CN85100163A - A kind of method of from the decomposition nut liquid of alumina producing, extracting gallium - Google Patents
A kind of method of from the decomposition nut liquid of alumina producing, extracting gallium Download PDFInfo
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- CN85100163A CN85100163A CN85100163.7A CN85100163A CN85100163A CN 85100163 A CN85100163 A CN 85100163A CN 85100163 A CN85100163 A CN 85100163A CN 85100163 A CN85100163 A CN 85100163A
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- gallium
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Abstract
A kind of method of from the decomposition nut liquid of alumina producing, extracting gallium.Go out in the later mother liquor of aluminium hydroxide to feed CO to the carbonating decomposition and separation
2, carry out thorough carbonating and decompose.Gallium, aluminium enter precipitation with the form of amorphous hydrate.Precipitation separation is removed most of Na
2O adds lime milk dealuminium in precipitation, obtain the solution of rich gallium, feeds CO again
2, generate the precipitation of rich gallium, with the rich gallium precipitation of dissolution of sodium hydroxide, and add sodium sulfide technique for removing heavy metal simultaneously, make the electrolytic solution that contains gallium 3～9g/l.Make the electrolytic tank electrolysis of anode and cathode with stainless steel, on negative electrode, obtain gallium, use the salt acid treatment again, can produce purity and be 99.99～99.999% gallium.
Description
The invention belongs to the commercial run (C22B58/00) that extracts gallium.
Used in the world gallium mainly is to extract from the decomposition nut liquid of alumina producing at present.Extracting method was divided into for two steps mostly, and the firstth, produce the aluminum oxide of rich gallium, the secondth, make electrolytic solution with the rich gallium aluminum oxide of sodium hydroxide stripping, during electrolysis, on negative electrode, obtain gallium.As United States Patent (USP) 2,582,376.
Its processing method is, adds calcium oxide in the sodium aluminate solution that had decomposed, makes the form precipitation of aluminum oxide with the calcium aluminate mixture, feeds CO again
2, make part or all sodium aluminate solution inefficacies in the solution, make a kind of aluminum oxide of rich gallium, then the aluminum oxide of rich gallium is dissolved in the sodium hydroxide solution, then send to electrolysis.The shortcoming of this method is, a large amount of Na in the sodium aluminate solution
2O does not give removing earlier and just adds calcium oxide, and the quantity that generates the calcium aluminate mixture is big, and during separation, the gallium that solid phase is taken away is many, has reduced the rate of recovery, simultaneously, a large amount of calcium aluminate mixtures, alumina producing is difficult to use, and sends difficulty.In addition serious calcium aluminate is scabbed, do not find the good treatment method, make the production operation difficulty.
The purpose of this invention is to provide a kind of processing method, this method can reduce the growing amount of calcium aluminate mixture, improves the rate of recovery of gallium, and calcium aluminate is carried out appropriate processing, solves it and scabs and problem of outlet.
Present method is just to divide to charcoal to feed CO in the mother liquor before adding calcium oxide
2, make gallium, aluminium enter precipitation with the form of amorphous hydrate, then, precipitation separation, a large amount of Na
2O stays in the liquid phase, and this liquid is returned the alumina producing system, solid after the separation enters dealumination process, in the presence of milk of lime, generate the calcium aluminate mixture, the ratio of gallium and aluminium is improved, used Lv Fan to separate dealuminzation slurries, solid phase calcium aluminate mixture, after adding the milk of lime stirring, deliver to alumina producing and make desilicifying additive, the calcium aluminate washing lotion is returned gallium flow process batching, and filtrate feeds CO again
2Carry out thorough charcoal acidifying, gallium, aluminium enter precipitation again, after the liquid-solid separation, with the dissolution of sodium hydroxide precipitation, add sodium sulphite simultaneously and remove heavy metal, must contain gallium 3～9g/l clarification electrolytic solution after the press filtration, do electrolysis in the glass steel tank of cathode and anode at stainless steel, obtain gallium on the negative electrode, the gallium that obtains with salt acid treatment electrolysis can output purity be 99.99～99.999% gallium.
