CN101696468A - Acid-method regenerative organic phase process in vanadium extraction cycle - Google Patents
Acid-method regenerative organic phase process in vanadium extraction cycle Download PDFInfo
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- CN101696468A CN101696468A CN200910218487A CN200910218487A CN101696468A CN 101696468 A CN101696468 A CN 101696468A CN 200910218487 A CN200910218487 A CN 200910218487A CN 200910218487 A CN200910218487 A CN 200910218487A CN 101696468 A CN101696468 A CN 101696468A
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Abstract
The invention provides an acid-method regenerative organic phase process in vanadium extraction cycle, which is characterized in that the regeneration of solvent-extraction poor organic phase in extraction cycle adopts sulfuric acid solution with the concentration between 250 and 300 g/l as regenerant; the flow ratio of the poor organic phase to the regenerant is 10-15:1; the volume ratio (contact phase ratio) of the poor organic phase to regeneration aqueous phase in a mixed system is 1.2-1.5:1; and regeneration temperature is controlled between 40 and 50 DEG C. The process has the advantages of producing no three-phase material during regeneration, leaving out three-phase separation tank necessary in alkali-method regeneration, reducing the accompanying loss of organic phase caused by the generation of iron, aluminum and other hydroxide precipitates in the alkali-method regeneration, reducing the cost of products per ton and saving 12,000 yuan for the cost of products per ton and one million yuan for investment in regeneration equipment.
Description
Technical field
The present invention relates to the regenerative organic phase process in a kind of vanadium extraction circulation, be specifically related to the acid-method regenerative organic phase process in a kind of vanadium extraction circulation.
Background technology
As everyone knows, containing the scherbinaite coal is distinctive one of the vanadium resource that enriches of China, but for a long time, contains scherbinaite coal process for extracting vanadium by the ruling with the salt sinter process of classics, and the key of this technology is that one is seriously polluted, does not meet the requirement of social development; The 2nd, the rate of recovery of vanadium is extremely low, and usually≤50%, the so low rate of recovery also is the significant wastage that contains the scherbinaite coal resource to China's abundant; The 3rd, mechanize continuous production process degree is poor, particularly original two step precipitation methods, so be difficult to the scale that goes up, this for this reason old technology is got down from horse one after another or is forced to be banned by government.
The substitute is direct acidleach in recent years, after connect solvent-extracted process for extracting vanadium, facts have proved that the acid system process for extracting vanadium has not only solved the pollution problem of former classics with the salt sinter process, realized the streamline operration of mechanize, made in the enterprise scale; Also improved the total yield (can reach about 70%) of vanadium simultaneously widely, this is a no small breakthrough for extracting vanadium from stone coal.
Acid technological process adopts the solvent extraction purification technique, part of impurity elements such as iron, aluminium also are extracted in extraction process, and progressively accumulation, poison and can not extracting vanadium until organic phase, therefore the organic phase step for regeneration must be set in extraction cycle promptly remove impurity in the organic phase, make organic phase recover the ability of extracting vanadium with regenerator.Alkali process is adopted at present common organic phase regeneration, regenerator is the ammonium bicarbonate solution of alkalescence, the contained impurity of organic phase forms with iron, aluminium hydroxide form and carries the three-phase thing of a large amount of organic phases secretly during regeneration, must be through the organic phase after special three phase separation equipment just can obtain regenerating, and after acidifying, just can be used for extraction.Alkaline regeneration exists and to consume not only that alkali is big, the organic phase loss is big but also drawback such as required equipment is many, and it has also increased a lot of costs virtually.
Summary of the invention
The object of the present invention is to provide the acid-method regenerative organic phase process in a kind of vanadium extraction circulation, it has reduced raw-material consumption, has reduced the investment of reclaim equiment, has saved unit cost.
The acid-method regenerative principle:
P
204Be a kind of liquid cation crossover extraction agent, in organic phase, two P
204Molecule aggregation becomes a polymerizable molecular, and its polyreaction formula is as follows:
The aqueous phase metal ion removes VO during extraction
2+, Fe
3+, MoO
2 2+Outside being extracted Deng element, other metal ions such as Fe
2+, Ca
2+, Mg
2+, Cu
2+, Zn
2+, Al
3+Still stay aqueous phase Deng extraction seldom or hardly, thereby reach the purifying purpose with the foreign metal ion isolation.Metallic cation that is extracted and P
204Hydrogen atom in the polymerizable molecular carries out cationic exchange, and metal ion enters organic phase, and hydrogen ion enters water, and following chemical reaction takes place extraction process:
Above-mentioned reaction is reversible reaction, as long as improve aqueous phase acidity reaction is moved in the opposite direction, can reach organic phase regenerated purpose with foreign metal positively charged ions such as the higher sulphuric acid soln reextraction iron of acidity, aluminium again with the higher sulphuric acid soln of the acidity vanadium of stripping.
