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A method for reclaiming anhydrous indium salt and anhydrous tin salt from indium tin oxide

A technology of indium tin oxide and tin salt, applied in the field of alloy waste recycling, can solve the problems of consuming resin, large secondary waste, large energy, etc., and achieve the effects of energy saving, simple operation and high economy

Active Publication Date: 2019-01-22
顾帅
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unfortunately, all three methods have obvious disadvantages. The first method uses a large amount of organic solvent and water, and produces a large amount of secondary waste, and the final product of separation exists in the form of an aqueous solution of the ion, requiring Further use a large amount of alkali for precipitation to obtain the oxide or hydroxide of the metal, which is not economical
The second method is only suitable for the separation of extremely low concentration substances, generally less than 5ppm, and produces a large amount of secondary waste, consumes a large amount of resin, and is not economical
The third method, operating under high temperature and high vacuum conditions, consumes a lot of energy, and puts forward extremely high requirements on device materials, which is not economical

Method used

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  • A method for reclaiming anhydrous indium salt and anhydrous tin salt from indium tin oxide
  • A method for reclaiming anhydrous indium salt and anhydrous tin salt from indium tin oxide
  • A method for reclaiming anhydrous indium salt and anhydrous tin salt from indium tin oxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Firstly, the waste ITO material was pulverized into fine powder for composition analysis, the components of waste ITO were checked by XRF, and the mass fraction of each component in ITO was measured by standard FP quantitative procedure (SQX) analysis. Since SQX is only a semi-quantitative analysis method, after dissolving ITO powder with aqua regia, ICP-OES (Optima 5300DV) was used to determine the actual mass fractions of In and Sn in waste products. Table 1 summarizes the In of three different masses of ITO powder samples determined by ICP-OES 3+ , Sn 4+ and Zn 2+ The average mass fraction of ZnO as the main impurity, In 2 o 3 with SnO 2 The mass ratio is about 95:5.

[0041] Table 1 Chemical composition of spent ITO materials determined by SQX analysis of XRF and ICP-OES

[0042] Composition determined by XRF

In 2 o 3

SnO 2

ZnO

other

Quality score (%)

94.92

4.94

0.12

0.02

Components determined by ICP

...

Embodiment 2

[0070] Follow the steps below to recover anhydrous indium chloride, anhydrous indium nitrate and anhydrous tin chloride:

[0071] 1. Dissolving: the waste ITO material (In 2 o 3 and SnO 2 The mass ratio is 90:10) and crushed into fine powder, using aqua regia to completely dissolve the waste indium tin oxide powder, the ratio of ITO to solvent is 1g:8mL, the leaching temperature is 70°C, the stirring speed is 500rpm, and the time is 1.5h. Indium and tin then exist in aqua regia in the form of indium ions and tin ions, respectively.

[0072] 2. Distillation: The leaching solution is then distilled under reduced pressure, and the residue after distillation is a mixture of indium nitrate trihydrate, indium chloride tetrahydrate and tin chloride pentahydrate.

[0073] 3. Dehydration: Then grind the crystal mixture, add benzene to the crystal mixture, add 5mL of benzene per gram of crystal mixture, heat the flask, reflux the benzene for 3 hours, and fully remove the water in the...

Embodiment 3

[0077] Follow the steps below to recover anhydrous indium chloride and anhydrous tin chloride:

[0078] 1. Dissolving: the waste ITO material (In 2 o 3 and SnO 2 The mass ratio of 96:4) was crushed into fine powder, and the waste indium tin oxide powder was completely dissolved with hydrochloric acid. The ratio of ITO to solvent was 1g:40mL, the concentration of hydrochloric acid was 1M, the leaching temperature was 100°C, and the stirring speed was 500rpm. The time is 1 h, after which indium and tin exist in the hydrochloric acid solution in the form of indium ions and tin ions, respectively.

[0079] 2. Distillation: The leaching solution is then distilled under reduced pressure to recycle hydrochloric acid, and the residue after distillation is a mixture of indium chloride tetrahydrate and tin chloride pentahydrate.

[0080] 3. Dehydration: Then grind the crystal mixture, add n-butanol to the crystal mixture, add 6 mL of n-butanol per gram of crystal mixture, heat the fl...

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Abstract

The invention belongs to the technical field of alloy waste material recovery and utilization, and discloses a method for recovering anhydrous indium salt and anhydrous tin salt from indium tin oxide. The method comprises the following steps that S1, the indium tin oxide is dissolved by acid; indium and tin exist in the acid in an ion form; S2, the acid is removed through distillation; an indium salt hydrate and a tin salt hydrate are left; S3, a dehydrating agent is added into the hydrates in the S2; heating reflux is performed to obtain the anhydrous indium salt and the anhydrous tin salt; S4, the anhydrous indium salt and the anhydrous tin salt are separated. The method disclosed by the invention has the advantages that the product with extremely high purity can be obtained; all used reagents can be almost cyclically used; no pollution is generated on the environment; less energy and fewer reagents are consumed by the method; the method can be stably used for large-scale industrial practice; a large amount of energy can be saved; the operation is simple and convenient; the extremely high economic performance is realized.

Description

technical field [0001] The invention belongs to the technical field of alloy waste recycling and utilization, and in particular relates to a method for recycling anhydrous indium salt and anhydrous tin salt from indium tin oxide. Background technique [0002] Indium tin oxide (ITO) is an indium oxide (In 2 o 3 ) and tin oxide (SnO 2 ) mixture, due to its good electrical conductivity and optical transparency, is widely used in liquid crystal displays, flat panel displays, plasma displays, touch screens, electronic paper, organic light-emitting diodes and solar cells and other fields. Especially in the production process of various displays, because the process is sputtering, 85% of ITO becomes waste, and only 15% can be effectively utilized. At present, 65% of the global indium production is used to produce ITO, so it can be seen that it is imperative to recover scattered metal indium from waste ITO. At present, there are three mainstream recovery methods. One is liquid-l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G15/00C01G19/00C01G19/04
CPCC01G15/00C01G19/00C01G19/04C01P2002/72C01P2006/80
Inventor 慕平
Owner 顾帅
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