CN102030355A - Process for extracting discandium trioxide by utilizing waste acid from titanium dioxide plants - Google Patents
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- CN102030355A CN102030355A CN 201010521310 CN201010521310A CN102030355A CN 102030355 A CN102030355 A CN 102030355A CN 201010521310 CN201010521310 CN 201010521310 CN 201010521310 A CN201010521310 A CN 201010521310A CN 102030355 A CN102030355 A CN 102030355A
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Abstract
The invention provides a production method for extracting discandium trioxide from waste acid, comprising the following steps: (1) taking leach liquor generated by leaching zinc oxide ores with the waste acid as a raw material, adding lime milk to adjust the pH value, hydrolyzing scandium in the leach liquor to generate precipitates, and separating the scandium from zinc and iron in the liquor after filtration; (2) dissolving the scandium precipitates with the waste acid, adding lime milk to adjust the pH value, hydrolyzing scandium in the leach liquor to generate precipitates, and separating the scandium from iron in the liquor after filtration; (3) dissolving the scandium precipitates with the waste acid, adding lime milk to adjust the pH value, hydrolyzing scandium in the leach liquor to generate precipitates, and separating the scandium from iron in the liquor after filtration; (4) finally dissolving the scandium precipitates with sulfuric acid, adjusting the pH value of the liquor, adding oxalic acid to filtrate after filtration, ensuring the scandium in the liquor to generate scandium oxalate, and then precipitating the scandium oxalate; and (5) dissolving the filtered scandium oxalate with hydrochloric acid, then precipitating the scandium in the liquor with oxalic acid, repeatedly carrying out dissolving and precipitating twice, and finally calcining the scandium, thus obtaining the discandium trioxide.
Description
Technical field:
The present invention and spent acid leach zinc oxide ore, and the pH value that makes leach liquor is between 0.5～1.0, and the production method of extraction scandium oxide is relevant from leach liquor
Technical background:
Since in the spent acid that uses Production By Sulfuric Acid Process anatase thpe white powder factory, the scandium that contains 10～25g per ton, and Sichuan Province's Panzhihua City can produce about 1,200,000 tons in spent acid every year.The total amount of scandium wherein can reach about 12～30 tons/year, but because the sulfate ion content of spent acid is higher, reach about 20%, be the about 200g of sulfate ion in every 1000mL spent acid, and the content of scandium is lower, so the scandium in the present spent acid, its extraction process technology still can't extract scandium and utilize.Cause a large amount of scandium resources to lose in vain.
The content of invention:
It is simple to the purpose of this invention is to provide a kind of production technique, and raw material and additive are cheap and be easy to get, and facility investment is few, and production cost is low, production efficiency height, and the few production method of environmental pollution.
The present invention is achieved in that
The present invention extracts the production method of scandium oxide from spent acid, comprise the steps:
1. leach zinc oxide ore with spent acid, the pH value that makes the infusion solution that leaches zinc oxide ore is greater than 0.5, but less than 1.0.Extraction time is about 3～6 hours.
2. adopt milk of lime, the pH value of solution by 0.5～1.0, is adjusted between 5.0～5.5, produce precipitation after making the scandium hydrolysis in the infusion solution.After filtering, with solution in zinc separate with iron.
3. will containing the scandium precipitation slag, to be dissolved to pH value with spent acid be between 0.5～1.0, adjusts between pH value to 5.0～5.5 with milk of lime, produces precipitation after making the scandium hydrolysis in the infusion solution.After filtering, separate with iron in the solution.
4. will containing the scandium precipitation slag again, to be dissolved to pH value with spent acid be between 0.5～1.0, adjusts between pH value to 5.0～5.5 with milk of lime, produces precipitation after making the scandium hydrolysis in the infusion solution.After filtering, separate with iron in the solution.
