CN103160855A - Preparation method of high-purity indium - Google Patents
Preparation method of high-purity indium Download PDFInfo
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- CN103160855A CN103160855A CN2011104229800A CN201110422980A CN103160855A CN 103160855 A CN103160855 A CN 103160855A CN 2011104229800 A CN2011104229800 A CN 2011104229800A CN 201110422980 A CN201110422980 A CN 201110422980A CN 103160855 A CN103160855 A CN 103160855A
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Abstract
The invention provides a preparation method of high-purity indium. The method comprises: preparing an indium sulfate solution as an electrolyte, filling the prepared electrolyte into an electrolytic tank, preparing the indium raw material as a positive plate and a negative plate of the electrolytic tank, respectively putting the positive plate and the negative plate into an anode area and a cathode area of the electrolytic tank, and starting an electrolytic cycle of the electrolytic tank for direct current electrolysis so as to obtain electrolyzed indium on the negative plate. The preparation method of the high-purity indium enables a content of impurities difficult to be removed in the indium to be low, can prepare 5N indium, and is simple in production technology, large in production capacity of single set of equipment, energy saving and environmental protective.
Description
Technical field
The present invention relates to a kind of preparation method of high pure metal, relate in particular to a kind of preparation method of high purity indium.
Background technology
Indium (In) belongs to dissipated metal, is positioned at periodictable IIIA family, and ordination number is 49, and relative atomic mass is 114.82.Indium presents silvery white, and strong metal gloss is arranged, and plasticity-is larger, and ductility is good.Indium dissolves in mineral acid, can form alloy with various metals simultaneously.
Indium is a kind of multiduty metal, is widely used in the fields such as oxidation Indium Tin (Indium Tin Oxide is abbreviated as ITO) material, infrared detecting materials, Hall element, photovoltaic solar generation technology.Along with the development of new high-tech industry, the Application Areas of high purity indium is increasingly extensive in recent years.
The method for preparing at present high purity indium is many, and the precipitator method, ion exchange method, extraction process, electrolytic process, vacuum heat treatment method, crystallization process, Organometallic compound method and subhalide method etc. are arranged.
The precipitator method comprise precipitation of indium and precipitated impurities two aspects, but it is more difficult to prepare high purity indium.
Ion exchange method with obtaining spongiform indium after the aluminium displacement, is then carried out electrorefining with the sponge indium first with the ion exchange method indiumchloride solution of purifying, more than the purity of product can reach 5N, but the technical process more complicated.
Extraction process is after carrying out reextraction with ether, contain solution of indium with ammonia neutralization, generate the indium hydroxide precipitation, with this precipitation with hydrogen reduction or be made into electrolytic solution and carry out electrolysis and can obtain purity greater than the product of 5N, the method operation more complicated can cause certain pollution.
The vacuum distilling method is that indium is heated under vacuum condition, volatile impunty is separated, but S, Se and Te has higher avidity to indium, can not separate by time method.Crystallization process is actually zone melting and melting crystal method of purification, usually carries out in the final stage of indium deep purifying.
The organic method of metal is that preparation of metals is become organometallics, and is with remove portion impurity, larger but this method is polluted.
The subhalide method is the halogenide by indium, and particularly subhalide method purifying indium, separate out indium by the disproportionation reaction of indium by the subhalide of purifying, and the method reaction is difficult to control.
Electrolytic process is method the most commonly used on industrial production, adopt the method to be prepared into more than high purity indium can reach 6N, and industrial production is simpler.
Disclosed Chinese invention patent application publication number CN1221800A disclosed a kind of method of extracting indium from iron vitriol slag on July 7th, 1999, the method is with the iron vitriol slag roasting and leaches, then obtain the indium ingot of 4N through extraction and back-extraction, the purity of the indium that employing the method obtains is lower.
Disclosed Chinese invention patent application publication number CN1490433A disclosed a kind of method that adopts electrochemistry refining-vacuum distilling-electrochemistry refining to unite purification and has prepared high purity indium on April 21st, 2004, adopted the method can obtain the 6N product.The required technique of the method is more complicated, and is unfavorable for realizing suitability for industrialized production.
