CN103305693A - Method of preventing interphase impurity in vanadium-chromium extraction separation process - Google Patents
Method of preventing interphase impurity in vanadium-chromium extraction separation process Download PDFInfo
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Abstract
The invention discloses a method of preventing interphase impurity in a vanadium-chromium extraction separation process. The method is characterized by comprising the following steps of: deeply removing impurities in an extracted solution before extraction, such as phosphorus, silicon, calcium, iron, and the like; extracting the purified extracted solution through a mixed solution of an efficient composite amine extracting agent, a demulsifier and a thinner, regulating the pH of the extracted solution, controlling the extraction temperature, the extraction time, the concentration of the extracting agent and the concentration of the demulsifier in the extraction process. According to the method, solid particles possibly generating emulsification in the solution are deeply removed and the demulsifier is added to reduce the emulsification interphase stability when the extraction is finished so as to reduce the probability of inorganic salts in crystallizing on the interphase to form solid interphase membranes. The method can effectively eliminate the interphase impurity in the vanadium-chromium extraction separation process, improve the extraction equilibrium phase splitting speed, reduce the organic phase loss, save the operating cost and ensure the long-term circulation of the extraction system.
Description
Technical field
The invention belongs to metal extraction median surface dirt prevention area, be specifically related to a kind of method of preventing to occur in the vanadium-chromium extraction sepn process interphase impurity.
Background technology
Along with deepening continuously of environmental consciousness, the resource utilization of hazardous and noxious substances becomes a study hotspot of current scientific research.Heavy metal resources, the exploitation of especially low taste ore and recovery and the recycle of plurality of heavy metal more and more receive publicity.Contain and contain a large amount of Prospects of Rare Metal Vanadium and chromium in the chrome alum slag, if process irrelevantly, will consist of greatly ecotope and people's health and threaten, therefore will vanadium wherein separate rear recovery and resource utilization with chromium of far-reaching significance.
Separating of vanadium and chromium is a very thorny problem, but the investigator finds through a large amount of in depth research, primary amine can be from High-pH solution according to solvation mechanism extracting vanadium quantitatively, chromium is stayed in the raffinate, thereby is reached the purpose that vanadium chromium separates.Yet the experiment of primary amine extracting and separating vanadium and chromium is carried out in the laboratory usually, and the test reagent that the investigator adopts all is the AG medicine, in case adopt actual feed liquid as water, the problem of interphase impurity just occurred.
Interphase impurity is a difficult problem that often runs in the hydrometallurgy process, and it mainly contains water, organic phase and irregular subparticle and forms.The appearance of extraction process median surface dirt brings a lot of adverse influences will for whole extraction process, and it will seriously prolong the phase-splitting time, vanadium chromium be separated not thorough, also can cause the loss of extraction agent, strengthen production cost, severe patient can cause whole workshop to be stopped, and extracting-back extraction can't be circulated.Yet the processing interphase impurity is one more is added with a challenge ground difficult problem, because the influence factor of interphase impurity is a lot, the type of water composition, organic phase composition, external environment and agitator all can impel system to generate interphase impurity, and interphase impurity is the heterogeneous emulsification system of a stable existence, its composition can be different along with the variation of system, even in same system, its composition of interphase impurity that produces in the different time is also different, and this has just brought larger difficulty for the elimination of interphase impurity.
Chinese patent CN1048889A discloses the prevention method that relates to metallic yttrium separating-purifying process interface emulsification, it is characterized in that extracting front employing sulfide, the removal of impurities of muriate precipitation agent; CN102190567A discloses the separation method of depickling extracting and emulsifying layer, it is characterized in that showing emulsion layer sedimentation centrifugal treating, the different substances in the emulsion layer is separated again; The CN202671624U utility model patent discloses a kind of device of high efficiency separation emulsion layer; CN101565776A discloses a kind of amine, Phosphorus extraction system emulsification removing method, it is characterized in that adding trade names in advance in by extraction liquid is the metal cleaning additive of CSP-925, CSQ-926 or GEA-746, under certain condition, behind stirring, sedimentation, filtering and impurity removing, extract; US Patent No. 6500232 was also once reported the removing method of solvent extraction process median surface dirt, patent provides a kind of special device that the interphase impurity in the extraction process is removed, although this method that emulsion layer is separated is suitable for the elimination of various interface dirts, but need to increase in addition a kind of equipment, increase an operation, can improve running cost, and can not fundamentally eliminate interphase impurity, just solve problem assurance technique and normally moved.
