CN100570008C - The preparation method of indium sulfate - Google Patents
The preparation method of indium sulfate Download PDFInfo
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- CN100570008C CN100570008C CNB2007100312906A CN200710031290A CN100570008C CN 100570008 C CN100570008 C CN 100570008C CN B2007100312906 A CNB2007100312906 A CN B2007100312906A CN 200710031290 A CN200710031290 A CN 200710031290A CN 100570008 C CN100570008 C CN 100570008C
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Abstract
The present invention relates to a kind of preparation method of high-purity indium sulfate, mainly comprise the steps: it at first is preparation indium sulfate solution; Be the condensing crystal of indium sulfate solution then; Be the vacuum crystallization of indium sulfate at last.The present invention carries out impurity and purification and handles in preparation indium sulfate solution, improved the purity of indium sulfate solution; Adopt the technical scheme of secondary crystal, guaranteed the sufficient crystallising of indium sulfate solution, make indium sulfate solution be converted into the indium sulfate crystal as far as possible fully, transformation efficiency reaches 70%; Shorten technical process, reduced the loss of indium in process of production, saved the indium resource.
Description
[technical field]
The invention belongs to chemical field, relate to the method that a kind of 4N of utilization indium ingot is produced indium sulfate.
[background technology]
Explanation of nouns: ITO (Indium Tin Oxide) is the n N-type semiconductorN of a kind of heavy doping, high degeneracy, and it has optics, chemistry and the electric property of a series of excellences.
4N indium ingot: purity is greater than the smart indium more than 99.99%, and wherein the total impurities sum is less than 100PPM (PPM: 1,000,000/), and Cd＜10PPM, Sn＜15, Pb＜10PPM, Tl＜10ppm, and other elements are less than the high purity indium of 5PPM.
Indium sulfate is widely used in fields such as electroplating industry, preparation TTO composite powder and evaporation ITO conducting film, because indium resource rare and costing an arm and a leg, for guaranteeing to obtain the best product performance with the least possible indium consumption, the indium compound Application Areas is very high to its quality requirements using.At present, the preparation method of indium sulfate rarely has report, in Chinese patent, does not also have indium sulfate preparation method's patent application.Indium sulfate production process commonly used comprises the following steps: it at first is preparation indium sulfate solution, and common preparation method has membrane electrolysis, directly sulfuric acid dissolution preparation; Condensing crystal uses reactor that the indium sulfate solution of preparation is carried out condensing crystal then; Utilize at last and contain the saturated indium sulfate solution of crystalline after vacuumizing suction filtration or using the filter cloth filtering and concentrating, filter and obtain the indium sulfate crystal and do not have the saturated filtrate of complete crystalline, wherein filtering the crystal that obtains is exactly the indium sulfate product.
Take above-mentioned production technique to prepare indium sulfate solution, the common electrical solution is owing to will use as utility appliance such as electrolysis power, electrode, diaphragm sells, because the different Faradaic current that causes of pH value at negative electrode and anode place is little in electrolytic process, thereby exist the production cycle long, the indium sulfate strength of solution that obtains is low, and electrolysis voltage changes in electrolytic process, after indium sulfate concentration acquires a certain degree the hydrolysis phenomenon takes place, the indium sulfate solution quality instability of preparation, the not high shortcoming of purity.Directly the acid dissolving is because the overpotential of indium is very big, and in fact block indium is difficult to dissolving when dissolving, actual and infeasible in process of production.In addition, also there is employing the molten metal indium to be poured into the indium that obtains high-specific surface area in the water, prepare indium sulfate solution with sulfuric acid dissolution then, this method is influenced by human factor in producing the indium sulfate process because during operation, the specific surface area fluctuation of the high-ratio surface indium that obtains is very big, because the variation of processing parameter such as best sulfuric acid concentration when the variation of specific surface causes dissolution time and dissolving, and can't accurately control the preparation technology parameter of indium sulfate solution.