In addition, in the system electrolysis process, in indium the content of troublesome impurity higher as, Sn, Fe, Cu Ni, Pb etc.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of high purity indium, it can process troublesome impurity in indium, thereby has reduced the content of troublesome impurity, has improved purity.
Another object of the present invention is to provide a kind of preparation method of high purity indium, it can simplify technique, is conducive to suitability for industrialized production.
Another object of the present invention is to provide a kind of preparation method of high purity indium, it can prepare the 5N indium.
In order to reach purpose of the present invention, the invention provides a kind of preparation method of high purity indium, comprise step: preparation indium sulfate solution is as electrolytic solution; The electrolytic solution of preparation is packed in electrolyzer; The indium raw material is made as positive plate and the negative plate of electrolyzer; Positive plate and negative plate are respectively charged in the positive column and cathodic area of electrolyzer; And the electrolysis cycle that starts electrolyzer, carry out dc electrolysis, obtain the electrolysis indium on negative plate.
Beneficial effect of the present invention is as follows.
Compare traditional electrolysis process, the preparation method of high purity indium of the present invention can make the content of troublesome impurity in the indium of preparation low.
The preparation method of high purity indium of the present invention can prepare the 5N indium.
Preparation method's production technique of high purity indium of the present invention is simple, and single complete equipment production capacity is large, energy-conserving and environment-protective.
Description of drawings
Fig. 1 has provided the schema according to the preparation method of high purity indium of the present invention.
Wherein, description of reference numerals is as follows:
S1, S2, S3, S4, S5 step
Embodiment
Below in conjunction with the preparation method of description of drawings according to high purity indium of the present invention.
As shown in Figure 1, the preparation method according to high purity indium of the present invention comprises step: preparation indium sulfate solution is as electrolytic solution (step S1); With the electrolytic solution of preparation pack into (step S2) in electrolyzer; The indium raw material is made as positive plate and the negative plate (step S3) of electrolyzer; Positive plate and negative plate are respectively charged in the positive column and cathodic area of described electrolyzer (step S4); And the electrolysis cycle that starts electrolyzer, carry out dc electrolysis, to obtain electrolysis indium (step S5) on negative plate.
In step S1, preferably, in indium sulfate solution, indium ion concentration is 10～100g/L, and sulfuric acid concentration is 10～20g/L.Preparation indium sulfate solution can be not limited to this certainly by the 5N indium as raw material, as long as can reach desired concn.
In step S1, preferably, the temperature of electrolytic solution is 20～50 ℃.
In step S3, preferably, the indium raw material is the 4N indium.
In step S3, preferably, the interpole gap between the homonymy electrode plate in electrolyzer is 1～40cm.Wherein, interpole gap refers to the distance between homonymy electrode plate (being all positive plate or negative plate) center in staggered many antianodes plate and negative plate.
In step S5, preferably, the current density of dc electrolysis is 100～400A/m
2The required direct current of dc electrolysis can be undertaken by the rectifier that is arranged on the electrolytic tank electrolysis circulation path.
Next, embodiment according to the preparation method of high purity indium of the present invention is described.
