CN102628101A - Method of extracting vanadium from acid leaching solution of stone coal vanadium ore - Google Patents
Method of extracting vanadium from acid leaching solution of stone coal vanadium ore Download PDFInfo
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- CN102628101A CN102628101A CN2012101281643A CN201210128164A CN102628101A CN 102628101 A CN102628101 A CN 102628101A CN 2012101281643 A CN2012101281643 A CN 2012101281643A CN 201210128164 A CN201210128164 A CN 201210128164A CN 102628101 A CN102628101 A CN 102628101A
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Abstract
The invention relates to a method of extracting vanadium from an acid leaching solution of stone coal vanadium ore. Acid leaching is carried out on the stone coal vanadium ore to obtain a vanadium-containing leaching solution with the pH value of 0-1 and an electrical potential of 250-450mV. The method is characterized by obtaining extract liquid with an electrical potential of 800-1400 mV by heating the vanadium-containing leaching solution to 60 DEG C, adding oxidant while stirring the heated solution, and carrying out a reaction for 5-60 min; obtaining vanadium-carrying organic phase and raffinade through 1-6 grade extraction with an organic phase and the extract liquid, wherein the organic phase is composed of 10-20% by mass of extractant and 80-90% by mass of sulfonated kerosene, and the volume ratio of the extract liquid to the organic phase is 1-5:1; and using the raffinade for leaching of the stone coal vanadium ore. The method of the invention utilizes superfluous acid of the leaching solution, which saves a neutralization process and cost thereof before extraction. The raffinade is returned and further used in leaching of the stone coal vanadium ore, which can decrease discharging of waste residues.
Description
Technical field
A kind of method that the present invention relates to a kind of by bone coal navajoite pickling liquor extracting vanadium.
Background technology
Vanadium is a kind of important strategic resource, and the content in the earth's crust is 0.015%, but does not have independent rich ore, generally is with low-grade and other mineral paragenesiss, like bone coal, sefstromite etc.Wherein, Bone coal is a kind of most important vanadium minerals that contains; Claim according to " southern bone coal resource comprehensive investigation report ": province, autonomous region's bone coal total reservess such as Hunan, Hubei, Zhejiang, Jiangxi, Guangxi, Guizhou, Anhui, Henan, Shaanxi are 618.8 hundred million tons; Proven reserve are 39.0 hundred million tons, only contain V in the bone coal of Hunan, Hubei, Zhejiang, Jiangxi, Guizhou, Anhui, Shaanxi Qi Sheng
2O
5Just reach 1.1797 hundred million tons, wherein V
2O
5The reserves of %>=0.5% just reach 7705.0 ten thousand tons, are 6.7 times of content of vanadium in China's vanadium titano-magnetite, are about the summation of other various countries' vanadium reserves of the world.This shows, from bone coal, extract vanadium, in the industry of smelting vanadium, have conclusive status.
The pickling process process for extracting vanadium is the smelting vanadium technology of a kind of environmental protection of growing up in recent years; Its typical process process can be sketched and be: the bone coal navajoite powder is mixed with sulfuric acid (and little auxiliary); Under the condition of heating, vanadium is leached from breeze, obtain containing the leach liquor of vanadium after filtering; Regulate the pH value of leach liquor, obtain the extraction liquid of pH=2～3; Obtain red vanadium through extraction, reextraction, oxidation, precipitation and calcination process then.
The shortcoming of pickling process is to need to consume a large amount of sulfuric acid, and the vitriolic consumption is 20～35% of a powdered ore quality in the production.In whole smelting vanadium technology, the cost of general leaching process accounts for 30～50% of whole vanadium extraction cost, and the vitriolic consuming cost accounts for 70～80% of whole leaching cost, therefore reduces the effective measure that the acid consumption is a control vanadium extraction cost.Acid leaching process improved effectively to reduce acid consumption, obtained important achievement.