Technical solution of the present invention is:
Acid-method regenerative organic phase process in a kind of vanadium extraction circulation, its special character is: the regeneration of the poor organic phase of solvent extraction employing concentration is that the sulphuric acid soln of 250～300g/l is a regenerator in extraction cycle; The throughput ratio of its poor organic phase and regenerator is 10～15: 1, when poor organic phase impurity concentration is high, strengthens the regenerator flow, and common 10: 1 enough, otherwise lessly is advisable by 15: 1; Poor organic phase and regeneration water are 1.2～1.5: 1 for good mixing volume ratio (contact and compare) in real, and when contact is compared less than 1.2: 1, water can occur is external phase, is unfavorable for being separated, and can reduce the regeneration required time simultaneously, and influences regeneration efficiency; When contact is compared greater than 1.5: 1, again can be because of regenerator is few, and reduce regeneration efficiency.Its regeneration temperature is controlled at 40～50 ℃.Improve regeneration temperature and help improving regeneration efficiency, but too high regeneration temperature can increase the particularly volatilization loss of kerosene of organic phase; When the configuration regenerator, because of the heat energy that Dilution of sulphuric acid produces is kept required regeneration temperature, and needn't heat outward, the regeneration temperature in summer can reach 50 ℃ usually, and then be about 40 ℃ winter.
Following chemical reaction mainly takes place in above-mentioned extraction process:
The throughput ratio of above-mentioned poor organic phase and regenerator is 11～14: 1 for good.
The throughput ratio of above-mentioned poor organic phase and regenerator is 12～13: 1 for good.
Above-mentioned poor organic phase and the regeneration volume ratio (contact compare) of water in mixed stocker connect than being 1.3～1.4: 1.
Above-mentioned regeneration temperature is controlled at 45 ℃ for good.
Above-mentioned regeneration comprises 3～4 grades of regeneration of adverse current.
The invention has the advantages that:
1, adopts acid-method regenerative technology, the residual sulfuric acid of regenerated liquid can be used for leaching, accomplish to make the best use of everything, saved the consumption of alkaline regeneration carbon ammonium, no three-phase thing in the regenerative process, saved the necessary three phase separation groove of alkaline regeneration, reduced the organic phase loss of carrying secretly because of precipitations of hydroxide such as alkaline regeneration generation iron, aluminium;
2, adopt acid-method regenerative technology, can reduce the cost of ton product, product per ton is saved 1.2 ten thousand yuan of costs, reclaim equiment is invested 1,000,000 yuan.
Embodiment
Acid-method regenerative organic phase process in a kind of vanadium extraction circulation, the regeneration of the poor organic phase of solvent extraction employing concentration is that the sulphuric acid soln of 250～300g/l is a regenerator in extraction cycle; The throughput ratio of its poor organic phase and regenerator is 10～15: 1, when poor organic phase impurity concentration is high, strengthens the regenerator flow, and common 10: 1 enough, otherwise lessly is advisable by 15: 1; Poor organic phase and the regeneration volume ratio (contact compare) of water in mixed stocker connect than being 1.2～1.5: 1 for good, compare less than 1.2: 1 when contact, water can occur is external phase, is unfavorable for being separated, can reduce the regeneration required time simultaneously, and influence regeneration efficiency; When contact is compared greater than 1.5: 1, again can be because of regenerator is few, and reduce regeneration efficiency.Its regeneration temperature is controlled at 40～50 ℃.Improve regeneration temperature and help improving regeneration efficiency, but too high regeneration temperature can increase the particularly volatilization loss of kerosene of organic phase; When the configuration regenerator, because of the heat energy that Dilution of sulphuric acid produces is kept required regeneration temperature, and needn't heat outward, the regeneration temperature in summer can reach 50 ℃ usually, and then be about 40 ℃ winter.
Following chemical reaction mainly takes place in its extraction process:
The throughput ratio of wherein poor organic phase and regenerator is 11～14: 1 for good.
The throughput ratio of wherein poor organic phase and regenerator is 12～13: 1 for good.
Wherein poor organic phase and the regeneration volume ratio (contact compare) of water in mixed stocker connect than being 1.3～1.4: 1.
Wherein regeneration temperature is controlled at 45 ℃ for good.
Wherein regeneration comprises 3～4 grades of regeneration of adverse current.