5. will contain the scandium precipitation slag at last with 20% technical grade sulfuric acid dissolution, the pH value that makes leach liquor is between 0.5～1.0, after filtering, adds oxalic acid in filtrate, and the compound precipitation that makes scandium in the solution generate the oxalic acid scandium is separated out.
6. the oxalic acid scandium that filters out is used dissolving with hydrochloric acid, and then with oxalic acid the scandium in the solution is precipitated out, again twice dissolving and precipitation repeatedly.
7. at last the oxalic acid scandium is calcined 1～3 hour time down as for 800～850 ℃ of temperature condition, can obtain content and be 98% white Scium trioxide, again through dissolving with hydrochloric acid and oxalic acid precipitation, and then once calcined 1～3 hour, can obtain 99.5% Scium trioxide, be scandium oxide, total recovery rate is 75～80%.
1. step leaches zinc oxide ore with spent acid, and the pH value that makes leach liquor is between 0.5～1.0, and promptly pH value is greater than 0.5, but less than 1.0.Extraction time is about 3～6 hour time.
Step 2. with milk of lime with the pH value of infusion solution by between 0.5～1.0, adjust between 5.0～5.5, make scandium hydrolysis in the infusion solution produce throw out and from solution, separate out.
3. step contains the scandium precipitation slag with spent acid dissolving, make pH value be 0.5～1.0 after, with milk of lime the pH value of leach liquor is adjusted between 5.0～5.5 again.
The 5. last primary sedimentation slag of step is with 20% dilute sulphuric acid (technical grade) dissolving, and making pH value is 0.5～1.0.Add oxalic acid then scandium is precipitated, be i.e. the oxalic acid scandium.
Step 7. through three times with dissolving with hydrochloric acid and oxalic acid precipitation, calcined 1～3 hour down through 800～850 ℃ of temperature condition, generation content is 98% white Scium trioxide, it is scandium oxide, and then use the dissolving with hydrochloric acid scandium oxide, use oxalic acid precipitation again, the gained compound was calcined 1～3 hour down through 800～850 ℃ of temperature condition once more, obtained 99.5% scandium oxide.Total recovery rate is 75～80%.
Technical characterstic of the present invention and advantage are as follows:
1. leach zinc oxide ore with spent acid, not only can reduce sulfate ion in the spent acid, make the content of its sulfate ion, reduce to 15g/L, also can obtain yttriums such as zinc, germanium, indium simultaneously by 200g/L.The pollution problem that has simultaneously solved spent acid again forms benign cyclic production pattern.
2. the scandium in the spent acid after three precipitations and three dissolving enrichments, is contained the scandium of 10～25mg by original every 1000mL, rise to and contain scandium 18～46g among every 1000mL, promptly increased about 2500 times, use be spent acid, white lime and part technical grade sulfuric acid, so cost is lower.
3. because the scandium content after the enrichment is higher,, can adopt directly heavy scandium in leach liquor of oxalic acid, simplify the input of technical process and equipment, be easy to grasp and operation so need not adopt extraction process with the scandium enrichment.
Comprehensive above-mentioned said, production technique of the present invention and technology have solved the technical problem of extracting scandium from the spent acid behind the Production By Sulfuric Acid Process anatase thpe white powder, make that also spent acid has obtained recycle, and can obtain metallic elements such as zinc, indium, germanium, cadmium, iron simultaneously, its economic worth is very remarkable, and production technique is simple, easy handling, the equipment less investment, and make that this valuable resource of scandium obtains extracting and utilizing.Also successfully solved simultaneously the environmental protection bottleneck problem that spent acid is restricting the titanium powder plant development to pollution problem and the spent acid of environment.
Description of drawings:
Fig. 1,2 is a process flow sheet of the present invention.