The applicant has carried out long-term further investigation for the interphase impurity of vanadium and chromium extraction sepn process appearance, find that this interphase impurity is comprised of solia particle, water, organic phase, solia particle is that it forms and stable first cause, and there is a large amount of dispersed phase drop interfaces at interface zone, the solia particle of wherein assembling will become the crystallization active centre, reduce the surperficial energy barrier of the inorganic salt sodium sulfate nucleation of aqueous phase higher concentration, the catalysis heterogeneous nucleation forms the sodium sulfate crystal with crystal water.Simultaneously, the electrostatic double layer electric field that forms of interface zone emulsification interfacial adsorption subparticle will reduce sodium sulfate and in the solubleness at interface it separated out at interfacial crystallization.
Based on above mechanism research, specific aim proposes the prevention method of this interface dirt, at home and abroad there is no at present the pertinent literature report.
Summary of the invention
Technical problem to be solved by this invention is: overcome the deficiencies in the prior art, a kind of method of preventing vanadium-chromium extraction sepn process interphase impurity is provided, can effectively eliminate vanadium-chromium extraction sepn process median surface dirt, can prevent interphase impurity in the situation that do not increase too many running cost, perhaps make its least possible appearance, thereby the quickening extraction separation process reduces the loss of extraction agent in operational process, and the assurance production technique is normally moved.
Technical solution of the present invention is: a kind of method of preventing vanadium-chromium extraction sepn process interphase impurity, its feature may further comprise the steps: the degree of depth is removed by the impurity in the extraction liquid before (1) extraction, behind extraction liquid deep impurity-removing, its total impurities is controlled at below the 0.1g/L; (2) adopt behind the mixing solutions abstraction impurity removal of high efficiency composition amine extractant, emulsion splitter and thinner by extraction liquid, the organic phase of the vanadium that obtains loading and contain the raffinate of chromium and a small amount of vanadium, the extraction process phase-splitting is fast, produces mutually without the centre under more excellent operational condition.Extraction process is regulated material liquid pH value, control extraction temperature, time, extractant concentration and demulsifier concentration; Described varies is the mixture of primary amine and tertiary amine, the primary amine concentration of volume percent be 5 ?40%, the tertiary amine concentration of volume percent 1 ?10%; Extraction process regulate by extraction liquid pH value scope be 2 ?6; Described extraction temperature be 10 ?90 ℃; Described extraction time be 1 ?30 minutes; Described emulsion splitter concentration of volume percent be 1 ?10%.The method of prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: in the step (1), the degree of depth is removed by the impurity in the extraction liquid before extracting, and after quilt was extracted the liquid deep impurity-removing, its total impurities was controlled at below the 0.07g/L; Particularly preferably, total impurities is controlled at below the 0.05g/L.The method of prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: primary amine described in the step (2) comprises that the carbochains such as N1923, Primene JMT, Primene81R or 7101 surpass 13 organic fatty primary amine and their mixture.The method of prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: described tertiary amine comprise N235, TOA, 7301 or Alamine336 etc. in long-chain fat tertiary amine and their mixture.The method of prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1, it is characterized in that: emulsion splitter is oil-soluble demulsifier described in the step (2), be preferably polyethers, comprise the polyethers take amine as initiator, polyethers take phenolic aldehyde as initiator and the polyethers take alcohol as initiator etc. are particularly preferably the polyethers that goods number is PAG and OSP series.The method of prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: when extraction described in the step (2) regulate by extraction liquid pH value scope be 3 ?6.The method of prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: described in the step (2) in the varies extraction agent primary amine concentration of volume percent be 10 ?30%, the tertiary amine concentration of volume percent be 1 ?5%.The method of prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: emulsion splitter concentration of volume percent described in the step (2) be 0.1 ?1.5%.The method of prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: thinner comprises sulfonated kerosene, toluene, normal hexane, sherwood oil, tetrachloromethane, benzene, n-Octanol, dimethylbenzene described in the step (2); Be particularly preferably sulfonated kerosene, normal hexane, toluene.The method of prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: extraction temperature described in the step (2) be 10 ?30 ℃; Extraction time be 1 ?15 minutes.
