KR20170027588A - Production of High-purity Indium Oxide from Indium Scrape - Google Patents
Production of High-purity Indium Oxide from Indium Scrape Download PDFInfo
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- KR20170027588A KR20170027588A KR1020150124408A KR20150124408A KR20170027588A KR 20170027588 A KR20170027588 A KR 20170027588A KR 1020150124408 A KR1020150124408 A KR 1020150124408A KR 20150124408 A KR20150124408 A KR 20150124408A KR 20170027588 A KR20170027588 A KR 20170027588A
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- C01G15/00—Compounds of gallium, indium or thallium
Abstract
Description
The present invention relates to a method for producing high purity indium oxide from indium scrap, and more particularly to a method for producing high purity indium oxide from indium scrap. More particularly, the present invention relates to a method for producing high purity indium oxide from indium scrap, And a high purity indium oxide produced by the method.
As the information and communication industry develops, there is a growing demand for the development of new electronic materials. As the electronic devices become smaller and thinner, the metal oxide processing technology and the thin film manufacturing technology are secured. It became a problem.
On the other hand, indium is used for intermetallic compounds such as InP and InAs, which are III-V compound semiconductors, or indium oxide (ITO) doped with tin, which is a material for solar cells, and transparent conductive thin films. .
Originally, indium has no major ore and is industrially produced by the by-product of zinc smelting and lead smelting, for example, by recovering concentrated indium in soot. Therefore, the raw material for the indium recovery contains a large amount of metal impurities such as Zn, Fe, Cu, Al, Ga, As, and Cd, and many other kinds of components are contained in trace amounts in addition to these metal components.
Therefore, complicated processes are required to recover indium of high purity by removing these metal impurities. In general, in the above-mentioned indium recovery process, a method of precipitating as a hydroxide by adjusting the pH, A precipitation method, a method of substitution deposition by addition of metal Al, Zn, Cd, or a Zn-Cd alloy, a method of recovering indium by solvent extraction, and a method of recovering indium by ion exchange And is combined with a smelting method.
However, the method of precipitating as hydroxide by pH adjustment in the recovery process is based on the difference in the pH range of the hydroxide formation pH of the metal ion. For example, when the pH is set to 12 or more as a separation method of Zn, Al and In, Zn and Al are dissolved Thereby precipitating In as hydroxide and recovering it. However, in this method, since the produced hydroxide of In is very poor in filtration property, the filtration equipment becomes large and the operation becomes long. Further, in this method, it is difficult to separate impurities such as Fe, Cu, As, Cd, and In from In.
The method of precipitating sulfides by adding the sulfiding agent is based on the difference in solubility of the metal sulfides, but a large amount of sulfides having a low purity is generated because it contains various metal impurities as described above. These sulfides generally have poor filtration properties, and when the obtained In sulfide is leached, In can not be completely leached out with sulfuric acid alone, which is a drawback that this method is difficult to apply to a wet zinc process.
In addition, the method of substitution deposition by adding the metal Al, Zn, Cd, Zn-Cd alloy or the like has a problem that it is impossible to separate In from the metal if it contains impurities that are more valuable than indium.
In addition, the method of recovering indium by the solvent extraction or the method of recovering indium by the ion exchange method is burdensome for the pretreatment depending on the impurities which are separated from In, and there is also a problem that the operation cost is high.
In any chemical purification method described above, separation of impurity metals is insufficient. Therefore, the electrolytic smelting method combined with the electrolytic smelting method can also be easily carried out by a simple electrolytic extraction method (electrolysis using an insoluble anode by leaching a target metal in an aqueous solution, A metal is obtained), and a complicated electrolytic refining method (refining the electrolytic solution of a coarse metal as a positive electrode and a high-purity metal as a negative electrode) can not be employed.
Therefore, any of the above methods has drawbacks, and the combination of the above methods is used for the actual number of times. In order to recover high-purity In, the process becomes complicated and cumbersome.