Embodiment:
One, when the spent acid that utilizes titanium powder plant to produce leaches zinc oxide ore, the control pH value is between 0.5～1.0.Scandium is a Sulfates, i.e. scandium sulfate, and this is because scandium has the characteristics of close stone, causes the loss of scandium at 1.0 o'clock greater than then being easy to combine with leached mud at pH value.Simultaneously, be between 0.5～1.0 at pH value, can to greatest extent the zinc in the zinc oxide ore, germanium, indium be leached again, extraction time is 3～6 hours, chemical equation is:
ZnO+H
2SO
4→ZnSO
4+H
2O
In
2O
3+3H
2SO
4→In
2(SO
4)
3+3H
2O
GeO+H
2SO
4→GeSO
4+H
2O
Two, make solid-liquid separation after filtration after, add milk of lime and make scandium hydrolysis in the leach liquor form the scandium hydroxide throw out to separate out in filtered liquid, it is that the throw out that makes germanium in the solution and indium also generate oxyhydroxide is simultaneously separated out that pH value is adjusted to purpose between 5.0～5.5.
1. primary sedimentation:
(annotate: the scandium in the solution is 15mg in the leach liquor after filtering, germanium is 4.5mg, indium is about 17mg) add milk of lime (with the white lime of the about 15～20g of calcium oxide dry basis) under normal temperature condition, stir while adding, slowly join in the leach liquor, after making pH value be adjusted to 5.0～5.5 by 0.5～1.0, continue to stir four hours, the pH value of its leach liquor is constant between remaining on 5.0～5.5, the throw out that makes scandium in its solution, germanium, indium hydrolysis form oxyhydroxide is separated out from solution, and chemical equation is:
Sc
2(SO
4)
3+3Ca(OH)
2→3CaSO
4+2Sc(OH)
3
In
2(SO
4)
3+3Ca(OH)
2→3CaSO
4+2In(OH)
3
GeSO
4+Ca(OH)
2→CaSO
4+Ge(OH)
2
After testing, the scandium in the solution is about that 0.1mg/L, germanium are about 0.1mg/L, indium is about 1.0mg/L, filters rear filtrate and delivers to the technology of extracting zinc.
2. once dissolving:
In leaching the pond, add a certain amount of sulfur waste acid with the scandium in the precipitation slag, germanium, indium dissolving.The control pH value is between 0.5～1.0, continues to stir four hours, and the pH value of solution is constant between remaining on 0.5～1.0, filter then, the solids after the filtration is promptly in the calcium sulfate slag, scandium is not more than that 10mg, germanium are not more than 10mg, indium is not more than 50mg, and chemical equation is:
2Sc(OH)
3+3H
2SO
4→Sc
2(SO
4)
3+6H
2O
2In(OH)
3+3H
2SO
4→In
2(SO
4)
3+6H
2O
Ge(OH)
2+H
2SO
4→GeSO
4+H
2O
Filter residue is a calcium sulfate, is used to produce terra alba, uses as material of construction.
3. secondary sedimentation:
Add milk of lime in the solution behind a dissolution filter, after the pH value of leach liquor adjusted to 5.0～5.5 by 0.5～1.0, continue to stir four hours, and keep pH value constant, make scandium, germanium, indium hydrolysis in the solution produce precipitation of hydroxide and from solution, separate out.
The scandium content that filters in the solution of back is about 0.1mg/L, and germanium is about 0.1mg/L, indium is about 1.0mg/L, filters surplus liquid and adopts " goethite process " that the iron in the solution is proposed, and produces " iron oxide red ", i.e. ferric oxide.
4. secondary dissolving:
The precipitation slag that will contain scandium, germanium, indium places and leaches the pond, adds an amount of spent acid with the scandium in the precipitation slag, germanium, indium dissolving, to pH value between 0.5～1.0, continue to stir four hours, and the maintenance pH value is constant, can filter.
Cross scandium content in the filter residue and be not more than that 10mg, germanium are not more than 10mg, indium is not more than 50mg.Filter residue is calcium sulfate, is used to produce terra alba and uses as material of construction.