The present invention uses organic phase that varies type extraction agent, emulsion splitter and thinner form that the feed liquid that contains behind the chrome alum slag leach liquor deep impurity-removing is carried out extracting and separating, under optimum extraction condition, during the one-level extraction, do not form interphase impurity, the percentage extraction of vanadium is very high to be 95.80%, and the percentage extraction of chromium only is 3.64%; Behind load organic oppositing back-extraction, the organic phase after the employing back extraction continues fresh feed liquid is carried out extracting and separating, is called second of organic phase and takes turns extraction, does not still have interphase impurity, and the percentage extraction of vanadium and chromium is respectively 96.90% and 3.35%; With carrying out the third round extraction behind the load organic oppositing back-extraction, there is not interphase impurity, the percentage extraction of vanadium and chromium is respectively 96.12% and 3.14%; With carrying out the 4th extraction behind the load organic oppositing back-extraction, there is not interphase impurity, the percentage extraction of vanadium and chromium is respectively 96.15% and 3.74%.The present invention has eliminated the interphase impurity in the vanadium-chromium extraction sepn process effectively, and has guaranteed the good percentage extraction of vanadium and the lasting low percentage extraction of chromium, and vanadium chromium is separated well; The four-wheel extraction occurs without the interface dirt, illustrates that this extraction system is stable, and extracting and separating is effective.
The present invention's advantage compared with prior art is:
(1) varies-emulsion splitter among the present invention-thinner extracting and separating system reaches the purpose of prevention vanadium-chromium extraction process median surface dirt, with new system extracting and separating vanadium chromium, not only effectively prevented interphase impurity, and guaranteed good vanadium chromium separating effect, and the extraction of organic phase four-wheel can both guarantee higher percentage extraction, has really accomplished to prevent interphase impurity in the situation that guarantee vanadium chromium separating effect.
(2) the present invention does not need to add any equipment in addition, and operation is simple, saves cost of equipment.
(3) need not carry out additional operations, save the labor force.
(4) fundamentally prevent interphase impurity, be better than method that interphase impurity is removed, reduce extraction agent and run off.
(5) improve minute phase effect of organic phase.
Specific embodiments
The below is accompanied by specific embodiment and introduces in detail the present invention.But following embodiment only limits to explain the present invention, and protection scope of the present invention should comprise the full content of claim, is not limited only to the present embodiment.
Embodiment 1:
To contain feed liquid behind the chrome alum slag leach liquor deep impurity-removing as extraction liquid, with primary amine N1923, tertiary amine TOA, goods number is that emulsion splitter and the thinner hexanaphthene of PAG is made into organic phase, carry out the extracting and separating test, wherein adjust material liquid pH value and be respectively 3.20,4.20,5.20,6.00, extraction agent primary amine concentration of volume percent is chosen as 15%, the tertiary amine concentration of volume percent is 5%, the emulsion splitter concentration of volume percent is 1%, extraction temperature is 25 ℃ of room temperatures, water and organic phase are mixed in separating funnel, then separating funnel is fixed on the Kang Shi vibrator and shook 15 minutes, took off the vibrator static layering 30 minutes, take out afterwards the interphase impurity between water and the organic phase, adopt the volume of the graduated cylinder measurement interphase impurity of appropriate size, then use the volume of the interphase impurity of surveying divided by the volume sum of initial water and organic phase, be designated as the production rate of interphase impurity; Get 1 milliliter of raffinate with transfer pipet afterwards and move in 100 milliliters of volumetric flasks, and add the aqueous hydrochloric acid of volume percent 1%, constant volume is measured vanadium chromium content in the raffinate with inductive coupling plasma emission spectrograph.The results are shown in Table 1.
The percentage extraction of vanadium and chromium and crud formation rate during table 1 different feed liquid initial pH value
*Crud formation rate=interphase impurity volume * 100%/(original water phase volume+initial oil phase volume)
Embodiment 2:
To contain feed liquid behind the chrome alum slag leach liquor deep impurity-removing as extraction liquid, with primary amine N1923, tertiary amine TOA, emulsion splitter and thinner hexanaphthene are made into organic phase, carry out the extracting and separating test, emulsion splitter PAG concentration of volume percent is respectively 0.3%, 0.5%, 1%, 1.5%, wherein adjusting material liquid pH value is 5.20, extraction agent primary amine concentration of volume percent is 15%, the tertiary amine concentration of volume percent is 5%, extraction temperature is 25 ℃ of room temperatures, water and organic phase are mixed in separating funnel, then separating funnel is fixed on the Kang Shi vibrator and shook 15 minutes, took off the vibrator static layering 30 minutes, take out afterwards the interphase impurity between water and the organic phase, adopt the volume of the graduated cylinder measurement interphase impurity of appropriate size, then use the volume of the interphase impurity of surveying divided by the volume sum of initial water and organic phase, be designated as the production rate of interphase impurity; Get 1 milliliter of raffinate with transfer pipet afterwards and move in 100 milliliters of volumetric flasks, and to add volume percent be 1% aqueous hydrochloric acid, constant volume is measured vanadium chromium content in the raffinate with inductive coupling plasma emission spectrograph.The results are shown in Table 2.