In addition, the conventional indium refining technology has a disadvantage in that a large amount of waste acid is generated to cause environmental pollution, and the process is complicated and expensive. In order to overcome this problem, the solvent extraction method is used to recover high purity indium metal (99.995%). However, the cost of the solvent extraction agent is high, the initial investment and operation cost are high, and environmental pollution problems may occur. Further, in order to convert metal indium to indium oxide, various processes such as acid dissolution, hydroxide formation, washing, filtration, drying and calcination are required, which is disadvantageous in that it is expensive.
The present invention relates to a method for producing high purity indium oxide from indium scrap which can obtain high purity indium oxide by pulverizing indium scrap of a low grade and producing colloidal particles and then crystallizing the colloidal particles and oxidizing them in the air, Purity indium oxide.
It is another object of the present invention to provide a process for producing high purity indium oxide from indium scrap using indium scrap which can recycle indium scrap without causing waste acid and which is easy to work, eco-friendly and economical, and to provide high purity indium oxide .
The various problems to be solved by the present invention are not limited to the above-mentioned problems, and other problems not mentioned can be clearly understood by those skilled in the art from the following description.
The method for producing high purity indium oxide from indium scrap according to the present invention comprises the steps of (S100) crushing an indium scrap for pulverizing an indium scrap into a predetermined size to be pulverized; (S110) dissolving the indium scrap and removing residues of the insoluble fractions by injecting an inorganic acid into the pulverized and pulverized indium scrap; A precipitant input and metal hydroxide precipitation step (S120) for precipitating a metal hydroxide in a pH range of 3 to 9 by adding a precipitant to the acid solution from which the insoluble residue is removed; An organic acid addition and crystallization step (S130) of adding an organic acid to the metal hydroxide to crystallize the metal oxalate; And an indium oxide production step (S140) of oxidizing the crystallized metal oxalate in air to produce indium oxide.
In step (S100), the indium scrap may be pulverized into a size of 180 to 220 mesh.
The indium scrap melting and the inorganic acid in the residue removing step (S110) is to 100 parts by weight of indium scrap powder by 300 to 900 parts by weight is used, the mineral acid is hydrochloric acid (HCl), nitric acid (HNO 3), sulfuric acid (H 2 SO 4 ) and aqua regia (HCO 3 and HNO 3 mixed at a weight ratio of 3: 1) can be used.
In the step of depositing the precipitant and depositing the metal hydroxide (S120), any one selected from ammonia, urea, sodium hydroxide, and potassium hydroxide may be used as the precipitant.
The organic acid may be used in an amount of 0.5 to 3.0 M in the organic acid addition and crystallization step (S120), and the organic acid may be selected from citric acid and oxalic acid.
In addition, the method for producing high purity indium oxide from indium scrap according to the present invention comprises: a step of injecting a precipitant and depositing a metal hydroxide (S200) for precipitating a metal hydroxide in a pH range of 3 to 9 by injecting a precipitant into washings waste; An organic acid addition and crystallization step (S210) of introducing an organic acid into the metal hydroxide to crystallize the metal oxalate; And an indium oxide preparation step (S220) of oxidizing the crystallized metal oxalate to produce indium oxide of high purity, wherein the precipitation agent is selected from ammonia, urea, sodium hydroxide or potassium hydroxide, 0.5 to 3.0 M of organic acid is used, and any one selected from citric acid and oxalic acid is used as the organic acid.
In addition, the method for producing high purity indium oxide from indium scrap according to the present invention includes: an organic acid input and crystallization step (S300) of adding an organic acid to the waste ITO powder to crystallize the metal oxalate; And a step (S310) of producing an indium oxide in which high-purity indium oxide is produced by oxidizing the crystallized metal oxalate in the air, wherein 0.5 to 3.0 M of the organic acid is used, and the organic acid is selected from citric acid or oxalic acid One is used.
The present invention also includes high purity indium oxide produced by the above-described production method.
The details of other embodiments are included in the detailed description.
In the method for producing high purity indium oxide from indium scrap according to the present invention, high-purity indium oxide can be obtained by pulverizing low-grade indium scrap to a predetermined size to produce colloidal particles, and then the colloidal particles are crystallized and oxidized in the air.
