Preparation method of metal indium

Abstract

The invention discloses a preparation method of metal indium. The preparation method comprises the following steps: S1, selecting an indium-containing material; s2, adding into a reaction barrel, slowly adding concentrated sulfuric acid, and stirring; s3, adding an oxidizing agent, continuously stirring, adding water for dilution, and cooling; s4, performing pressure filtration to obtain an indium solution; s5, putting into an extraction machine, and adding an extraction agent to extract indium; s6, adding a stripping agent, removing impurities, and pressurizing and filtering; s7, an AI plate is used for replacing sponge indium, and cake pressing and forming are conducted; s8, alkali is added for reduction; and S9, obtaining a finished product of crude indium. The acid amount of the concentrated sulfuric acid in the step S2 is 25% of the indium-containing material, and the stirring time is 4 hours. The oxidizing agent in the step S3 is a 1% hydrogen peroxide solution, and the stirring time is 2 hours. The pressure intensity in the step S4 is 0.15 MPa. The extraction agent in the step S5 is P2O4. The stripping agent in the step S6 is an HCl solution, and the PH value of the stripping agent is adjusted to be 2.5. The alkali in the S8 is NaOH.

Description

TECHNICAL FIELD

[0001] The application relates to the field of high-purity semiconductor metal materials, in particular to a preparation method of metallic indium. BACKGROUND

[0002] With the development of thin-film solar technology, high-purity indium is an important raw material, which can be used for manufacturing compound semiconductors and as a doping element of silicon and germanium; because of light transmittance, electrical conductivity and low melting point, the high-purity indium is widely used for manufacturing transparent conductive films for liquid crystal displays, and can also be used for transparent electrodes, electroluminescent elements and the like; and can also be used as an alloy contact material such as diode to improve the contact performance.

[0003] Although the indium resource is relatively abundant at present, in the medium and long term, if the related components are widely used and the recycling technology has no breakthrough, the indium supply and demand relationship and production cost may be affected, and the related preparation technology and recycling technology need to be continuously improved to ensure the stability of the supply and demand of indium. SUMMARY

[0004] The technical problem to be solved by the application is to provide a preparation method of metallic indium, which not only saves cost and improves production efficiency, but also has high purity of indium finished product.

[0005] In order to solve the above technical problems, the technical scheme of the application is as follows: a preparation method of metallic indium, comprising the following steps:

[0006] S1, selecting an indium-containing material;

[0007] S2, adding the reaction barrel, slowly adding concentrated sulfuric acid and stirring;

[0008] S3, adding an oxidizing agent, continuing to stir, then adding water for dilution and cooling;

[0009] S4, pressure filtration to obtain an indium solution;

[0010] S5, putting into an extraction machine and adding an extraction agent to extract indium;

[0011] S6, adding a stripping agent to remove impurities and perform pressure filtration;

[0012] S7, using an AI plate to replace the indium into sponge indium, and pressing the cake into a shape;

[0013] S8, adding alkali for reduction;

[0014] S9, rough indium finished product.

[0015] Preferably, the amount of concentrated sulfuric acid in S2 is 25% of the indium-containing material, and the stirring time is 4h.

[0016] Preferably, the oxidizing agent in S3 is 1% hydrogen peroxide solution, and the stirring time is 2h.

[0017] Preferably, the pressure in S4 is 0.15 MPa.

[0018] Preferably, the extractant in S5 is P2O4.

[0019] Preferably, the stripping agent HCl solution in S6 is adjusted to a pH of 2.5.

[0020] Preferably, the base in S8 is NaOH.

[0021] Compared with the prior art, the present application has the following beneficial effects:

[0022] 1. Cost savings;

[0023] 2. Improved production efficiency;

[0024] 3. Product purity of 99.90% or more. DETAILED DESCRIPTION

[0025] The specific embodiments of the present application will be further described below. It should be noted that the description of these embodiments is used to help understand the present application and does not constitute a limitation on the present application. In addition, the technical features involved in the various embodiments of the present application described below can be combined with each other as long as they do not conflict with each other.

[0026] A method for preparing metallic indium, comprising the following steps:

[0027] S1, selecting an indium-containing material;

[0028] S2, adding to a reaction bucket, slowly adding concentrated sulfuric acid and stirring;

[0029] S3, adding an oxidizing agent, continuing to stir, then adding water to dilute and cool;

[0030] S4, pressurized filtration to obtain an indium solution;

[0031] S5, placing in an extraction machine and adding an extractant to extract indium;

[0032] S6, adding a stripping agent to remove impurities and pressurized filtration;

[0033] S7, using an Al plate to replace the sponge indium and pressing the cake into a shape;

[0034] S8, adding a base for reduction;

[0035] S9, crude indium product.

