraction agent.Add tributyl phosphate as activator can effectively suppress the to come together emulsification of gallium extraction agent by the 0.5-1% volume.
Breakdown of emulsion and detoxifcation in step 3, the extraction process:
1. use our factory's novel intermittent formula abstraction pool to carry out the intermittent type extraction, can control flexibly and adopt suitable extraction, washing, back extraction starting time, intensity to suppress emulsification, quicken to detoxify.Generally be controlled to be 2-4 minute (the solution iron content is high more should use the short more extraction equilibrium time) of extraction, washed back extraction 10-30 minute 3 minutes.
2. extraction section: finish in abstraction pool, to pour into rapidly simultaneously the emulsification that the HF solution that accounts for extraction liquids 0.5-2% bulk specific gravity (concentration 50%) can better suppress and the formation of third phase in extraction, reduce the molten silicon amount of organic phase simultaneously.
3. washing section: enter washing section after the extraction, preparation acidity 6N hydrochloric acid soln is compared (oil: water=3-5: 1).This section can the flush away small portion iron arsenic and the metallic impurity of mechanical entrainment such as most copper, emulsification can not appear in this section, but can reduce follow-up stripping section emulsification pressure.
4. stripping section: in back extraction hydrochloric acid, add (concentration 50%) HF solution of 0.5-1% left and right sides volume, and keep temperature＞25 degree of back extraction acid.Adopt the two-stage back extraction, one-level control strip liquor terminal point acidity 2-3N, secondary control strip liquor terminal point acidity 1-2N.Stripping section except the back extraction gallium, also sufficient back extraction iron, arsenic, the extraction agent of effective regeneration.
Claims (7)
1. the deemulsification of a gallium extracting system and detoxification is characterized in that:
The pre-treatment of steps A, material, feed liquid:
Steps A-1 suspended particle is eliminated: add elder generation's amine of the poly-third second moon of polymeric flocculant by the 0.1-0.5Kg/ cubic meter in containing the gallium feed liquid, make suspended particle flocking settlings such as silica gel;
The pre-treatment of steps A-2 high ferro feed liquid: in relative encloses container, in containing the gallium feed liquid, feed sulfur dioxide gas or add S-WAT and reach capacity, so that ferric iron as much as possible in the solution is reduced to divalence;
The pre-treatment of the high arsenic feed liquid of steps A-3: in containing the gallium feed liquid, add clorox in container or pond and carry out oxidation operation, so that trivalent arsenic as much as possible in the solution is oxidized to pentavalent arsenic;
The interpolation of dilution, activator in step B, the extraction agent: press the 20-40% volume and add sulfonated kerosene, reduce emulsification, quicken layering as the viscosity of thinner with reduction load extraction agent; Add tributyl phosphate as activator can effectively suppress the to come together emulsification of gallium extraction agent by the 0.5-1% volume;
Breakdown of emulsion and detoxifcation in step C, the extraction process use container or pond to extract, and can control flexibly and adopt suitable extraction, washing, back extraction starting time, intensity to suppress emulsification, quicken to detoxify:
Step C-1 extraction section: the HF solution that finishes in abstraction pool, to pour into rapidly simultaneously the concentration 50% that accounts for extraction liquids 0.5-2% bulk specific gravity in extraction;
Step C-2 washing section: enter washing section after the extraction, preparation acidity 6N hydrochloric acid soln is compared oil: water=3-5: 1;
Step C-3 stripping section: the HF solution that in back extraction hydrochloric acid, adds the concentration 50% of 0.5-1% left and right sides volume.
2. the deemulsification of gallium extracting system according to claim 1 and detoxification is characterized in that: in steps A-1, the settling time is used the sedimentation of 1-3 level greater than the 24H/ level according to suspended particle size, quantity decision; Correctly select to use negatively charged ion or positively charged ion according to particle charge, negatively charged ion boiling water stirring and dissolving, positively charged ion adds feed liquid after with the normal-temperature water stirring and dissolving.
3. the deemulsification of gallium extracting system according to claim 1 and detoxification is characterized in that: in steps A-3, the temperature that contains the gallium feed liquid is greater than 80 degree.
4. the deemulsification of gallium extracting system according to claim 1 and detoxification is characterized in that: in step C, adopt novel intermittent formula abstraction pool to carry out the intermittent type extraction.
5. the deemulsification of gallium extracting system according to claim 4 and detoxification is characterized in that: in step C, generally be controlled to be extraction about 2-4 minute, washed about 3 minutes, about back extraction 10-30 minute.