CN101624650 discloses a kind of scherbinaite coal microwave exposure-acid-leaching vanadium-extracted method that contains.This method is compared with traditional leaching method, and extraction time reduces, and leaching yield obviously improves, and obviously, when identical leaching yield, can reach the purpose of obviously falling acid.But aforesaid method needs large-scale specific equipment, is difficult to realize successive scale operation in the mining area.
CN101624649 adopts the collaborative sulfuric acid of silicofluoric acid to soak vanadium, can practice thrift sulfuric acid and reach 5～25%, but this method is introduced the serious fluorion of corrodibility, and equipment is had a negative impact.
CN101760650 discloses the method for the spent acid leaching vanadium in a kind of abundant recycle part leach liquor; Be about to leach liquor and take out a part; Be used for leaching the vanadium in the original ore powder with initiate sulfuric acid in proportion, so cyclical operation go down acid in to the last the leach liquor, vanadium ion concentration and leaching yield preserve stable till, this method can reduce the sulfuric acid consumption and reach more than 20%; Can make through circulation repeatedly that vanadium concentration doubles in the leach liquor; Reduced the extraction cost, but it is loaded down with trivial details also to exist process, the shortcoming that flow process is many.
From disclosed method at present; The technic acid that falls of existing pickling process only is that leaching method to the vanadium extraction process improves or optimizes; Help the reduction of sour consumption, but still can not effectively utilize acid unnecessary in the leach liquor, need spend this part spent acid of cost neutralization on the contrary.This be because the bone coal navajoite powder through after the acidleach, the pH that obtains containing vanadium leachate must add in the alkaline matter and part acid between 0～1, obtains carrying out extraction again behind the extraction liquid of pH=2～3.Be to satisfy the requirement of extraction, must before extraction, add the alkali neutralization of tens times even hundreds of times, this part acid that is neutralized can not be utilized, and unavoidably because of the extra increase cost of adjusting pH.Simultaneously, the pH of raffinate has been reduced to 2～3, though raffinate can return the bone coal navajoite leaching process, the concentration of acid is to the utmost low and do not have a utility value.
Summary of the invention
The objective of the invention is to utilize acid unnecessary in the leach liquor need spend this part sour defective of cost neutralization on the contrary to present pickling process smelting vanadium method; Propose a kind of without neutralization procedure; But with pH=0～1; Current potential is that the vanadium leachate that contains of 250～450mV carries out extracting vanadium after the oxidation, and raffinate is returned the method that bone coal navajoite leaches.
The technical scheme that the present invention adopted is:
(1) the above-mentioned vanadium leachate to 60 ℃ of containing of heating stirs and adds oxygenant down, reacts 5～60 minutes, obtains the extraction liquid that current potential is 800～1400mV;
(2) use and to contain the organic phase that mass percent is the sulfonated kerosene of 10～20% extraction agent and 80～90%, by extraction liquid: the volume ratio of organic phase is 1～5: 1, extracts 1～6 grade, obtains load vanadium organic phase and raffinate;
(3) raffinate is used for the leaching of bone coal navajoite.
Oxygenant of the present invention is Sodium Persulfate, Potassium Persulphate, potassium permanganate, VAL-DROP, Potcrate, sodium perchlorate, potassium perchlorate, ydrogen peroxide 50 or Caro's acid.
Extraction agent of the present invention is 2-ethylphosphonic acid single 2-ethyl ester (P507), 2-hydroxy benzophenone oxime compounds or long-chain organic amine compound.
Above-mentioned 2-hydroxy benzophenone oxime compounds is 2-hydroxyl-5-(1, the 1-dimethyl propyl)-diphenyl-ketoxime, 2-hydroxyl-5-octyl group diphenyl-ketoxime or 2-hydroxyl-5-octadecyl diphenyl-ketoxime.
Above-mentioned long-chain organic amine compound is three octyl tertiary amines, octadecylamine or octadecyl dimethyl tertiary amine.
Add oxygenant the vanadium that mainly exists with the tetravalence attitude in the leach liquor is oxidized to the pentavalent vanadium, adopt described extraction agent in pH value 0～1 o'clock, the single extraction rate still can keep high percentage extraction all greater than 65%, therefore helps popularization.