Embodiment 1
Preparation indium sulfate solution is as electrolytic solution, wherein: indium ion concentration is 70g/L, and sulfuric acid concentration is 10g/L, and electrolyte temperature is 30 ℃; The electrolytic solution of preparation is packed in electrolyzer; 4N indium raw material is made as positive plate and the negative plate of electrolyzer; Positive plate and negative plate are respectively charged in the positive column and cathodic area of electrolyzer, and wherein interpole gap is 20cm; Start the electrolysis cycle of electrolyzer, carry out dc electrolysis, to obtain the electrolysis indium on negative plate, wherein current density is 100A/m
2
Embodiment 2
Preparation indium sulfate solution is as electrolytic solution, wherein: indium ion concentration is 100g/L, and sulfuric acid concentration is 20g/L, and electrolyte temperature is 40 ℃; The electrolytic solution of preparation is packed in electrolyzer; 4N indium raw material is made as positive plate and the negative plate of electrolyzer; Positive plate and negative plate are respectively charged in the positive column and cathodic area of electrolyzer, and wherein interpole gap is 18cm; Start the electrolysis cycle of electrolyzer, carry out dc electrolysis, to obtain the electrolysis indium on negative plate, wherein current density is 180A/m
2
Embodiment 3
Preparation indium sulfate solution is as electrolytic solution, wherein: indium ion concentration is 90g/L, and sulfuric acid concentration is 16g/L, and electrolyte temperature is 45 ℃; The electrolytic solution of preparation is packed in electrolyzer; 4N indium raw material is made as positive plate and the negative plate of electrolyzer; Positive plate and negative plate are respectively charged in the positive column and cathodic area of electrolyzer, and wherein interpole gap is 15cm; Start the electrolysis cycle of electrolyzer, carry out dc electrolysis, to obtain the electrolysis indium on negative plate, wherein current density is 170A/m
2
Embodiment 4
Preparation indium sulfate solution is as electrolytic solution, wherein: indium ion concentration is 10g/L, and sulfuric acid concentration is 10g/L, and electrolyte temperature is 20 ℃; The electrolytic solution of preparation is packed in electrolyzer; 4N indium raw material is made as positive plate and the negative plate of electrolyzer; Positive plate and negative plate are respectively charged in the positive column and cathodic area of electrolyzer, and wherein interpole gap is 1cm; Start the electrolysis cycle of electrolyzer, carry out dc electrolysis, to obtain the electrolysis indium on negative plate, wherein current density is 100A/m
2
Embodiment 5
Preparation indium sulfate solution is as electrolytic solution, wherein: indium ion concentration is 100g/L, and sulfuric acid concentration is 20g/L, and electrolyte temperature is 50 ℃; The electrolytic solution of preparation is packed in electrolyzer; 4N indium raw material is made as positive plate and the negative plate of electrolyzer; Positive plate and negative plate are respectively charged in the positive column and cathodic area of electrolyzer, and wherein interpole gap is 40cm; Start the electrolysis cycle of electrolyzer, carry out dc electrolysis, to obtain the electrolysis indium on negative plate, wherein current density is 400A/m
2
Provide at last test result.
Adopt icp ms (ICP-MS) to detect that (manufacturer is PE company, and model is: DRC-II), the testing conditions of this equipment is: temperature is 18 ℃-28 ℃, and relative humidity is 30-70%, and cleanliness factor is 1000 grades.Detect principle: the icp ms detection mode: element to be measured enters mass analyzer with the positive charge form after ionizing through plasma high-temperature, and the difference according to the mass/charge ratio is received by detector, produces signal.Signal and this element signal ratio of reference material that element to be measured produces draw constituent content to be measured.
Table 1 has provided the test result of embodiment 1-5.As seen from Table 1, the foreign matter content of the electrolysis indium of embodiment 1-5 is low, and all the quality of electrolysis indium reaches the 5N standard.
Foreign matter content (the unit: ppm) of the electrolysis indium of table 1 embodiment 1-5
Claims (7)
1. the preparation method of a high purity indium, is characterized in that, comprises step:
Preparation indium sulfate solution is as electrolytic solution;
The electrolytic solution of preparation is packed in electrolyzer;
The indium raw material is made as positive plate and the negative plate of electrolyzer;
Positive plate and negative plate are respectively charged in the positive column and cathodic area of electrolyzer; And
Start the electrolysis cycle of electrolyzer, carry out dc electrolysis, obtain the electrolysis indium on negative plate.
2. the preparation method of high purity indium according to claim 1, is characterized in that, described preparation indium sulfate solution by the 5N indium as raw material.
3. the preparation method of high purity indium according to claim 1, is characterized in that, in described indium sulfate solution, indium ion concentration is 10～100g/L, and sulfuric acid concentration is 10～20g/L.
4. the preparation method of high purity indium according to claim 1, is characterized in that, the temperature of described electrolytic solution is 20～50 ℃.
5. the preparation method of high purity indium according to claim 1, is characterized in that, described indium raw material is the 4N indium.