In a word, the subject matter that the method for existing preparation indium sulfate exists is: the foreign matter content of product is higher, dissolving clarity is not enough, contain suspended impurity, the apparent jaundice of product blackout, the finished product rate is low, crystallization transformation efficiency only 40%～50%, production cost is high, exists the indium resource inevitably to lose simultaneously.
[summary of the invention]
In order to overcome the above-mentioned shortcoming of prior art, the invention provides a kind ofly shortened technical process, improved indium sulfate crystalline transformation efficiency, reduced indium loss, reduced production cost, improved the preparation method of the indium sulfate of indium sulfate finished product purity.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of indium sulfate mainly comprises the steps:
The first step is a preparation indium sulfate solution: 4N high pure metal indium is cast metallic anode plate, carry out electrolytic preparation indium sulfate solution in molten being diluted to 20%～70% analytical pure sulfuric acid, then indium sulfate solution is filtered;
Second step was the condensing crystal of indium sulfate solution: will heat under agitation condition through the indium sulfate solution that the first step has purified, after mass crystallization occurring, said mixture all emitted and continue crystallization at ambient temperature;
The 3rd step was the vacuum crystallization of indium sulfate: the indium sulfate that second step was produced stirs fully, and mixture carries out heat tracing under vacuum condition, directly obtain pulverous indium sulfate product.
In described the first step production technique, the sulfuric acid amount that is added and the mol ratio of indium are 1: 1.1～1: 1.3, and electrolysis time 10～30 hours, electrolysis voltage are 0.2～1.2 volt; Adopt the bidirectional pulse power supply, supply frequency 50～20000Hz, negative plate and positive plate are 4N indium metal plate.
In the described second step production technique, type of heating adopts electrically heated or steam-heated mode, and Heating temperature is 70 ℃～130 ℃, and stirring velocity is 50～120 rev/mins.
In described the 3rd step production technique, vacuum tightness is 1 * 10
-1～1 * 10
-3Pa, Heating temperature is 90～160 ℃, soaking time is 10～40 hours.
The invention has the beneficial effects as follows: in preparation indium sulfate solution, carry out impurity and purification and handle, improved the purity of indium sulfate solution; Adopt the technical scheme of secondary crystal, guaranteed the sufficient crystallising of indium sulfate solution, make indium sulfate solution be converted into the indium sulfate crystal as far as possible fully, transformation efficiency reaches 70%; Shorten technical process, reduced the loss of indium in process of production, saved the indium resource.
[description of drawings]
Fig. 1 is a technical process block diagram of the present invention.
[embodiment]
The present invention is further described below in conjunction with drawings and Examples.
Embodiment 1:
Referring to Fig. 1, get 100 kilograms of indium metal, positive plate is cast in fusing, gets 60 liters of 200 liters of high purity waters and analytical pure sulfuric acids, is configured to electrolytic solution, carries out electrolysis, electrolysis time 24 hours, the indium sulfate solution that obtains purifying under the condition of 0.5 volt of groove pressure; The indium sulfate solution that obtains is joined in the reactor, under 110 ℃ condition, be concentrated into and begin to occur crystallization, under heated condition, emit enriched product; The indium sulfate of producing is stirred fully, be placed into then and be evacuated to 1.5 * 10 in the vacuum tank
-3Pa is heated to 140 ℃, is incubated taking-up in 12 hours, obtains the finished product indium sulfate; Final product detects qualified back packing.
Embodiment 2:
Referring to Fig. 1, get 50 kilograms of indium metal, positive plate is cast in fusing, gets 100 liters of high purity waters, and analytical pure sulfuric acid is configured to electrolytic solution for 30 liters, electrolysis under the condition of 0.4 volt of groove pressure, electrolysis 30 hours, the indium sulfate solution that obtains purifying; The indium sulfate solution that obtains joined to be concentrated under 100 ℃ condition in the reactor begin to occur crystallization, under heated condition, emit enriched product; The indium sulfate of producing is stirred fully, be placed into then and be evacuated to 1.0 * 10 in the vacuum tank
-3Pa is heated to 130 ℃, is incubated taking-up in 20 hours, obtains the finished product; Final product detects qualified back packing.