The inventive method is compared with the method for existing extracting vanadium, has following clear superiority:
(1) since through the raffinate pH after the extraction still between 0～1, some acidity in addition be higher than before leach liquor, therefore return bone coal navajoite leach can practice thrift a part of sour;
(2), save N-process and the cost before the extraction because the acid of leach liquor middle and high concentration does not need neutralization;
(3) method of existing extracting vanadium in leach liquor in excess acid the time, can produce solid waste, the inventive method does not produce solid waste, can reduce the discharging of waste residue.
(4) the inventive method has been carried out complete oxidation with the vanadium in the leach liquor before extraction, so the anti-stripping agent that subsequent handling obtains needn't reoxidize, so can significantly not increase the oxidation cost.
Embodiment
Embodiment 1
Get pH=0.46, current potential be 418.2mV contain vanadium leachate 1000mL, add the 6.g VAL-DROP down in 60 ℃, stirring reaction 15 minutes obtains extraction liquid after reducing to room temperature, the current potential of this extraction liquid is 906mV, pH=0.52.Get this solution 200mL and place separating funnel; Add the organic phase that 100mL is made up of 10% 2-hydroxyl-5-octyl diphenyl-ketoxime extraction agent and 90% sulfonated kerosene, shake on the earthquake device and extract 5min, behind the standing demix; The upper strata is a load vanadium organic phase, and lower floor is a raffinate.The percentage extraction of the vanadium of single extraction is 98.8%, and the pH value of raffinate is 0.24.
Embodiment 2
Method and step are with embodiment 1, and extraction agent is 2-hydroxyl-5-octadecyl diphenyl-ketoxime, and the single extraction rate that obtains vanadium is 94.9%, and the pH value of raffinate is 0.29.
Embodiment 3
Get pH=0.46, current potential be 418.2mV contain vanadium leachate 500mL, slowly stir in 60 ℃ and add 60mL 30% hydrogen peroxide down, stirring reaction 60 minutes, reduce to room temperature after, the current potential of this extraction liquid is 822mV, pH=0.68.The solution 200mL that gets after this oxidation places separating funnel; Other adds the organic phase that 200mL is made up of the sulfonated kerosene of 20%P507 extraction agent and 80%; Vibrations extraction 10min behind the standing demix, proceeds same extracting operation with the water of lower floor on the earthquake device.After 6 extractions of successive, the percentage extraction that obtains vanadium is 95.4%, and the pH value of raffinate is 0.43.
Embodiment 4
Get embodiment 1 and place separating funnel through the extraction liquid 200mL that oxidation obtains; Add the organic phase that 200mL is made up of 20% 3 octyl tertiary amine (N-235) extraction agent and 80% sulfonated kerosene; Vibrations extraction 5min proceeds same extracting operation with the water of lower floor behind the standing demix on the earthquake device.After 3 extractions, the percentage extraction that obtains vanadium is 97.4%, and the pH value of raffinate is 0.58.
Embodiment 5
Method and step are with embodiment 4, and extraction agent is the octadecyl dimethyl tertiary amine, and the percentage extraction that obtains vanadium is 95.5%, and the pH value of raffinate is 0.62.
Embodiment 6
The 200mL raffinate that embodiment 1 is obtained is added 98% sulfuric acid 45g and is made [H
+]=6mol/L mixes with 200g bone coal navajoite powder then, and at 90 ℃ of refluxed heating 6h, the vanadium in the leach liquor is measured in cooling suction filtration, washing back, and obtaining leaching yield is 75.6%.This example can save acid about 10%.
Embodiment 7
The 200mL raffinate that embodiment 5 is obtained is added 98% sulfuric acid 48g and is made [H
+]=6mol/L mixes with 200g bone coal navajoite powder then, and at 90 ℃ of refluxed heating 6h, the vanadium in the leach liquor is measured in cooling suction filtration, washing back, and obtaining leaching yield is 74.3%.This example can save acid about 4%.
