US 11,939,229 B2
Method for treating copper-containing waste etching solution
Zhang Lin, Changsha (CN); Xu Yan, Changsha (CN); Xueming Liu, Changsha (CN); Fandongkun Meng, Changsha (CN); and Yanjie Liang, Changsha (CN)
Assigned to Central South University, Changsha (CN)
Filed by Central South University, Changsha (CN)
Filed on Nov. 18, 2022, as Appl. No. 17/990,441.
Application 17/990,441 is a continuation of application No. PCT/CN2022/086882, filed on Apr. 14, 2022.
Claims priority of application No. 202111444073.6 (CN), filed on Nov. 30, 2021.
Prior Publication US 2023/0166979 A1, Jun. 1, 2023
Int. Cl. C01G 3/10 (2006.01); C02F 1/52 (2023.01); C02F 1/66 (2023.01); C02F 1/72 (2023.01); C02F 9/00 (2023.01); C02F 101/10 (2006.01)
CPC C01G 3/10 (2013.01) [C02F 9/00 (2013.01); C01P 2004/03 (2013.01); C02F 1/5236 (2013.01); C02F 1/66 (2013.01); C02F 1/722 (2013.01); C02F 2101/10 (2013.01)] 10 Claims
OG exemplary drawing
 
1. A method for treating a copper-containing waste etching solution, comprising steps:
S1, preparing an inducer containing basic copper chloride nanometer seed crystals: mixing and curing a copper chloride solution and an ammonia solution in a sequence to obtain the inducer containing the basic copper chloride nanometer seed crystals;
wherein a mixing temperature is 0-45° C., a mixing stirring speed is 750-1000 r/min, a concentration of copper ions in the copper chloride solution used in the mixing is 200-350 g/L, and an initial pH of the mixing is 1.0-3.0; a curing temperature is 35-60° C., and a curing duration is 8-48 h;
S2, preparing a slurry containing basic copper chloride mono-crystals: making the inducer react with the copper chloride solution and the ammonia solution to obtain the slurry containing the basic copper chloride mono-crystals;
wherein a concentration of copper ions in the copper chloride solution used in an induced reaction is 25-75 g/L, an induced reaction temperature is 45-75° C., an initial pH of the induced reaction is 2.5-3.5, and a stirring speed of the induced reaction is 20-120 r/min;
S3, classifying the copper-containing waste etching solution for treatment: collecting a to-be-treated copper-containing waste etching solution, and classifying the copper-containing waste etching solution into an acidic waste etching solution and an alkaline waste etching solution;
S4, making the acidic waste etching solution to be subjected to an agglomeration reaction with an ammonium-containing solution and the slurry containing the basic copper chloride mono-crystals to obtain basic copper chloride crystal particles and a copper-removed waste solution;
wherein an agglomeration reaction temperature is 80-100° C., an initial pH of the agglomeration reaction is 3.5-4.5, and a stirring speed of the agglomeration reaction is 150-300 r/min; and
S5, making the alkaline waste etching solution react with sulfuric acid to obtain a copper sulfate mixed solution; and then evaporating, concentrating, cooling and crystallizing the copper sulfate mixed solution obtained by the reaction of the alkaline waste etching solution and the sulfuric acid to obtain copper sulfate pentahydrate solids.