5. precipitate for three times:
Add an amount of milk of lime in the leach liquor after the secondary dissolving, the pH value of leach liquor is adjusted to 5.0～5.5 by 0.5～1.0, continue to stir four hours, and keep pH value constant, make the throw out that forms oxyhydroxide after scandium in the leach liquor, germanium, the indium hydrolysis, from solution, separate out, filter.Scandium in the filtrate is not more than that 0.1mg/L, germanium are not more than 0.1mg/L, indium is not more than 1.0mg/L, and filtrate is used " goethite process " extraction " iron oxide red ", i.e. ferric oxide.
6. three dissolvings:
The filter residue that will contain scandium, germanium, indium places and leaches the pond, adds the acid of appropriate amount of industrial level bright sulfur, and promptly 20% dilute sulphuric acid makes scandium, germanium, the indium dissolving in the precipitation slag, and pH value is controlled between 0.5～1.0, and continues to stir four hours, and keeps the constant after-filtration of pH value.Scandium in the filter residue is not more than that 10mg, germanium are not more than 10mg, indium is not more than 50mg, and filter residue is calcium sulfate, is used to produce terra alba, uses as material of construction.
Through three precipitations and after dissolving for three times solution in scandium, can be from the scandium content the former spent acid by the original about 10～25g of every 1000Kg, be enriched to and contain the scandium amount in every 1000mL solution and be about 18～46g/L, contain the scandium amount in promptly every 1000Kg solution and be about 18～46KG.
Three, the heavy scandium of oxalic acid:
Add oxalic acid to containing the scandium amount in 18～46g/L solution, make the scandium in the solution combine the oxalic acid scadium compound precipitation that generates white with oxalic acid, separate out from solution, the scandium content in the solution is not more than 20mg and is advisable.Filter rear filtrate and be used to extract germanium and indium.Chemical equation is:
Sc
2(SO
4)
3+3H
2C
2O
4→Sc
2(C
2O
4)
3+3H
2SO
4
Four, produce high-quality scandium oxide:
The oxalic acid scadium compound that is settled out uses three dissolvings of hydrochloric acid and three precipitations, and three solution of post precipitation neutralize with milk of lime, the emission problem of treatment soln, and the scandium in the surplus liquid is fully reclaimed.Chemical equation is:
Sc
2(C
2O
4)
3+6HCl→2ScCl
3+3H
2C
2O
4
After the oxalic acid scandium drying that is settled out for the third time, send in 800～850 ℃ of calcining furnaces under the temperature condition and calcine.Time is about 1～3 hour, makes its oxalic acid scandium decomposing oxidation, and formation content is 98% white Scium trioxide, i.e. scandium oxide.
Through the scandium oxide that calcining generates, again with behind the dissolving with hydrochloric acid, use oxalic acid precipitation again, to calcine 1～3 hour down in 800～850 ℃ of temperature condition again, the content of the scandium oxide of gained can reach 99.5%, and its total recovery rate can reach about 75～80%.
Claims (6)
1. leach zinc oxide ore with containing the scandium spent acid, the pH value of infusion solution is controlled between 0.5～1.0, promptly pH value is greater than 0.5, but less than 1.0, extraction time is 3～6 hours.
2. adopt the heavy scandium of milk of lime, the control pH value is between 5.0～5.5.
3. containing the scandium precipitation slag dissolves with spent acid.
4. the content of dissolution precipitation slag employing for the third time is 20% dilute sulphuric acid (technical grade) dissolving.
5. adopt oxalic acid directly from contain scandium solution, the scandium precipitation to be separated out, generate the oxalic acid scandium.