Comparative Examples 1
Get pH=0.46; Current potential be 418.2mV contain vanadium leachate 200mL; Use 20%P507,20%N-235,20%P204 and 2-hydroxyl-5-octyl diphenyl-ketoxime as extraction agent respectively; Mix with 80% sulfonated kerosene and to form organic phase and extract, extracting process is with embodiment 1, and the percentage extraction behind single extraction is respectively 3.82%, 0,16.92% and 0.
Comparative Examples 2
Get the extraction liquid 200mL that is obtained by embodiment 1, the organic phase of forming with the sulfonated kerosene of 20%P204 and 80% extracts, and extracting process is with embodiment 1, and percentage extraction is 0 behind single extraction.
Comparative Examples 3
Get pH=0.46, current potential be 418.2mV contain vanadium leachate 400mL, after regulating pH value to 2.64 and filter with ammoniacal liquor, extract by comparing 1: 1 with the organic phase of 90% sulfonated kerosene composition with 10%P204, extracting process is with embodiment 3.After 6 extractions of successive, the percentage extraction that obtains vanadium is 94.4%, and the pH value of raffinate is 2.12.This raffinate is divided into two parts; Portion mixes with the sulfuric acid of 50g 98%; Another part then mixes with the sulfuric acid (it is identical with embodiment 6 to add the acid amount) of 45g 98%, and two parts of solution mix with 200g bone coal navajoite powder respectively then, at 90 ℃ of refluxed heating 6h; The vanadium in the leach liquor is measured in cooling suction filtration, washing back, obtains leaching yield and is respectively 76.4%, 51.3%.
Comparison through embodiment and Comparative Examples can be found, if not oxidation leach liquor makes its low price vanadium be transformed into the pentavalent vanadium, even select different extraction agents all to be difficult under pH=0～1 condition vanadium is extracted; With the leach liquor oxidation, make after at a low price vanadium is transformed into the pentavalent vanadium, use extraction agent of the present invention can be under the condition of pH=0～1 effective extracting vanadium, and can reach and save N-process, reduce cost.Raffinate returns and replaces a part of sulfuric acid, still can reach original leaching yield, has the effect that reduces the acid consumption, and traditional collection vanadium method raffinate of Comparative Examples 3 representatives returns leaching and can not save acid.
Claims (5)
1. method by bone coal navajoite pickling liquor extracting vanadium; PH=0 after the bone coal navajoite acidleach～1; Current potential is the vanadium leachate that contains of 250～450mV, and it is characterized in that being made up of following steps: the above-mentioned vanadium leachate to 60 ℃ of containing of (1) heating, stir and add oxygenant down; Reacted 5～60 minutes, and obtained the extraction liquid that current potential is 800～1400mV; (2) use and to contain the organic phase that mass percent is the sulfonated kerosene of 10～20% extraction agent and 80～90%, by extraction liquid: the volume ratio of organic phase is 1～5: 1, extracts 1～6 grade, obtains load vanadium organic phase and raffinate; (3) raffinate is used for the leaching of bone coal navajoite.
2. the method for bone coal navajoite pickling liquor extracting vanadium according to claim 1 is characterized in that described oxygenant is Sodium Persulfate, Potassium Persulphate, potassium permanganate, VAL-DROP, Potcrate, sodium perchlorate, potassium perchlorate, ydrogen peroxide 50 or Caro's acid.
3. the method for bone coal navajoite pickling liquor extracting vanadium according to claim 1 is characterized in that described extraction agent is 2-ethylphosphonic acid single 2-ethyl ester (P507), 2-hydroxy benzophenone oxime compounds or long-chain organic amine compound.
4. according to the method for claim 1 or 3 described bone coal navajoite pickling liquor extracting vanadium; It is characterized in that said 2-hydroxy benzophenone oxime compounds is 2-hydroxyl-5-(1, the 1-dimethyl propyl)-diphenyl-ketoxime, 2-hydroxyl-5-octyl group diphenyl-ketoxime or 2-hydroxyl-5-octadecyl diphenyl-ketoxime.