The percentage extraction of vanadium and chromium and crud formation rate during the different demulsifier concentration of table 2
*Crud formation rate=interphase impurity volume * 100%/(original water phase volume+initial oil phase volume)
Embodiment 3:
To contain feed liquid behind the chrome alum slag leach liquor deep impurity-removing as extraction liquid, with primary amine N1923, tertiary amine TOA, goods number is that emulsion splitter and the thinner hexanaphthene of PAG is made into organic phase, carry out the extracting and separating test, wherein thinner is respectively kerosene, toluene, n-Octanol, hexanaphthene, adjusting material liquid pH value is 5.20, the extraction agent concentration of volume percent is chosen as 15%, the tertiary amine concentration of volume percent is 5%, extraction temperature is 25 ℃ of room temperatures, water and organic phase are mixed in separating funnel, then separating funnel is fixed on the Kang Shi vibrator and shook 15 minutes, took off the vibrator static layering 30 minutes, take out afterwards the interphase impurity between water and the organic phase, adopt the volume of the graduated cylinder measurement interphase impurity of appropriate size, then use the volume of the interphase impurity of surveying divided by the volume sum of initial water and organic phase, be designated as the production rate of interphase impurity; Get 1 milliliter of raffinate with transfer pipet afterwards and move in 100 milliliters of volumetric flasks, and add the aqueous hydrochloric acid of volume percent 1%, constant volume is measured vanadium chromium content in the raffinate with inductive coupling plasma emission spectrograph.The results are shown in Table 3.
The percentage extraction of vanadium and chromium and crud formation rate during the different thinner of table 3
*Crud formation rate=interphase impurity volume * 100%/(original water phase volume+initial oil phase volume)
Embodiment 4:
To contain feed liquid behind the chrome alum slag leach liquor deep impurity-removing as extraction liquid, with primary amine N1923, tertiary amine TOA, emulsion splitter and thinner hexanaphthene are made into organic phase, carry out the extracting and separating test, emulsion splitter PAG or OSP, its concentration of volume percent is 1%, wherein adjusting material liquid pH value is 5.20, the extraction agent concentration of volume percent is 15%, the tertiary amine concentration of volume percent is 5%, extraction temperature is 25 ℃ of room temperatures, water and organic phase are mixed in separating funnel, then separating funnel is fixed on the Kang Shi vibrator and shook 15 minutes, took off the vibrator static layering 30 minutes, take out afterwards the interphase impurity between water and the organic phase, adopt the volume of the graduated cylinder measurement interphase impurity of appropriate size, then use the volume of the interphase impurity of surveying divided by the volume sum of initial water and organic phase, be designated as the production rate of interphase impurity; Get 1 milliliter of raffinate with transfer pipet afterwards and move in 100 milliliters of volumetric flasks, and to add volume percent be 1% aqueous hydrochloric acid, constant volume is measured vanadium chromium content in the raffinate with inductive coupling plasma emission spectrograph.The results are shown in Table 4.
The percentage extraction of vanadium and chromium and crud formation rate during the different demulsifier concentration of table 4
*Crud formation rate=interphase impurity volume * 100%/(original water phase volume+initial oil phase volume)
In a word, the present invention can eliminate the interphase impurity of vanadium-chromium extraction sepn process effectively, improves extraction equilibrium minute phase velocity, reduces the organic phase loss, saves running cost.
Need to prove, according to the various embodiments described above of the present invention, those skilled in the art are the four corners that can realize independent claim of the present invention and appurtenance fully, implementation procedure and method same the various embodiments described above; And the non-elaborated part of the present invention belongs to techniques well known.
