CN107460501B - A kind of preparation method of indium industry electrolysis sulfuric acid solution of indium used - Google Patents
A kind of preparation method of indium industry electrolysis sulfuric acid solution of indium used Download PDFInfo
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- CN107460501B CN107460501B CN201710763994.6A CN201710763994A CN107460501B CN 107460501 B CN107460501 B CN 107460501B CN 201710763994 A CN201710763994 A CN 201710763994A CN 107460501 B CN107460501 B CN 107460501B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/22—Electrolytic production, recovery or refining of metals by electrolysis of solutions of metals not provided for in groups C25C1/02 - C25C1/20
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Abstract
The invention discloses a kind of preparation methods of indium sulfate electrolyte used in indium industry.Smart indium is fused into indium liquid first, it is colored at indium that indium liquid is poured into water quenching in distilled water；Gained indium flower is added in batches in the concentrated sulfuric acid of heating and is stirred to react, the fully dissolved until indium is used up stands cooling after dissolution, with indium sulfate solid state deposition after cooling；Indium sulfate after cooling is separated by filtration unreacted sulfuric acid, indium sulfate exists in the form of indium sulfate solid or aqueous sulfuric acid indium crystal after separation；Then the acidity of distilled water and sodium hydroxide adjustment solution is added, stirring to indium sulfate or aqueous sulfuric acid indium crystal all dissolve, and obtain sulfuric acid solution of indium；Gelatin finally is added into indium sulfate solution and sodium chloride is configured to indium sulfate electrolyte.Indium sulfate electrolyte is prepared using the present invention, preparation speed is fast, at low cost, in the new electrolyte periodic replenishment to electrolytic cell of preparation, can be effectively controlled impurity in electrolyte, realization standardization electrolysis operation solves enterprise and produces difficulty.
Description
One, technical field:
The invention belongs to technical field of non-ferrous metallurgy, and in particular to a kind of preparation side of indium sulfate electrolyte used in indium industry
Method.
Two, background technique:
Indium is silvery white and slightly nattier blue metal, and quality is very soft, can use nail indentation；The plasticity of indium is strong, has
Ductility can be pressed into piece.Indium metal is mainly for the manufacture of raw materials such as acolite, bearing metal, semiconductor, point light sources.From normal
Temperature is between fusing point, and slowly, surface forms very thin oxidation film to the oxygen effect in indium and air；It is and active non-when temperature is higher
Metal function.Bulk metal indium is not reacted with boiling water and aqueous slkali, but powdered indium can slowly be acted on water, generates hydroxide
Indium.Indium and the effect of cold diluted acid slowly, are soluble in the inorganic acid and acetic acid, oxalic acid of dense heat.Indium can form alloy with many metals
(especially iron, the indium for being stained with iron can be significantly oxidized).The main oxidation state of indium is+1 and+3, and main compound has In2O3、
In(OH)3、InCl3, when with halogen chemical combination, monohalide and trihalid can be respectively formed.
Currently, indium is many high-new in aviation, medical treatment, high-end electronic element, new energy development etc. as a kind of rare precious metal
Field is widely used, and as indium is using more and more extensive, the mankind increasingly increase the demand of indium, the value of indium visible one
Spot.Smart indium production will be refined by electrolysis, and indium electrolysis generally does electrolyte with Indium Sulfate, and thick indium does electrolysis sun
Pole, titanium plate do electrolysis cathode, and electrolysing period general 7 days, it is desirable that electrolyte concentration containing indium is in 70~100g/L when electrolysis.It is being electrolysed
It carries out in period production process, because electrolysis anode and cathode is uneven, the reasons such as electrolyte solution loss when slot, electrolyte are located always containing indium out
In downward trend, this just needs the sulfuric acid solution of indium of the periodically compounding high concentration into electrolyte.