In addition, the method for producing high purity indium oxide from the indium scrap according to the present invention can recycle the indium scrap in a simple and environmentally friendly and economical manner without generating waste acid.
It will be appreciated that embodiments of the technical idea of the present invention can provide various effects not specifically mentioned.
1 is a flowchart illustrating a method for producing high purity indium oxide from indium scrap according to the first embodiment of the present invention.
2 is a flowchart illustrating a method for producing high purity indium oxide from indium scrap according to a second embodiment of the present invention.
3 is a flowchart illustrating a method for producing high purity indium oxide from indium scrap according to a third embodiment of the present invention.
4 is a graph showing the results of X-ray diffraction analysis of indium oxide prepared according to the present invention.
FIG. 5 is a photograph showing a transmission electron microscope image of indium oxide prepared according to the present invention. FIG.
Advantages and features of the present invention, and methods of accomplishing the same, will be apparent from and elucidated with reference to the embodiments described hereinafter in detail. However, the present invention is not limited to the embodiments described herein but may be embodied in other forms. Rather, the embodiments disclosed herein are provided so that the disclosure can be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The terminology used in this application is used only to describe a specific embodiment and is not intended to limit the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise.
Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the meaning in the context of the relevant art and are to be construed as ideal or overly formal in meaning unless explicitly defined in the present application Do not.
Hereinafter, a method for producing high purity indium oxide from indium scrap according to the present invention will be described in detail with reference to the drawings.
1 is a flowchart illustrating a method for producing high purity indium oxide from indium scrap according to the first embodiment of the present invention.
Referring to FIG. 1, a method for producing high purity indium oxide from indium scrap according to the present invention comprises: pulverizing a low-grade indium scrap into a predetermined size to produce colloidal particles, then crystallizing the colloidal particles and oxidizing them in the air, Can be obtained.
The indium scrap, which is used in the present invention, can be produced by a process for preparing an ITO target, a vacuum deposition process, a process for producing a high-purity indium oxide It is a concept that includes the scrap made up of abrasive sludge, waste ITO target, flake, sanding powder, and washing waste generated in the industrial field.
The method for producing high purity indium oxide from indium scrap according to the first embodiment of the present invention comprises the steps of crushing indium scrap (S100), dissolving indium scrap and removing residue (S110), introducing precipitant and metal hydroxide precipitate (S120) An organic acid addition and crystallization step (S130), and an indium oxide production step (S140).
In the first embodiment of the present invention, indium scrap produced in the ITO target manufacturing process or the vacuum deposition process with the indium scrap can be used to produce indium oxide of high purity.
1. Crushing the indium scrap (S100)
The step (S100) of crushing the indium scrap is a step of crushing the indium scrap produced in the ITO target manufacturing process or the vacuum deposition process into a predetermined size and pulverizing the scrap.
In step S100, the indium scrap may be crushed using a crusher or the like, and the indium scrap may be crushed to a size of 180 to 220 mesh. The indium scrap may be crushed by 200 mesh it is preferable to be pulverized to a size of a mesh.
2. Indium scrap melting and residue removal step (S110)
The step of dissolving indium scrap and removing residues (S110) is a step of completely dissolving the indium scrap and removing residues of insoluble matter by introducing inorganic acid into the pulverized and pulverized indium scrap.
The inorganic acid may be used in an amount of 300 to 900 parts by weight based on 100 parts by weight of the indium scrap powder in the step of dissolving and removing the indium scrap (S110). The inorganic acid may include at least one hydrogen ion (H +), (SO 4 2-), or nitrate (NO3 -) may be selected from the acid having, for example, the inorganic acid is hydrochloric acid (HCl), nitric acid (HNO 3), sulfuric acid (H 2 SO 4), and aqua regia is any one selected from the group consisting of: (a HCl and HNO 3 3 mixed in a weight ratio of 1) can be used.
3. Step of injecting precipitant and precipitating metal hydroxide (S120)
In the step of depositing the precipitant and depositing the metal hydroxide (S120), precipitating agent is added to the acid solution from which the insoluble residue is removed in the step of dissolving indium scrap and removing the residue (S110) to precipitate the metal hydroxide in the range of pH 3 to 9 to be.