5. according to the method for claim 1 or 3 described bone coal navajoite pickling liquor extracting vanadium, it is characterized in that said long-chain organic amine compound is three octyl tertiary amines, octadecylamine or octadecyl dimethyl tertiary amine.
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Cited By (8)
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| CN102851500A (en) * | 2012-09-19 | 2013-01-02 | 中南大学 | Method for extracting vanadium from vanadium-containing highly concentrated sulfuric acid solution and application of extracting agent |
| CN103074503A (en) * | 2013-02-27 | 2013-05-01 | 老河口市绿华环保科技有限公司 | Wastewater zero discharging system and method for vanadium extraction from stone coal |
| CN103409626A (en) * | 2013-07-29 | 2013-11-27 | 中国科学院过程工程研究所 | Method for asynchronously extracting and separating vanadium and manganese from solution containing V (IV) and Mn (II) |
| CN106048261A (en) * | 2016-08-22 | 2016-10-26 | 东北大学 | Method for extracting vanadium from acidic solution by using ionic liquid [OMIM]BF4 |
| CN108866356A (en) * | 2018-04-03 | 2018-11-23 | 东北大学 | A method of the extraction vanadium extraction from vanadium slag high acidic oils liquid |
| CN114438346A (en) * | 2022-01-29 | 2022-05-06 | 华北理工大学 | Method for extracting vanadium from vanadium slag by direct atmospheric-pressure acid leaching |
| CN115558803A (en) * | 2022-10-08 | 2023-01-03 | 武汉科技大学 | Method for purifying and enriching vanadium from vanadium shale pickle liquor |
| CN115676887A (en) * | 2022-10-08 | 2023-02-03 | 武汉科技大学 | Method for preparing high-purity vanadium pentoxide from vanadium shale by full-wet method |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102851500A (en) * | 2012-09-19 | 2013-01-02 | 中南大学 | Method for extracting vanadium from vanadium-containing highly concentrated sulfuric acid solution and application of extracting agent |
| CN103074503A (en) * | 2013-02-27 | 2013-05-01 | 老河口市绿华环保科技有限公司 | Wastewater zero discharging system and method for vanadium extraction from stone coal |
| CN103074503B (en) * | 2013-02-27 | 2014-04-02 | 老河口市绿华环保科技有限公司 | Wastewater zero discharging system and method for vanadium extraction from stone coal |
| CN103409626A (en) * | 2013-07-29 | 2013-11-27 | 中国科学院过程工程研究所 | Method for asynchronously extracting and separating vanadium and manganese from solution containing V (IV) and Mn (II) |
| CN106048261A (en) * | 2016-08-22 | 2016-10-26 | 东北大学 | Method for extracting vanadium from acidic solution by using ionic liquid [OMIM]BF4 |
| CN108866356A (en) * | 2018-04-03 | 2018-11-23 | 东北大学 | A method of the extraction vanadium extraction from vanadium slag high acidic oils liquid |
| CN114438346A (en) * | 2022-01-29 | 2022-05-06 | 华北理工大学 | Method for extracting vanadium from vanadium slag by direct atmospheric-pressure acid leaching |
| CN115558803A (en) * | 2022-10-08 | 2023-01-03 | 武汉科技大学 | Method for purifying and enriching vanadium from vanadium shale pickle liquor |
| CN115676887A (en) * | 2022-10-08 | 2023-02-03 | 武汉科技大学 | Method for preparing high-purity vanadium pentoxide from vanadium shale by full-wet method |
| CN115676887B (en) * | 2022-10-08 | 2023-11-17 | 武汉科技大学 | Method for preparing high-purity vanadium pentoxide by vanadium shale full wet process |
| CN115558803B (en) * | 2022-10-08 | 2023-12-22 | 武汉科技大学 | Method for purifying and enriching vanadium from vanadium shale pickle liquor |
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Application publication date: 20120808 |