6. the preparation method of high purity indium according to claim 1, is characterized in that, the interpole gap between the homonymy electrode plate in described electrolyzer is 1～40cm.
7. the preparation method of high purity indium according to claim 1, is characterized in that, the current density of described dc electrolysis is 100～400A/m
2
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| CN2011104229800A CN103160855A (en) | 2011-12-15 | 2011-12-15 | Preparation method of high-purity indium |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103498051A (en) * | 2013-09-30 | 2014-01-08 | 昆明理工大学 | Method for recovering copper and nickel from nickel-iron-copper alloy waste |
| CN106757157A (en) * | 2016-12-12 | 2017-05-31 | 贵州宏达环保科技有限公司 | One kind reclaims thick indium method from indium purification slag |
| CN107354485A (en) * | 2017-09-12 | 2017-11-17 | 武汉峰则惠电子材料股份有限公司 | A kind of method that electrorefining prepares high purity indium |
| CN108085518A (en) * | 2017-12-21 | 2018-05-29 | 广东先导先进材料股份有限公司 | A kind of preparation method of vacuum distillation plant and super high purity indium |
| CN110863216A (en) * | 2019-10-28 | 2020-03-06 | 中南大学 | Method for preparing high-purity indium through step cyclone electrodeposition |
| CN111118545A (en) * | 2019-11-28 | 2020-05-08 | 广东先导稀材股份有限公司 | Preparation method of high-purity indium |
| CN114561670A (en) * | 2022-03-28 | 2022-05-31 | 云南锡业集团（控股）有限责任公司研发中心 | High-purity indium electrolysis device and electrolysis method thereof |
| CN114875451A (en) * | 2022-06-08 | 2022-08-09 | 广东先导稀材股份有限公司 | Indium sulfate electrolyte and preparation method thereof |
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| CN101104890A (en) * | 2007-06-11 | 2008-01-16 | 华南师范大学 | Method for recycling indium from waste mercury-free alkaline zinc-manganese dioxide battery |
| CN101892495A (en) * | 2010-06-29 | 2010-11-24 | 葫芦岛锌业股份有限公司 | Method for producing 4N5 pure indium by electrolyzing high impurity crude indium once |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103498051A (en) * | 2013-09-30 | 2014-01-08 | 昆明理工大学 | Method for recovering copper and nickel from nickel-iron-copper alloy waste |
| CN106757157A (en) * | 2016-12-12 | 2017-05-31 | 贵州宏达环保科技有限公司 | One kind reclaims thick indium method from indium purification slag |
| CN106757157B (en) * | 2016-12-12 | 2018-09-25 | 贵州宏达环保科技有限公司 | One kind recycling thick indium method from indium purification slag |
| CN107354485A (en) * | 2017-09-12 | 2017-11-17 | 武汉峰则惠电子材料股份有限公司 | A kind of method that electrorefining prepares high purity indium |
| CN108085518A (en) * | 2017-12-21 | 2018-05-29 | 广东先导先进材料股份有限公司 | A kind of preparation method of vacuum distillation plant and super high purity indium |
| CN110863216A (en) * | 2019-10-28 | 2020-03-06 | 中南大学 | Method for preparing high-purity indium through step cyclone electrodeposition |
| CN110863216B (en) * | 2019-10-28 | 2020-12-11 | 中南大学 | Method for preparing high-purity indium through step cyclone electrodeposition |
| CN111118545A (en) * | 2019-11-28 | 2020-05-08 | 广东先导稀材股份有限公司 | Preparation method of high-purity indium |
| CN114561670A (en) * | 2022-03-28 | 2022-05-31 | 云南锡业集团（控股）有限责任公司研发中心 | High-purity indium electrolysis device and electrolysis method thereof |
| CN114875451A (en) * | 2022-06-08 | 2022-08-09 | 广东先导稀材股份有限公司 | Indium sulfate electrolyte and preparation method thereof |
| CN114875451B (en) * | 2022-06-08 | 2024-02-27 | 先导电子科技股份有限公司 | Indium sulfate electrolyte and preparation method thereof |
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Application publication date: 20130619 |