6. through with the oxalic acid scandium behind dissolving with hydrochloric acid and three oxalic acid precipitations, under 800～850 ℃ of temperature condition, calcined 1～3 hour, generate 98% scandium oxide, use dissolving with hydrochloric acid and oxalic acid precipitation once more, calcined 1～3 hour down in 800～850 ℃ of temperature condition once more, obtain 99.5% Scium trioxide, i.e. scandium oxide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976527A (en) * | 2012-12-14 | 2013-03-20 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for obtaining scandium-rich material from acidic wastewater of titanium dioxide environment-friendly workshop |
| CN103194609A (en) * | 2013-04-23 | 2013-07-10 | 桃江瑞龙金属新材料有限责任公司 | Method for preparing scandium oxide by using rough scandium extracted from waste acid water of titanium dioxide as raw material |
| EP2931927A4 (en) * | 2012-12-17 | 2016-04-06 | Scandium Pty Ltd | Method for producing a solid scandium-containing material of enhanced scandium content |
| CN106011476A (en) * | 2016-06-21 | 2016-10-12 | 昆明冶金研究院 | New process for extracting scandium in gas ash |
| CN106048263A (en) * | 2016-06-25 | 2016-10-26 | 昆明冶金研究院 | Novel process of extracting scandium in gas ash by using waste acids |
| US20180023168A1 (en) * | 2015-02-02 | 2018-01-25 | Sumitomo Metal Mining Co., Ltd. | Method for recovering scandium |
| CN115094229A (en) * | 2022-02-22 | 2022-09-23 | 中国恩菲工程技术有限公司 | Method for recovering scandium in nickel hydroxide cobalt prepared from laterite-nickel ore |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976527A (en) * | 2012-12-14 | 2013-03-20 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for obtaining scandium-rich material from acidic wastewater of titanium dioxide environment-friendly workshop |
| CN102976527B (en) * | 2012-12-14 | 2014-06-25 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for obtaining scandium-rich material from acidic wastewater of titanium dioxide environment-friendly workshop |
| EP2931927A4 (en) * | 2012-12-17 | 2016-04-06 | Scandium Pty Ltd | Method for producing a solid scandium-containing material of enhanced scandium content |
| AU2013362874B2 (en) * | 2012-12-17 | 2018-11-15 | Element 21 Pty Ltd | Method for producing a solid scandium-containing material of enhanced scandium content |
| CN103194609A (en) * | 2013-04-23 | 2013-07-10 | 桃江瑞龙金属新材料有限责任公司 | Method for preparing scandium oxide by using rough scandium extracted from waste acid water of titanium dioxide as raw material |
| CN103194609B (en) * | 2013-04-23 | 2015-02-04 | 桃江瑞龙金属新材料有限责任公司 | Method for preparing scandium oxide by using rough scandium extracted from waste acid water of titanium dioxide as raw material |
| AU2015381819B2 (en) * | 2015-02-02 | 2018-08-23 | Sumitomo Metal Mining Co., Ltd. | Method for recovering scandium |
| US20180023168A1 (en) * | 2015-02-02 | 2018-01-25 | Sumitomo Metal Mining Co., Ltd. | Method for recovering scandium |
| US10156002B2 (en) | 2015-02-02 | 2018-12-18 | Sumitomo Metal Mining Co., Ltd. | Method for recovering scandium |
| CN106011476B (en) * | 2016-06-21 | 2018-01-12 | 昆明冶金研究院 | The technique of scandium in a kind of extraction gas ash |
| CN106011476A (en) * | 2016-06-21 | 2016-10-12 | 昆明冶金研究院 | New process for extracting scandium in gas ash |
| CN106048263A (en) * | 2016-06-25 | 2016-10-26 | 昆明冶金研究院 | Novel process of extracting scandium in gas ash by using waste acids |
| CN115094229A (en) * | 2022-02-22 | 2022-09-23 | 中国恩菲工程技术有限公司 | Method for recovering scandium in nickel hydroxide cobalt prepared from laterite-nickel ore |
| CN115094229B (en) * | 2022-02-22 | 2024-02-27 | 中国恩菲工程技术有限公司 | Method for recovering scandium in cobalt nickel hydroxide prepared from lateritic nickel ore |
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