In the step of injecting the precipitant and precipitating metal hydroxide (S120), the precipitant is used to precipitate metal ions in the acid solution as a metal hydroxide. As the precipitator, any one selected from ammonia, urea, sodium hydroxide, Can be used.
4. Addition of organic acid and crystallization step (S130)
The organic acid addition and crystallization step (S130) is a step of introducing the precipitant and introducing an organic acid into the metal hydroxide prepared in the metal hydroxide precipitation step (S120) to crystallize the metal oxalate.
In the organic acid addition and crystallization step (S120), organic acid may be used in an organic acid of 0.5 to 3.0 M (molar concentration). The organic acid may be used to crystallize the metal hydroxide into a metal oxalate by performing a substitution reaction with the metal hydroxide .
In the present invention, the organic acid may be any one selected from citric acid and oxalic acid.
When the precipitant is added in the step of depositing precipitant and metal hydroxide precipitation step (S120), a metal hydroxide is generated. Generally, metal hydroxide is in a colloidal state, and the particle size is several nm. When the filtrate is applied by vacuum or compression method, the filtration rate is slow Impurities (or other metal ions) are not removed, and the purity of the indium oxide is lowered.
However, in the present invention, the metal hydroxide is crystallized into a metal oxalate using an organic acid to increase the particle size, thereby increasing the filtration rate, and the impurity can be removed by generating an organic acid and a metal-complex compound, thereby increasing the purity of the indium oxide.
5. Indium oxide production step (S140)
The step (S140) of preparing the indium oxide is a step of preparing indium oxide of high purity by oxidizing the metal oxalate crystallized by the substitution reaction in the organic acid addition and crystallization step (S130).
The metal oxalate crystallized by the substitution reaction may be oxidized by reacting with air by allowing the metal oxalate crystallized by the substitution reaction to remain in the air. In the present invention, the metal oxalate crystallized as described above is dissolved in air By natural oxidation, a high purity indium oxide can be produced by a simple process.
2 is a flowchart illustrating a method for producing high purity indium oxide from indium scrap according to a second embodiment of the present invention.
Referring to FIG. 2, a high purity indium oxide can be obtained from indium scrap according to the present invention by precipitating metal hydroxide by using washing waste, crystallizing it and oxidizing it in the air.
The method for producing high purity indium oxide from indium scrap according to the second embodiment of the present invention includes a step of introducing a precipitant and a metal hydroxide precipitation step (S200), an organic acid addition and crystallization step (S210), and an indium oxide production step (S220).
In the second embodiment of the present invention, indium scrap produced from the washing waste by using the indium scrap can be used to produce indium oxide of high purity.
1. Step of injecting precipitant and precipitating metal hydroxide (S200)
The step of introducing the precipitant and precipitating metal hydroxide (S200) is a step of precipitating a metal hydroxide in a pH range of 3 to 9 by adding a precipitant to washing waste.
In the step S200 of depositing the precipitant and depositing the metal hydroxide, the precipitant is used to precipitate metal ions in the acid solution as a metal hydroxide. As the precipitator, any one selected from ammonia, urea, sodium hydroxide, and potassium hydroxide Can be used.
2. Addition of organic acid and crystallization (S210)
The organic acid addition and crystallization step (S210) is a step of introducing the precipitant and introducing an organic acid into the metal hydroxide produced in the metal hydroxide precipitation step (S200) to crystallize the metal oxalate.
In the organic acid addition and crystallization step (S210), organic acid may be used in an organic acid of 0.5 to 3.0 M (molar concentration), and the organic acid may be used to crystallize the metal hydroxide into a metal oxalate by performing a substitution reaction with the metal hydroxide .
In the present invention, the organic acid may be any one selected from citric acid and oxalic acid.
When a precipitant is added in the step of injecting precipitant and precipitating metal hydroxide (S200), a metal hydroxide is generated. Generally, metal hydroxide is in a colloidal state. Therefore, the particle size is several nm. When the filtrate is applied by vacuum or compression method, Impurities (or other metal ions) are not removed, and the purity of the indium oxide is lowered.
