Method for treating waste liquid from process of etching indium tin oxide

Patent metadata

Field	Value
Publication number	US-10202703-B2
Application number	US-201715685736-A
Country	US
Kind code	B2
Filing date	Aug 24, 2017
Priority date	Jan 5, 2017
Publication date	Feb 12, 2019
Grant date	Feb 12, 2019

Abstract

This disclosure provides a method for treating an etching waste liquid from an etching process of indium tin oxide comprising hydrochloric acid, acetic acid, tin ions, indium ions and water, comprising the steps of: distilling the etching waste liquid to obtain a distillate comprising hydrochloric acid and acetic acid and a post-distillation liquid comprising tin ions and indium ions; generating a precipitate by reacting tin ions in the post-distillation liquid with sulfide ions to remove tin ions from the solution so as to obtain a post-precipitation solution containing indium ions; and electrolyzing the post-precipitation solution to obtain crude indium.

First claim

What is claimed is:

1. A method for treating an etching waste liquid from an etching process of indium tin oxide comprising hydrochloric acid, acetic acid, tin ions, indium ions and water, comprising the steps of:
distilling the etching waste liquid to obtain a distillate comprising hydrochloric acid and acetic acid and a post-distillation liquid comprising tin ions and indium ions;
generating a precipitate by reacting tin ions in the post-distillation liquid with sulfide ions to remove tin ions from the solution so as to obtain a post-precipitation solution containing indium ions; and
electrolyzing the post-precipitation solution to obtain crude indium.

2. The method according to claim 1 , further comprising the step of performing electrolytic refining on the crude indium to obtain indium with a purity of 99 wt % or more.

3. The method according to claim 2 , wherein in the electrolytic refining, the crude indium is used as an anode, pure indium is used as a cathode, the electrolytic solution is an aqueous indium sulfate solution with a concentration of 40 to 100 g/L, the pH of the electrolytic solution is 1.5 to 2.5, the cell voltage is controlled at 0.15 to 0.3V, the current density is 60 to 80 A/m 2 , and the electrolysis temperature is controlled at 20 to 30° C.

4. The method according to claim 3 , wherein sodium chloride is added to the electrolytic solution.

5. The method according to claim 1 , wherein the distillation is performed under 0.9-1 atmospheric pressure and at 90-100° C.

6. The method according to claim 1 , wherein
the etching waste liquid comprises, in terms of weight, 5 to 30% of hydrochloric acid, 2 to 10% of acetic acid, 60 to 92% of water, 0.005 to 1% of tin ions, and 0.005 to 2.5% of indium ions;
the distillate comprises, in terms of weight, 30 to 40% of hydrochloric acid, 8 to 12% of acetic acid, and 38 to 62% of water; and
the post-distillation liquid comprises, in terms of weight, 0.01 to 2% of tin ions and 0.01 to 5% of indium ions.

7. The method according to claim 1 , wherein the etching waste liquid comprises, in terms of weight, 17 to 22% of hydrochloric acid, 4 to 6% of acetic acid, 73 to 79% of water, 0.005 to 1% of tin ions, and 0.005 to 2.5% of indium ions;
the distillate comprises, in terms of weight, 30 to 40% of hydrochloric acid, 8 to 12% of acetic acid, and 38 to 62% of water; and
the post-distillation liquid comprises, in terms of weight, 0.01 to 2% of tin ions and 0.01 to 5% of indium ions.

8. The method according to claim 1 , wherein the volume ratio of the distillate to the post-distillation liquid is 0.2 to 5.

9. The method according to claim 1 , wherein the precipitation is performed at a pH of 0 to 2; and when the pH of the post-distillation liquid is less than 0, distillation is continued, and when the pH of the post-distillation liquid is greater than 2, the pH of the post-distillation liquid is adjusted to less than or equal to 2 by using hydrochloric acid, acetic acid, sulfuric acid, and/or an etching waste liquid.

10. The method according to claim 1 , wherein a hydrogen sulfide gas is introduced to perform reaction of tin ions and sulfide ions in the post-distillation liquid for 0.5 minutes to 60 minutes.

11. The method according to claim 10 , wherein the ratio of the molar amount of hydrogen sulfide introduced to the molar amount of tin ions is 1.1 to 10.

12. The method according to claim 1 , wherein the electrolysis is performed by using a lead-silver electrode as an anode and a pure-indium electrode as a cathode, wherein the current density of the electrolysis is 60 to 80 A/m 2 and the cell voltage is controlled at 0.15 to 0.3V, to obtain crude indium with a purity of 90 to 98 wt %.

13. The method according to claim 1 , wherein the distillate comprising hydrochloric acid and acetic acid is used for preparing an etching liquid for indium tin oxide.

Assignees

• Boe Technology Group Co Ltd
• Hefei Xinsheng Optoelectronics Technology Co Ltd

Inventors

• Xie Yongxian
• Deng Chuanfeng
• Li Youlu
• He Zhiyang

Classifications

• C25F3/08 Primary

  of refractory metals · CPC title

• C02F1/048

  Purification of waste water by evaporation · CPC title

• C02F1/5236

  using inorganic agents · CPC title

• C02F2103/346

  from semiconductor processing, e.g. waste water from polishing of wafers · CPC title

• C02F1/4678

  of metals · CPC title