Sulfuric acid solution of indium generally use smart indium (99.99% or more purity) aqueous sulfuric acid (sulfuric acid concentration 300g/L~
90 DEG C of thawings are heated in 500g/L)；Due to the physico-chemical property of phosphide element, dissolved slowly in dilute sulfuric acid, the operating time is long
(1kg essence indium dissolves completely needs 6~8h), brings inconvenience to production.
Most domestic enterprise is because traditional indium sulfate electrolyte quota is difficult, generally with loop cycle and reduction electrolyte pH
The methods of value maintains electrolysis production, causes electrolyte impurity high, and liberation of hydrogen is serious, and precipitation indium is of poor quality, and smart indium product tin, lead are frequent
It is exceeded.
Three, summary of the invention:
The technical problem to be solved by the present invention is according to deficiency existing during existing indium sulfate electrolyte quota
Place, the present invention provide a kind of preparation method of indium industry electrolysis sulfuric acid solution of indium used.Indium sulfate is prepared using the method for the present invention
Electrolyte can effectively overcome defect present in existing sulfuric acid solution of indium process for preparation.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that:
The present invention provides a kind of preparation method of indium sulfate electrolyte used in indium industry, and the preparation method includes following step
It is rapid:
A, smart indium melt water quenching: the smart indium of material purity >=99.99% is melted under the conditions of 200~260 DEG C,
Indium liquid is obtained after fusing；The equidirectional rotation of gained indium liquid is poured into and carries out water quenching in the container for fill distilled water, obtains indium flower；
B, the concentrated sulfuric acid heats: the pure concentrated sulfuric acid of analysis that mass concentration is 98% being heated to 40~50 DEG C, then by step a
The indium flower that water quenching obtains pulls viscous water suction part out from distilled water, and it is molten that at the uniform velocity stirring progress is then added portionwise in the concentrated sulfuric acid of heating
Solution reaction, the fully dissolved until water quenching indium is used up；Cooling is stood after dissolution, with indium sulfate solid state deposition after cooling；
C, it separates sulfuric acid: being first separated by filtration sulfuric acid unreacted in step b, distillation is then added into indium sulfate
Water is further separated by filtration sulfuric acid；After sulfuric acid separation, indium sulfate is deposited in the form of indium sulfate solid or aqueous sulfuric acid indium crystal
?；
D, it prepares sulfuric acid solution of indium: distilled water is added in the indium sulfate after separating sulfuric acid to step c, is then slowly added into point
The acidity for analysing pure cerium hydroxide sodium adjustment acquired solution, the pH value for controlling solution is 1.5~2.0, is at the uniform velocity stirred, indium sulfate or aqueous
Indium sulfate crystal all dissolves, the sulfuric acid solution of indium of the 80~100g/L containing indium prepared；
E, prepare indium sulfate electrolyte: pure 0.5~1.0g/L of gelatin is analyzed in addition in the sulfuric acid solution of indium that step d is obtained
With analysis 70~90g/L of pure sodium chloride, preparation obtains indium sulfate electrolyte.
According to the preparation method of indium sulfate electrolyte used in above-mentioned indium industry, in step a, indium liquid, which is poured into, fills distilled water
Container in when, pour into speed be 6~8g/s.
According to the preparation method of indium sulfate electrolyte used in above-mentioned indium industry, the concentrated sulfuric acid and water quenching indium flower in step b
Between additional amount ratio be 1.0~2.5:1.
According to the preparation method of indium sulfate electrolyte used in above-mentioned indium industry, in step c between distilled water and indium sulfate
The ratio of additional amount is 1:2~3.
According to the preparation method of indium sulfate electrolyte used in above-mentioned indium industry, the addition volume of distilled water is in step d
2~4 times of indium sulfate solid, aqueous sulfuric acid indium crystal total volume.