However, in the present invention, the metal hydroxide is crystallized into a metal oxalate using an organic acid to increase the particle size, thereby increasing the filtration rate, and the impurity can be removed by generating an organic acid and a metal-complex compound, thereby increasing the purity of the indium oxide.
3. In the indium oxide production step (S220)
The step of preparing indium oxide (S220) is a step of preparing high-purity indium oxide by oxidizing the metal oxalate crystallized by the substitution reaction in the organic acid addition and crystallization step (S210).
The metal oxalate crystallized by the substitution reaction may be oxidized by reacting with air by allowing the metal oxalate crystallized by the substitution reaction to remain in the air. In the present invention, By natural oxidation, a high purity indium oxide can be produced by a simple process.
3 is a flowchart illustrating a method for producing high purity indium oxide from indium scrap according to a third embodiment of the present invention.
Referring to FIG. 3, a high purity indium oxide can be obtained from indium scrap according to the present invention by crystallizing a waste ITO powder and oxidizing it in the air.
The method for producing high purity indium oxide from indium scrap according to the third embodiment of the present invention includes an organic acid addition and crystallization step (S300), and an indium oxide production step (S310).
In the third embodiment of the present invention, a high-purity indium oxide can be produced by using the pulverized ITO powder as the indium scrap.
1. Introduction of organic acid and crystallization step (S300)
In the organic acid addition and crystallization step (S300), an organic acid is added to the waste ITO pulverized powder to crystallize the metal oxalate.
In the organic acid addition and crystallization step (S300), an organic acid of 0.5 to 3.0 M (molar concentration) may be used. The organic acid may be used to crystallize the metal hydroxide into a metal oxalate by performing a substitution reaction with the metal hydroxide .
In the present invention, the organic acid may be any one selected from citric acid and oxalic acid.
2. In the indium oxide production step (S310)
The indium oxide production step (S310) is a step of preparing indium oxide of high purity by oxidizing the metal oxalate crystallized by the substitution reaction in the organic acid addition and crystallization step (S300).
The metal oxalate crystallized by the substitution reaction may be oxidized by reacting with air by allowing the metal oxalate crystallized by the substitution reaction in the air to be oxidized. In the present invention, the metal oxalate crystallized as described above is dissolved in air By natural oxidation, a high purity indium oxide can be produced by a simple process.
Hereinafter, preferred embodiments of a method for producing high purity indium oxide from indium scrap according to the present invention will be described in more detail with reference to the accompanying drawings.
≪ Example 1 >
As in the manufacturing method according to the first embodiment, the indium scrap produced in the ITO target manufacturing process or the vacuum deposition process is milled to a size of 200 mesh, and inorganic acid is added thereto to completely dissolve the scratched indium scrap, The residue was removed. At this time, the inorganic acid was used in an amount of 500 parts by weight based on 100 parts by weight of the indium scrap powder.
Next, a precipitant was added to the acid solution from which the insoluble residue was removed to precipitate a metal hydroxide having a pH in the range of 3 to 9, and an organic acid was added to the metal hydroxide to crystallize the metal oxalate.
The high-purity indium oxide according to the first embodiment of the present invention was prepared by oxidizing the crystallized metal oxalate in air.
≪ Example 2 >
As in the case of the manufacturing method according to the second embodiment, metal hydroxide is precipitated using washing waste, and then crystallized and oxidized in the air to obtain a high-purity indium oxide according to the second embodiment of the present invention. .
≪ Example 3 >
As in the manufacturing method according to the third embodiment, high purity indium oxide according to the third embodiment of the present invention was produced by crystallizing using a pulverized ITO powder and oxidizing it in the air.
The purity of indium was analyzed using indium oxide prepared as in Examples 1, 2 and 3 above.
In Table 1, [Table 1] is a purity analysis table of the indium oxide prepared in Example 1, [Table 2] is an indium oxide purity analysis table prepared in Example 2, and [Table 3] FIG. 4 is a graph showing the results of X-ray diffraction analysis of indium oxide prepared according to the present invention, and FIG. 5 is a graph showing the purity of indium oxide prepared by the transmission electron microscope It is a photograph showing the image.