Accompanying drawing is one embodiment of the present of invention, is described in detail as follows: the mother liquor that alumina producing carbonating decomposition and separation goes out behind the aluminium hydroxide is that charcoal divides 1. (composition: Na of mother liquor
2CO
3120～376g/l, NaOH 13～65g/l, Al
2O
32. 6～32g/l, gallium 0.01～0.1g/l) pump into charcoal acidifying decomposer, and feed CO
23., thoroughly decompose, 65～98 ℃ of logical steam (12) insulations, stirred 2.5～7 hours, gallium, aluminium are separated out with amorphous hydrate, slurries after the decomposition pump into pressure filter and 4. carry out liquid, the solid separation, and after the separation, 6. filtrate send filtrate tank (20), then, deliver to the dissolution fluid of alumina producing (21) deallocation system stripping grog, 7. 5. precipitation enter dosing vessel, in dosing vessel, add milk of lime 8. with the calcium aluminate washing lotion 10., prepare burden at normal temperatures, during batching, the add-on of milk of lime is pressed CaO and Al
2O
3Mole ratio 2～4, CaO and CO
2Mole ratio 0.8～1.2 calculate.The slip for preparing pump into dealuminzation groove (11) and add electrolysis mother liquor (30) and milk of lime 8., logical steam (12) reacted 1.5～4 hours down at 85～110 ℃, generate the calcium aluminate mixture and enter solid phase, these slurries are pumped into filter (13) carry out liquid-solid separation, after filter cake calcium aluminate (16) 8. dashes with milk of lime, the desiliconization process of delivering to alumina producing (21) is as desilicifying additive, and 10. the calcium aluminate washings returns dosing vessel and 7. prepare burden, filtrate (14) (composition: Na
2O 25～65g/l, Al
2O
30.6～3g/l, gallium 0.06～0.2g/l) pump into stoste decomposer (15) and feed CO
23. carrying out thorough carbonating decomposes, decomposition temperature is controlled at 55～95 ℃, and gallium, aluminium enter precipitation with the form of hydrate again, and the decomposition slurries pump into pressure filter (17) and carry out liquid-solid separation, filtrate (19) send filtrate tank (20) 6. to mix with filtrate, send the alumina producing system.Rich gallium precipitation is sent into dissolving tank (22) (18) (containing gallium 1.5～2.5%), adds sodium hydroxide and sodium sulfide solution (23), logical stripping temperature dissolving, and the add-on of sodium hydroxide is by causticity Na
2O and Al
2O
3Mole ratio 1.5～1.9, causticity Na
2O and CO
2Mole ratio 0.8～1.2 calculate.The add-on of sodium sulphite is 0.5 of weight of precipitate～5 ‰, 80～110 ℃ of solvent temperatures, and time＞2.5 hour, the slurries after the dissolving pump into the liquid-solid separation of solution tension filter Fan, and 9. molten slag is delivered to dosing vessel and is 7. prepared burden, filtrate, i.e. electrolytic solution (25) (composition: Na
2O 160～245g/l, Al
2O
340～120g/l, gallium 3～9g/l) send into electrolyzer (26) electrolysis, and electrolytic condition is: current density 0.05～0.1 peace/Cm
2Bath voltage 2.5～5V, 40～75 ℃ of temperature, pole span 15～45mm, on negative electrode, obtain gallium (thick gallium (27)), thick gallium is put into acid and is boiled jar and carry out acid and boil, and the condition that acid is boiled is with 0.5～5 centinormal 1 hydrochloric acid (29), feeds steam (12) and is incubated 60～100 ℃, acid solution and liquid metal gallium stirred 2～10 hours, leave standstill eliminating hydrochloric acid then, use the distilled water thorough washing, obtain purity and be 99.99～99.999% gallium (31).
Claims (5)
1, a kind of method of extracting gallium from the decomposition nut liquid of alumina producing is added calcium oxide in decomposition nut liquid, generates calcium aluminate mixture solid precipitation, and then, liquid, solid phase are separated, and obtain the solution of rich gallium, feed CO to this solution again
2Generate amorphous gallium aluminium hydrate precipitation, after the liquid-solid separation, use the sodium hydroxide solution dissolution precipitation, filter and obtain clarifying electrolytic solution, make the electrolytic tank electrolysis of electrode with metal, obtain gallium on negative electrode, it is characterized in that, used decomposition nut liquid is a charcoal acidifying decomposition nut liquid, in decomposition nut liquid, add before the calcium oxide dealuminzation, at first logical CO in mother liquor
2Thoroughly charcoal acidifying, generate amorphous gallium aluminium hydrate precipitation, after liquid-solid body separated, liquid returned grog stripping operation in the alumina producing, the solid interpolation calcium oxide of rich gallium, calcium aluminate wash water, molten slag are finished dealumination reaction, the calcium aluminate mixture solid phase that generates pours alumina producing with milk of lime and makes desilicifying additive, the gallium that electrolysis goes out, use the salt acid treatment, obtain purity and be 99.99～99.999% gallium.
2, in accordance with the method for claim 1, the composition that it is characterized in that said charcoal acidifying decomposition nut liquid is Na
2CO
3120～376g/l, NaOH13～65g/l, Al
2O
36～32g/l, gallium 0.01～0.1g/l.
3,, it is characterized in that the temperature of said thorough charcoal acidization control is 65～99 ℃ according to claim 1,2 described methods.
4, according to claim 1,2 described methods, it is characterized in that said condition with salt acid treatment gallium is, hydrochloric acid with 0.5～5N concentration mixes stirring down after 2～10 hours at 60～100 ℃ with the liquid metal gallium, leave standstill eliminating hydrochloric acid, gallium is with distilled water or deionized water thorough washing.