Positive beneficial effect of the invention:
1, the present invention prepares indium sulfate electrolyte method, is dissolved into indium sulfate (with 1kg indium flower dissolution time from water quenching indium flower
Meter) it can be completed in 2h, it is faster than traditional preparation method speed, 50~60 yuan/kg of energy consumption and cost of labor is saved, year electrolysis is precipitated
The manufacturing enterprise that 20 tons of indium indium sulfate electrolyte of preparing estimated every year needs water quenching indium flower 900kg or so, 500,000 yuan of left sides of energy conservation wound effect
It is right.
2, the method for the present invention indium sulfate electrolyte quota is fast, at low cost, by the new electrolyte periodic replenishment of preparation to electricity
It solves in slot, can be effectively controlled impurity in electrolyte, realize standardization electrolysis operation, it is difficult to solve enterprise's production.
3, indium sulfate electrolye analysis result and conventional method electrolye analysis Comparative result obtained by the method for the present invention, is detailed in
Table 1,2 and 3.
The new electrolyte composition (g/L) that 1 the method for the present invention of table is prepared
| pH | In | Cl | Sn | Bi | Zn | Fe | Pb | Cd | Tl |
| 1.5~2.0 | 95~110 | 52~56 | —— | —— | —— | —— | —— | —— | —— |
Electrolyte composition (g/L) after the new electrolyte periodic replenishment of 2 present invention of table
| pH | In | Cl | Sn | Bi | Zn | Fe | Pb | Cd | Tl |
| 2.0~2.3 | 80~90 | 50~55 | ≦0.001 | ≦0.01 | ≦2 | ≦0.02 | ≦0.0031 | ≦0.03 | ≦0.03 |
3 conventional method electrolye analysis (g/L) of table
After the electrolyte that conventional method is prepared periodically produces and uses, electrolyte is because evaporating and a setting loss caused by tankage out
It loses, and indium content is substantially reduced, generates partial impurities in electrolyte, the later period is supplemented only with distilled water, cannot be effective
Various impurity contents in electrolyte are controlled, the content of indium in electrolyte can not be effectively improved.And the electrolyte that the present invention prepares
After periodically producing and using, electrolyte generates partial impurities because evaporating and centainly losing caused by tankage out, and indium content is not bright
Aobvious to reduce, the later period is supplemented using the electrolyte newly prepared, and is contained so that impurity content and indium in electrolyte can be effectively controlled
Amount improves electrolyte quality so that production electrolyte impurity be made to stablize in lower range, stablizes and indium quality is precipitated, effectively improve
It is electrolysed production capacity.
Four, specific embodiment:
The present invention is further explained with reference to embodiments, but is not intended to limit the technology contents that the present invention protects.
Embodiment 1:
The indium cell bath 100L produced and used, after a cycle (7 days), because evaporating and tankage has lost out
Complete analysis is made in 20L, sampling (see Table 4 for details for analysis result).And result is analyzed according to electrolyte composition with the method for the present invention and prepares conjunction
Suitable indium sulfate electrolyte 20L.
Table 4, which takes, produces and uses indium sulfate electrolyte detection and analysis result (g/L)
| pH | In | Cl | Sn | Bi | Zn | Fe | Pb | Cd | Tl |
| 2.0 | 90 | 52 | 0.0012 | 0.013 | 1.5 | 0.033 | 0.004 | 0.037 | 0.051 |
Result is analyzed by table 4 it is found that analysis electrolyte impurity is higher, electrolyte is normal containing indium, and plan supplement 20L is newly electrolysed
Liquid, and electrolyte indium ion is stablized to 90~100g/L, while reducing electrolyte impurity, it is analysed when ensureing high current density production
Indium quality is stablized out.
Calculating preparation 20L indium sulfate electrolyte using the method for the present invention needs essence indium (purity 99.995%) 2.0~2.5kg.