Referring to Tables 1 to 3 and FIGS. 4 and 5, the method for producing high purity indium oxide using the indium scrap according to the present invention is characterized in that the indium scrap powder, the washing waste, or the waste ITO Indium oxide can be produced by using pulverized powder. As shown in the table, it can be seen that a high purity indium oxide having a purity of 99.99% or more is produced.
While the present invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, It will be possible. It is therefore to be understood that one embodiment described above is illustrative in all aspects and not restrictive.
Claims (8)
(S110) dissolving the indium scrap and removing residues of the insoluble fractions by injecting an inorganic acid into the pulverized and pulverized indium scrap;
A precipitant input and metal hydroxide precipitation step (S120) for precipitating a metal hydroxide in a pH range of 3 to 9 by adding a precipitant to the acid solution from which the insoluble residue is removed;
An organic acid addition and crystallization step (S130) of adding an organic acid to the metal hydroxide to crystallize the metal oxalate; And
And a step (S140) of producing an indium oxide by oxidizing the crystallized metal oxalate in the air to produce indium oxide.
Wherein the indium scrap is milled to a size of 180 to 220 mesh in the step (S100) of crushing the indium scrap.
The indium scrap melting and the inorganic acid in the residue removing step (S110) is to 100 parts by weight of indium scrap powder by 300 to 900 parts by weight is used, the mineral acid is hydrochloric acid (HCl), nitric acid (HNO 3), sulfuric acid (H 2 SO 4 ) and a mixture of a mixture of HCl and HNO 3 in a weight ratio of 3: 1.
Wherein the precipitant is selected from the group consisting of ammonia, urea, sodium hydroxide, and potassium hydroxide in the step of introducing the precipitant and metal hydroxide precipitation (S120).
Wherein the organic acid is used in an amount of 0.5 to 3.0 M in the organic acid addition and crystallization step (S120), and the organic acid is selected from the group consisting of citric acid and oxalic acid.
An organic acid addition and crystallization step (S210) of introducing an organic acid into the metal hydroxide to crystallize the metal oxalate; And
And an indium oxide production step (S220) of oxidizing the crystallized metal oxalate to produce a high-purity indium oxide,
As the precipitating agent, any one selected from ammonia, urea, sodium hydroxide or potassium hydroxide is used,
Wherein the organic acid is used in an amount of 0.5 to 3.0 M, and the organic acid is selected from the group consisting of citric acid and oxalic acid.
And an indium oxide production step (S310) of oxidizing the crystallized metal oxalate in air to produce indium oxide of high purity,
Wherein the organic acid is used in an amount of 0.5 to 3.0 M, and the organic acid is selected from the group consisting of citric acid and oxalic acid.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11479475B2 (en) * | 2020-03-06 | 2022-10-25 | Zhengzhou University | Method of preparing indium oxide spherical powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100932706B1 (en) | 2009-08-31 | 2009-12-21 | (주)티에스엠 | Method for recycling indium from indium containing waste solution |
| KR100940621B1 (en) | 2006-09-28 | 2010-02-05 | 도와 메탈스 앤드 마이닝 가부시끼가이샤 | Method for withdrawing indium from indium-containing material |
| KR20150078431A (en) | 2013-12-30 | 2015-07-08 | 경북대학교 산학협력단 | Method for recycling indium from ITO scrap |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100940621B1 (en) | 2006-09-28 | 2010-02-05 | 도와 메탈스 앤드 마이닝 가부시끼가이샤 | Method for withdrawing indium from indium-containing material |
| KR100932706B1 (en) | 2009-08-31 | 2009-12-21 | (주)티에스엠 | Method for recycling indium from indium containing waste solution |
| KR20150078431A (en) | 2013-12-30 | 2015-07-08 | 경북대학교 산학협력단 | Method for recycling indium from ITO scrap |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11479475B2 (en) * | 2020-03-06 | 2022-10-25 | Zhengzhou University | Method of preparing indium oxide spherical powder |
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| E902 | Notification of reason for refusal | ||
| E601 | Decision to refuse application |