Compare with traditional alkaline regeneration, product per ton reduces by 1.2 ten thousand yuan, save reclaim equiment invests 1,000,000 yuan, and regeneration rate reaches about 70%.
Claims (7)
1. the acid-method regenerative organic phase process during a vanadium extraction circulates is characterized in that: the regeneration of the poor organic phase of solvent extraction employing concentration is that the sulphuric acid soln of 250～300g/l is a regenerator in extraction cycle; The throughput ratio of its poor organic phase and regenerator is 10～15: 1; Poor organic phase and the regeneration volume ratio (contact compare) of water in mixed stocker connect than being 1.2～1.5: 1; Its regeneration temperature is controlled at 40～50 ℃.
2. according to the acid-method regenerative organic phase process in the described vanadium extraction circulation of claim 1, it is characterized in that following chemical reaction mainly takes place described extraction process:
3. according to the acid-method regenerative organic phase process in the described vanadium extraction circulation of claim 1, it is characterized in that: the throughput ratio of described poor organic phase and regenerator is 11～14: 1.
4. according to the acid-method regenerative organic phase process in the described vanadium extraction circulation of claim 2, it is characterized in that: the throughput ratio of described poor organic phase and regenerator is 12～13: 1.
5. according to the acid-method regenerative organic phase process in the circulation of the described vanadium extraction of claim 1, it is characterized in that: described poor organic phase and the volume ratio (contact compare) of water in mixed stocker of regenerating connect than being 1.3～1.4: 1.
6. according to the acid-method regenerative organic phase process in the described vanadium extraction circulation of claim 1, it is characterized in that: described regeneration temperature is controlled at 45 ℃
7. according to the acid-method regenerative organic phase process in the described vanadium extraction circulation of claim 1～6, it is characterized in that: described regeneration comprises 3～4 grades of regeneration of adverse current.
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Cited By (8)
| 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 |
| CN103014338A (en) * | 2013-01-18 | 2013-04-03 | 株洲冶炼集团股份有限公司 | Method for processing poor organic phase after solvent extraction indium extracting |
| 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 |
| CN107254589A (en) * | 2017-07-06 | 2017-10-17 | 河北工程大学 | A kind of rubidium caesium in t BAMBP extractions separation and Extraction salt lake bittern |
| CN108642282A (en) * | 2018-03-26 | 2018-10-12 | 杨秋良 | The recovery method of vanadium in a kind of fluorine-containing extracting vanadium from stone coal pickle liquor |
| CN110714121A (en) * | 2018-12-13 | 2020-01-21 | 中核沽源铀业有限责任公司 | Method for reducing consumption of organic phase in uranium molybdenum extraction process |
| CN110923449A (en) * | 2019-12-11 | 2020-03-27 | 南昌航空大学 | Method for recovering P204 from waste P204 extracted organic phase |
| CN110923450A (en) * | 2019-12-13 | 2020-03-27 | 南昌航空大学 | Method for recovering C272 from waste C272 extraction organic phase |
-
2009
- 2009-10-23 CN CN200910218487A patent/CN101696468A/en active Pending
Cited By (11)
| 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 |
| CN103014338A (en) * | 2013-01-18 | 2013-04-03 | 株洲冶炼集团股份有限公司 | Method for processing poor organic phase after solvent extraction indium extracting |
| 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 |
| CN103233134B (en) * | 2013-05-10 | 2014-04-23 | 桃江瑞龙金属新材料有限责任公司 | Recycling method of organic phase used for extracting scandium |
| CN107254589A (en) * | 2017-07-06 | 2017-10-17 | 河北工程大学 | A kind of rubidium caesium in t BAMBP extractions separation and Extraction salt lake bittern |
| CN108642282A (en) * | 2018-03-26 | 2018-10-12 | 杨秋良 | The recovery method of vanadium in a kind of fluorine-containing extracting vanadium from stone coal pickle liquor |
| CN110714121A (en) * | 2018-12-13 | 2020-01-21 | 中核沽源铀业有限责任公司 | Method for reducing consumption of organic phase in uranium molybdenum extraction process |
| CN110923449A (en) * | 2019-12-11 | 2020-03-27 | 南昌航空大学 | Method for recovering P204 from waste P204 extracted organic phase |
| CN110923449B (en) * | 2019-12-11 | 2021-06-22 | 南昌航空大学 | Method for recovering P204 from waste P204 extracted organic phase |
| CN110923450A (en) * | 2019-12-13 | 2020-03-27 | 南昌航空大学 | Method for recovering C272 from waste C272 extraction organic phase |
| CN110923450B (en) * | 2019-12-13 | 2021-06-22 | 南昌航空大学 | Method for recovering C272 from waste C272 extraction organic phase |
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