Specific preparation method is as follows:
A, smart indium melt water quenching: weighing the smart indium 2.0kg of purity >=99.99%, is placed in the enamel basin that volume is 12L,
Enamel basin is placed on electric furnace plate and is heated to melting under the conditions of 200~260 DEG C, indium liquid is obtained after fusing；Steaming is filled in preparation
Gained indium liquid is poured into fill and is carried out water quenching in distilled water by the basin of distilled water with the equidirectional rotation of the speed of 6~8g/s, and water quenching obtains
Indium flower；Pull indium Hua Bingyong Adsorption of Filter Paper moisture out after ten minutes；
B, the concentrated sulfuric acid heats: weighing the pure concentrated sulfuric acid 2.5L of analysis that mass concentration is 98% and pours into enamel basin, is placed on electricity
It is heated in furnace plate, when temperature rises to 40~50 DEG C, the indium flower that step a is obtained is added portionwise in the concentrated sulfuric acid of heating, is used in combination
Pyroceram stick at the uniform velocity stirs and carries out dissolution reaction, the fully dissolved until water quenching indium is used up；After dissolution stand be cooled to 100 DEG C with
Under, with indium sulfate solid state deposition after cooling；
C, separate sulfuric acid: the unreacted concentrated sulfuric acid is assembled on indium sulfate upper layer after standing, it is poured slowly into glass beaker will
Unreacted sulfuric acid separation, is added the distilled water of 1.0L into indium sulfate after separation, stirring is separated by filtration sulfuric acid after standing；This
When, the sulfuric acid in indium sulfate is largely separated, but indium sulfate solid solution is also in highly acid, with indium sulfate solid or aqueous
The form of indium sulfate crystal exists；
D, it prepares sulfuric acid solution of indium: distilled water 15L is added in gained indium sulfate solid 5L after separating sulfuric acid to step c, so
It is slowly added to the acidity of analysis pure cerium hydroxide sodium adjustment acquired solution afterwards, the pH value for adjusting solution is 2.0, is at the uniform velocity stirred, sulfuric acid
Indium or aqueous sulfuric acid indium crystal all dissolve, the sulfuric acid solution of indium of the 80~100g/L containing indium prepared；
E, it prepares indium sulfate electrolyte: adding the gelatin and 1800g of 20g dissolution in the sulfuric acid solution of indium that step d is obtained
Sodium chloride, filtering is stood after stirring and dissolving, and preparation obtains required indium sulfate electrolyte (see Table 5 for details for analysis result).
The new indium sulfate electrolyte that 5 present invention of table prepares tests and analyzes result (g/L)
| pH | In | Cl | Sn | Bi | Zn | Fe | Pb | Cd | Tl |
| 2.0 | 94 | 52~56 | —— | —— | —— | —— | —— | —— | —— |
The 20L indium sulfate electrolyte newly prepared is mixed with remaining 80L electrolyte is produced and used, is configured to productive power solution
Liquid, see Table 6 for details for composition analysis result.
Electrolye analysis result (g/L) after table 6 mixes
| pH | In | Cl | Sn | Bi | Zn | Fe | Pb | Cd | Tl |
| 2.0 | 91 | 53 | 0.0009 | 0.01 | 1.22 | 0.027 | 0.003 | 0.03 | 0.039 |
Production electrolyte impurity can be made to stablize it follows that periodically preparing indium sulfate electrolyte using the method for the present invention
Lower range improves electrolyte quality, stablizes and indium quality is precipitated, effectively improve electrolysis production capacity.