5, according to claim 1,2 described methods, it is characterized in that said thorough charcoal acidization controlled temperature is 65～99 ℃, said condition with salt acid treatment gallium is, hydrochloric acid with 0.5～5N concentration mixes stirring down after 2～10 hours at 60～100 ℃ with the liquid metal gallium, leave standstill eliminating hydrochloric acid, gallium is with distilled water or deionized water thorough washing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85100163.7A CN1006235B (en) | 1985-04-01 | 1985-04-01 | Method of extracting gallium form dissociation mother liquor form the prodn. of alumina |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85100163.7A CN1006235B (en) | 1985-04-01 | 1985-04-01 | Method of extracting gallium form dissociation mother liquor form the prodn. of alumina |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85100163A true CN85100163A (en) | 1986-07-30 |
| CN1006235B CN1006235B (en) | 1989-12-27 |
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ID=4790939
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85100163.7A Expired CN1006235B (en) | 1985-04-01 | 1985-04-01 | Method of extracting gallium form dissociation mother liquor form the prodn. of alumina |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1006235B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0438790A1 (en) * | 1990-01-19 | 1991-07-31 | Europäische Wirtschaftsgemeinschaft (E.W.G.) | Process for the separation and the concentration of gallium from an aqueous solution containing gallium together with aluminium, zinc and/or copper |
| CN102011019A (en) * | 2010-12-14 | 2011-04-13 | 中国铝业股份有限公司 | Method for removing heavy-metal impurities in process of producing gallium by resin adsorption method |
| CN102703928A (en) * | 2012-05-23 | 2012-10-03 | 中国科学院过程工程研究所 | Method for extracting gallium through ultrasonic-assisted intensified electrolysis |
| CN103031450A (en) * | 2012-12-28 | 2013-04-10 | 北京吉亚半导体材料有限公司 | Purification method for gallium |
| CN103060573A (en) * | 2012-12-06 | 2013-04-24 | 中南大学 | Comprehensive recovery technology of valuable components in corundum smelting smoke ash containing gallium and potassium |
| CN103382531A (en) * | 2012-05-04 | 2013-11-06 | 中国科学院过程工程研究所 | Method for enriching gallium from mother-liquor in technology for producing alumina from high-alumina fly ash |
| CN103993331A (en) * | 2014-05-29 | 2014-08-20 | 珠海经济特区方源有限公司 | Method for treating gallium electrolysis tail liquid |
| CN115679381A (en) * | 2022-10-24 | 2023-02-03 | 武汉纺织大学 | Electrolytic recovery device of gallium-containing production mother liquor and use method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100371472C (en) * | 2006-08-25 | 2008-02-27 | 中国铝业股份有限公司 | Method for extracting metallic gallium from aluminium oxide production procedure |
-
1985
- 1985-04-01 CN CN85100163.7A patent/CN1006235B/en not_active Expired
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0438790A1 (en) * | 1990-01-19 | 1991-07-31 | Europäische Wirtschaftsgemeinschaft (E.W.G.) | Process for the separation and the concentration of gallium from an aqueous solution containing gallium together with aluminium, zinc and/or copper |
| CN102011019A (en) * | 2010-12-14 | 2011-04-13 | 中国铝业股份有限公司 | Method for removing heavy-metal impurities in process of producing gallium by resin adsorption method |
| CN103382531A (en) * | 2012-05-04 | 2013-11-06 | 中国科学院过程工程研究所 | Method for enriching gallium from mother-liquor in technology for producing alumina from high-alumina fly ash |
| CN103382531B (en) * | 2012-05-04 | 2015-09-30 | 中国科学院过程工程研究所 | A kind of method of producing enrichment gallium alumina technology mother liquor from aluminous fly-ash |
| CN102703928A (en) * | 2012-05-23 | 2012-10-03 | 中国科学院过程工程研究所 | Method for extracting gallium through ultrasonic-assisted intensified electrolysis |
| CN103060573A (en) * | 2012-12-06 | 2013-04-24 | 中南大学 | Comprehensive recovery technology of valuable components in corundum smelting smoke ash containing gallium and potassium |
| CN103060573B (en) * | 2012-12-06 | 2014-07-09 | 中南大学 | Comprehensive recovery technology of valuable components in corundum smelting smoke ash containing gallium and potassium |
| CN103031450A (en) * | 2012-12-28 | 2013-04-10 | 北京吉亚半导体材料有限公司 | Purification method for gallium |
| CN103031450B (en) * | 2012-12-28 | 2015-08-19 | 北京吉亚半导体材料有限公司 | A kind of method of purification of gallium |
| CN103993331A (en) * | 2014-05-29 | 2014-08-20 | 珠海经济特区方源有限公司 | Method for treating gallium electrolysis tail liquid |
| CN115679381A (en) * | 2022-10-24 | 2023-02-03 | 武汉纺织大学 | Electrolytic recovery device of gallium-containing production mother liquor and use method |
| CN115679381B (en) * | 2022-10-24 | 2023-03-28 | 武汉纺织大学 | Electrolytic recovery device of gallium-containing production mother liquor and use method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1006235B (en) | 1989-12-27 |
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Correct: Jiang Zhongyi False: Jiang Yizhong Number: 11 Page: 26 Volume: 2 |
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Free format text: CORRECT FROM: JIANG YIZHONG TO: JIANG ZHONGYI |
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