6. the deemulsification of gallium extracting system according to claim 1 and detoxification is characterized in that: in step C-3, keep the temperature of back extraction acid to spend greater than 25.
7. the deemulsification of gallium extracting system according to claim 6 and detoxification is characterized in that: in step C-3, adopt the two-stage back extraction, one-level control strip liquor terminal point acidity 2-3N, secondary control strip liquor terminal point acidity 1-2N.
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| CN2010101981016A CN101892386B (en) | 2010-06-10 | 2010-06-10 | Demulsifying and detoxifying method of gallium extracting system |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350086A (en) * | 2011-09-11 | 2012-02-15 | 江西铜业股份有限公司 | Method for recovering organic phase from ammonium perrhenate extraction waste liquid |
| CN107557598A (en) * | 2017-05-25 | 2018-01-09 | 中国科学院过程工程研究所 | The method for preparing V electrolyte |
| CN108085492A (en) * | 2017-12-18 | 2018-05-29 | 中核二七二铀业有限责任公司 | A kind of method of zirconium hafnium extract and separate system emulsion recycling TBP |
| CN109179756A (en) * | 2018-09-26 | 2019-01-11 | 衢州华友钴新材料有限公司 | A kind for the treatment of process purifying SS from hydrometallurgy cobalt copper solution |
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| CN101070486A (en) * | 2007-05-14 | 2007-11-14 | 杨永林 | Water-in-oil type diesel-oil emulsifying agent and preparing method |
| US20090240081A1 (en) * | 2008-03-19 | 2009-09-24 | Andrew Michael Lemonds | Process for converting alkanes to unsaturated carboxylic acids |
| CN101717868A (en) * | 2009-12-01 | 2010-06-02 | 南京中锗科技股份有限公司 | Method for comprehensively recovering indium and gallium from distilled waste acid containing indium and gallium |
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- 2010-06-10 CN CN2010101981016A patent/CN101892386B/en not_active Expired - Fee Related
Patent Citations (5)
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| CN1071465A (en) * | 1991-10-11 | 1993-04-28 | 中国科学院金属研究所 | Soaking while grinding and its equipment-liquid film extraction gold-extraction process |
| CN1562761A (en) * | 2004-04-06 | 2005-01-12 | 同济大学 | Method for synthesizing one dimension nano material of lanthanum oxide through emulsion liquid membrane |
| CN101070486A (en) * | 2007-05-14 | 2007-11-14 | 杨永林 | Water-in-oil type diesel-oil emulsifying agent and preparing method |
| US20090240081A1 (en) * | 2008-03-19 | 2009-09-24 | Andrew Michael Lemonds | Process for converting alkanes to unsaturated carboxylic acids |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350086A (en) * | 2011-09-11 | 2012-02-15 | 江西铜业股份有限公司 | Method for recovering organic phase from ammonium perrhenate extraction waste liquid |
| CN107557598A (en) * | 2017-05-25 | 2018-01-09 | 中国科学院过程工程研究所 | The method for preparing V electrolyte |
| CN107557598B (en) * | 2017-05-25 | 2019-04-30 | 中国科学院过程工程研究所 | The method for preparing V electrolyte |
| CN108085492A (en) * | 2017-12-18 | 2018-05-29 | 中核二七二铀业有限责任公司 | A kind of method of zirconium hafnium extract and separate system emulsion recycling TBP |
| CN109179756A (en) * | 2018-09-26 | 2019-01-11 | 衢州华友钴新材料有限公司 | A kind for the treatment of process purifying SS from hydrometallurgy cobalt copper solution |
| CN109179756B (en) * | 2018-09-26 | 2022-02-11 | 衢州华友钴新材料有限公司 | Treatment process for purifying SS from hydrometallurgical cobalt-copper solution |
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| CN101892386B (en) | 2012-05-30 |
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Owner name: NANJING CHINA GERMANIUM TECHNOLOGY CO., LTD. Free format text: FORMER NAME: NANJING GERMANIUM TECHNOLOGY CO., LTD. |
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Address after: 211165 general road, Jiangning Development Zone, Jiangsu, Nanjing, China, No. 718 Patentee after: CHINA GERMANIUM CO., LTD. Address before: 211165 general road, Jiangning Development Zone, Jiangsu, Nanjing, China, No. 718 Patentee before: Nanjing Germanium Technology Co., Ltd. |
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Granted publication date: 20120530 Termination date: 20180610 |