Claims (4)
1. a kind of preparation method of indium sulfate electrolyte used in indium industry, which is characterized in that the preparation method includes following step
It is rapid:
A, smart indium melt water quenching: the smart indium of material purity >=99.99% is melted under the conditions of 200~260 DEG C, after fusing
Obtain indium liquid；The equidirectional rotation of gained indium liquid is poured into and carries out water quenching in the container for fill distilled water, obtains indium flower；
B, the concentrated sulfuric acid heats: the pure concentrated sulfuric acid of analysis that mass concentration is 98% being heated to 40~50 DEG C, then by step a water quenching
Obtained indium flower pulls viscous water suction part out from distilled water, and at the uniform velocity stirring is then added portionwise in the concentrated sulfuric acid of heating and dissolve instead
It answers, the fully dissolved until water quenching indium is used up；Cooling is stood after dissolution, with indium sulfate solid state deposition after cooling；
C, it separates sulfuric acid: sulfuric acid unreacted in step b being separated by filtration first, distilled water is then added into indium sulfate, into
One step is separated by filtration sulfuric acid；The volume ratio of the distilled water and indium sulfate is 1:2~3；After separation, indium sulfate is with indium sulfate solid
Or the form of aqueous sulfuric acid indium crystal exists；
D, it prepares sulfuric acid solution of indium: distilled water is added in the indium sulfate after separating sulfuric acid to step c, it is pure to be then slowly added into analysis
Sodium hydroxide adjusts the acidity of acquired solution, and the pH value for controlling solution is 1.5~2.0, at the uniform velocity stirs, indium sulfate or aqueous sulfuric acid
Indium crystal all dissolves, the sulfuric acid solution of indium of the 80~100g/L containing indium prepared；
E, prepare indium sulfate electrolyte: addition is analyzed pure 0.5~1.0g/L of gelatin and is divided in the sulfuric acid solution of indium that step d is obtained
70~90g/L of pure sodium chloride is analysed, preparation obtains indium sulfate electrolyte.
2. the preparation method of indium sulfate electrolyte used in indium industry according to claim 1, it is characterised in that: in step a
When indium liquid is poured into the container for fill distilled water, pouring into speed is 6~8g/s.
3. the preparation method of indium sulfate electrolyte used in indium industry according to claim 1, it is characterised in that: in step b
The ratio of additional amount is 1.0~2.5:1 between the concentrated sulfuric acid and water quenching indium flower.
4. the preparation method of indium sulfate electrolyte used in indium industry according to claim 1, it is characterised in that: in step d
The addition volume of distilled water is indium sulfate solid, 2~4 times of aqueous sulfuric acid indium crystal total volume.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1490433A (en) * | 2002-10-16 | 2004-04-21 | 沈奕林 | Preparation of high purity indium |
| CN102092781A (en) * | 2010-12-10 | 2011-06-15 | 株洲冶炼集团股份有限公司 | Method for preparing battery grade indium hydroxide and indium oxide |
| CN102943284A (en) * | 2012-12-07 | 2013-02-27 | 株洲科能新材料有限责任公司 | Preparation method of indium electrolyte solution |
| CN103103566A (en) * | 2013-01-31 | 2013-05-15 | 湖南化工研究院 | Preparation method of high-purity indium |
| CN103880065A (en) * | 2014-04-14 | 2014-06-25 | 清远先导材料有限公司 | Method and device for preparing indium sulfate |
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- 2017-08-30 CN CN201710763994.6A patent/CN107460501B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1490433A (en) * | 2002-10-16 | 2004-04-21 | 沈奕林 | Preparation of high purity indium |
| CN102092781A (en) * | 2010-12-10 | 2011-06-15 | 株洲冶炼集团股份有限公司 | Method for preparing battery grade indium hydroxide and indium oxide |
| CN102943284A (en) * | 2012-12-07 | 2013-02-27 | 株洲科能新材料有限责任公司 | Preparation method of indium electrolyte solution |
| CN103103566A (en) * | 2013-01-31 | 2013-05-15 | 湖南化工研究院 | Preparation method of high-purity indium |
| CN103880065A (en) * | 2014-04-14 | 2014-06-25 | 清远先导材料有限公司 | Method and device for preparing indium sulfate |
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Denomination of invention: A preparation method of electrolytic indium sulfate solution used in indium industry Effective date of registration: 20221230 Granted publication date: 20190730 Pledgee: Bank of China Limited by Share Ltd. Jiyuan branch Pledgor: HENAN YUGUANG ZINC INDUSTRY Co.,Ltd. Registration number: Y2022980029760 |