The present invention adopts the reasonable control of suitable acid concentration and Faradaic current, can prevent that other trace metal impurities in the indium is dissolved out in the process of preparation indium sulfate solution, in the indium sulfate solution that obtains, has played the effect that purifies indium sulfate solution.Cleaning principle can be expressed as:
In-3e＝In
3+
Thereby in above-mentioned electrolytic process, owing to can not discharge resulting indium sulfate solution is further purified than the high heavy metal element of indium current potential.In appropriate acidity, temperature with reasonably under the current density, the indium sulfate solution that can be fully purified.
Claims (4)
1, a kind of preparation method of indium sulfate is characterized in that: mainly comprise the steps:
The first step is a preparation indium sulfate solution: 4N high pure metal indium is cast metallic anode plate, carry out electrolytic preparation indium sulfate solution in being diluted to 20%～70% analytical pure sulfuric acid solution, then indium sulfate solution is filtered;
Second step was the condensing crystal of indium sulfate solution: will heat under agitation condition through the indium sulfate solution that the first step has purified, after mass crystallization occurring, said mixture all emitted and continue crystallization at ambient temperature;
The 3rd step was the vacuum crystallization of indium sulfate: the indium sulfate that second step was produced stirs, and mixture carries out heat tracing under vacuum condition, directly obtain pulverous indium sulfate product.
2, the preparation method of indium sulfate as claimed in claim 1 is characterized in that: in described the first step production technique, the sulfuric acid amount that is added and the mol ratio of indium are 1: 1.1～1: 1.3, and electrolysis time 10～30 hours, electrolysis voltage are 0.2～1.2 volt; Adopt the bidirectional pulse power supply, supply frequency 50～20000Hz, negative plate and positive plate are 4N indium metal plate.
3, the preparation method of indium sulfate as claimed in claim 1 is characterized in that: in the described second step production technique, type of heating adopts electrically heated or steam-heated mode, and Heating temperature is 70 ℃～130 ℃, and stirring velocity is 50～120 rev/mins.
4, the preparation method of indium sulfate as claimed in claim 1 is characterized in that: in described the 3rd step production technique, vacuum tightness is 1 * 10
1～1 * 10
-3Pa, Heating temperature is 90～160 ℃, soaking time is 10～40 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100312906A CN100570008C (en) | 2007-11-08 | 2007-11-08 | The preparation method of indium sulfate |
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|---|---|---|---|
| CNB2007100312906A CN100570008C (en) | 2007-11-08 | 2007-11-08 | The preparation method of indium sulfate |
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| CN101235508A CN101235508A (en) | 2008-08-06 |
| CN100570008C true CN100570008C (en) | 2009-12-16 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491406B (en) * | 2011-11-24 | 2013-08-14 | 中国铝业股份有限公司 | Method for preparing gallium sulfate |
| CN103046108B (en) * | 2012-12-24 | 2017-03-29 | 上海申和热磁电子有限公司 | Application of the electrolysis process in ito film is cleaned |
| CN103880065B (en) * | 2014-04-14 | 2015-09-30 | 清远先导材料有限公司 | A kind of indium sulfate preparation method and device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1233585A (en) * | 1998-03-30 | 1999-11-03 | 三菱瓦斯化学株式会社 | Process for producing persulfate |
| CN1723299A (en) * | 2002-12-06 | 2006-01-18 | Om集团公司 | Electrolytic process for preparing metal sulfonates |
-
2007
- 2007-11-08 CN CNB2007100312906A patent/CN100570008C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1233585A (en) * | 1998-03-30 | 1999-11-03 | 三菱瓦斯化学株式会社 | Process for producing persulfate |
| CN1723299A (en) * | 2002-12-06 | 2006-01-18 | Om集团公司 | Electrolytic process for preparing metal sulfonates |
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| CN101235508A (en) | 2008-08-06 |
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