The above; only be part embodiment of the present invention, but protection scope of the present invention is not limited to this, any those skilled in the art are in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (10)
1. method of preventing vanadium-chromium extraction sepn process interphase impurity, its feature may further comprise the steps:
(1) extract the front degree of depth and remove by the impurity in the extraction liquid, after quilt was extracted the liquid deep impurity-removing, its total impurities was controlled at below the 0.1g/L;
(2) adopt behind the mixing solutions abstraction impurity removal of high efficiency composition amine extractant, emulsion splitter and thinner by extraction liquid, the organic phase of the vanadium that obtains loading and contain the raffinate of chromium and a small amount of vanadium; Extraction process is regulated material liquid pH value, control extraction temperature, time, extractant concentration and demulsifier concentration; Described varies is the mixture of primary amine and tertiary amine, and the primary amine concentration of volume percent is 5-40%, and the tertiary amine concentration of volume percent is at 1-10%; It is 2-6 that extraction process is regulated by extraction liquid pH value scope; Described extraction temperature is 10-90 ℃; Described extraction time is 1-30 minute; Described emulsion splitter concentration of volume percent is 1-10%.
2. the method for prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: in the step (1), the degree of depth is removed by the impurity in the extraction liquid before the extraction, extracted the liquid deep impurity-removing after, its total impurities is controlled at below the 0.07g/L; Particularly preferably, total impurities is controlled at below the 0.05g/L.
3. the method for prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: primary amine described in the step (2) comprises that N1923, Primene JMT, Primene81R or 7101 carbochains surpass 13 organic fatty primary amine or their mixture.
4. the method for prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: described tertiary amine comprise N235, TOA, 7301 or Alamine336 in long-chain organic fatty tertiary amine or their mixture.
5. the method for prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1, it is characterized in that: emulsion splitter is oil-soluble demulsifier described in the step (2), be preferably polyethers, comprise the polyethers take amine as initiator, polyethers take phenolic aldehyde as initiator or the polyethers take alcohol as initiator are particularly preferably the polyethers that goods number is PAG and OSP series.
6. the method for prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: regulate during extraction described in the step (2) by extraction liquid pH value preferable range be 3 ?6.
7. the method for prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1, it is characterized in that: described in the step (2) in the varies extraction agent primary amine concentration of volume percent be preferably 10 ?30%, the tertiary amine concentration of volume percent be preferably 1 ?5%.
8. the method for prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: emulsion splitter concentration of volume percent described in the step (2) be preferably 0.1 ?1.5%.
9. the method for prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1, it is characterized in that: thinner comprises sulfonated kerosene, toluene, normal hexane, sherwood oil, tetrachloromethane, benzene, n-Octanol, dimethylbenzene described in the step (2); Be particularly preferably sulfonated kerosene, normal hexane, toluene.
10. the method for prevention vanadium-chromium extraction sepn process interphase impurity according to claim 1 is characterized in that: extraction temperature described in the step (2) be preferably 10 ?30 ℃; Extraction time be preferably 1 ?15 minutes.
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| CN103937998A (en) * | 2014-04-21 | 2014-07-23 | 中国科学院过程工程研究所 | Method for preparing low-silicon vanadium pentoxide from solution containing vanadium, chromium and silicon |
| CN106282559A (en) * | 2016-08-26 | 2017-01-04 | 重庆康普化学工业股份有限公司 | Copper extraction system organic facies desilication method |
| CN106811599A (en) * | 2015-11-30 | 2017-06-09 | 北京有色金属研究总院 | A kind of technique for controlling wet method metallurgy of copper leachate interphase impurity to be formed |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103937998A (en) * | 2014-04-21 | 2014-07-23 | 中国科学院过程工程研究所 | Method for preparing low-silicon vanadium pentoxide from solution containing vanadium, chromium and silicon |
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| CN103937998B (en) * | 2014-04-21 | 2016-02-10 | 中国科学院过程工程研究所 | A kind of method from preparing low silicon Vanadium Pentoxide in FLAKES containing vanadium chrome-silicon solution |
| CN106811599A (en) * | 2015-11-30 | 2017-06-09 | 北京有色金属研究总院 | A kind of technique for controlling wet method metallurgy of copper leachate interphase impurity to be formed |
| CN106282559A (en) * | 2016-08-26 | 2017-01-04 | 重庆康普化学工业股份有限公司 | Copper extraction system organic facies desilication method |
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