[0036] Specifically, the amount of concentrated sulfuric acid in S2 is 25% of the indium-containing material, and the stirring time is 4h.

[0037] Specific, the oxidizing agent in S3 is 1% hydrogen peroxide solution, the stirring time is 2h.

[0038] Specific, the pressure in S4 is 0.15MPa.

[0039] Specific, the extractant in S5 is P2O4.

[0040] Further, the stripping agent in S6 is HCl solution, and the PH value is adjusted to 2.5.

[0041] Further, the base in S8 is NaOH.

[0042] The indium-containing material is added to the reaction bucket, and 25% concentrated sulfuric acid is slowly added and stirred for 4h,

[0043] The displacement overall reaction formula is:

[0044] In2O3+3H2SO4=In2(SO4)3+3H2O

[0045] (1) 2In+3H2SO4=In2(SO4)3+3H2↑

[0046] (2) In+H2SO4=In2(SO4)3+H2↑

[0047] After the reaction is completed, 1% hydrogen peroxide solution is added, and the mixture is stirred for 2h to perform oxidation reaction,

[0048] The chemical reaction formula is:

[0049] In2(SO4)3+6NaOH=2In(OH)3↓+3Na2SO4

[0050] Then dilute with water and cool; the indium-containing material after reaction is filtered under pressure to separate the residue and water, the obtained Pb residue is put into the warehouse to make Pb brick, and the aqueous solution is added with iron powder for reduction, and other metals such as bismuth and copper are precipitated,

[0051] The regeneration reaction formula is:

[0052] 2Fe(R2PO4)3+3H2C2O4=Fe2(C2O4)3+6HR2PO4

[0053] After obtaining the qualified indium solution, it is put into an extraction machine to extract indium; P2O4 extractant is used to extract indium, and the extraction reaction formula is:

[0054] 3In 3+ (aqueous)+3H2R2PO4(solid)=3In(R2PO4)3+6H +

[0055] 6N HCl is added for stripping,

[0056] The stripping reaction formula is:

[0057] In(R2PO4)3+3HCl=3HR2PO4+InCl3

[0058] After the stripping agent is adjusted to a pH value of 2.5 by NaHO, impurities are removed, pressure filtration is performed; then, AI plate is used for displacement to obtain sponge indium, the sponge indium is compressed into a cake, NaHO is added for smelting reduction to obtain crude indium;

[0059] The displacement reaction formula is:

[0060] (I) InCl3+Al=AlCl3+In↓

[0061] (II) 2InCl3+3Zn=3ZnCl2+2In↓

[0062] (III) Zn+2HCl=H2↑+ZnCl2

[0063] The purity can reach more than 99.90%.

[0064] The embodiments of the present application are described in detail above, but the present application is not limited to the described embodiments. For those skilled in the art, various changes, modifications, replacements and variations of the embodiments can be made without departing from the principles and spirits of the present application, and still fall within the protection scope of the present application.

Claims

1. A method for producing metallic indium, characterized by, The method comprises the following steps: S1, selecting indium-containing materials; S2, adding into a reaction barrel, slowly adding concentrated sulfuric acid and stirring; S3, adding an oxidizing agent, continuing to stir, then adding water for dilution and cooling; S4, pressure filtration to obtain an indium solution; S5, placing into an extraction machine and adding an extractant to extract indium; S6, adding a stripping agent to remove impurities and pressure filtration; S7, using an Al plate to replace the indium into sponge indium, and pressing the cake into a shape; S8, adding alkali for reduction; S9, obtaining crude indium.

2. The method of producing indium metal according to claim 1, characterized by, The amount of concentrated sulfuric acid in S2 is 25% of the indium-containing materials, and the stirring time is 4h.

3. The method of producing indium metal according to claim 1, characterized by, The oxidizing agent in S3 is 1% hydrogen peroxide solution, and the stirring time is 2h.

4. The method of producing indium metal according to claim 1, characterized by, The pressure in S4 is 0.15MPa.

5. The method of producing indium metal according to claim 1, wherein The extractant in S5 is P2O4.

6. The method of producing indium metal according to claim 1, wherein The stripping agent in S6 is HCl solution, and the PH value is adjusted to 2.

5.

7. The method of producing indium metal according to claim 1, wherein The alkali in S8 is NaOH.