Alkaline CuC12 spent etching solution copper removal regeneration method

A waste etching solution and decopper technology, which is applied in the field of chemical metallurgy, can solve the problems of high environmental pressure, not a method of recycling copper, and large quantities, and achieve the effects of easy operation, avoiding secondary pollution, and environmental friendliness

Inactive Publication Date: 2015-10-28
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the chemical precipitation method is simple in process, it produces a large amount of Cl-containing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0029] Example 1

[0030] Take 1000ml of etching solution with a pH of 8.5 and 158.5g / L of Cu. Stir and add concentrated hydrochloric acid to acidify the solution to pH=0.5. A precipitate of copper ammonium chloride double salt is immediately formed. After cooling at 5°C for 5 hours, the precipitate increases significantly. 526.3 g of copper chloride crystals and a filtrate containing 39.5 g / L of Cu were obtained by filtration. The obtained filtrate is stirred with ammonia to adjust the pH to a solution of 9.8, and is returned to the etching process for use as a supplementary solution. The obtained copper ammonium chloride crystals are dried and dehydrated and then pyrolyzed at 380°C to obtain ammonium chloride and anhydrous copper chloride.

Example Embodiment

[0031] Example 2

[0032] Take 3m of etching solution with pH 8.8 and Cu 142.3g / L 3 Firstly, deammonia by evaporation at 105°C under normal pressure, the pH of the solution drops to 7.3 to stop evaporation, add phosphoric acid to acidify to pH=6.5, then freeze at -17°C for 8h, filter to obtain 1696.5kg copper ammonium chloride crystals and Cu 13.1 g / L of crystallization liquid, the ammonia gas produced by evaporation is cooled and absorbed at 5°C to obtain ammonia water. After the obtained crystallization, the liquid is filled with ammonia until the pH value rises to 9.7, and then returns to the etching process to continue using; the obtained copper ammonium chloride crystals are stirred and dissolved in water, and the copper is extracted with the P204-kerosene system as the organic phase. The organic phase is loaded with 2mol / L H 2 SO 4 As a copper stripping solution. The copper sulfate solution obtained by stripping has a cell voltage of 2.0V and a current density of 200A / m 2 T...

Example Embodiment

[0033] Example 3

[0034] Take 1m of etching solution with pH 8.3 and Cu 126.8g / L 3 , Firstly by 85 ℃ vacuum evaporation forced deamination, so that the pH value of the solution drops to 6.8, and then frozen at -12 ℃ for 18h, filtered to obtain 448.6kg copper ammonium chloride double salt crystals and Cu 24.5g / L crystallization liquid . Add the obtained crystallization solution to the ammonia solution obtained in Example 2 to adjust the pH=9.5 and return to the etching process for continued use; after the obtained copper chloride ammonium double salt crystals are dissolved in water, the copper in the solution is converted into copper oxalate at 1 times the stoichiometric amount. Ammonium oxalate, stirred at room temperature for 1.5 hours, filtered to obtain copper oxalate precipitate and precipitated liquid; the obtained copper oxalate was directly sold as a product, and the obtained precipitated liquid was evaporated and concentrated to crystallize to obtain ammonium chloride pr...

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PUM

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Abstract

The invention discloses an alkaline CuC12 spent etching solution copper removal regeneration method. Evaporation is conducted on a spent alkaline etching solution for deamination; acid is added or directly added for acidifying; cooling or freezing is conducted so that copper in the solution can be precipitated out with ammonium cupric chloride double salt crystals; filtering is conducted, and the ammonium cupric chloride double salt crystals and after-crystallization liquid of the ammonium cupric chloride double salt crystals are obtained; obtained ammonium cupric chloride double salt is separated, and copper is obtained; at least one of ammonia water, ammonia gas, hydrochloric acid and ammonium chloride is selected to be added to the after-crystallization liquid to be used as a regenerating agent so that the liquid can be regenerated and returned to the etching process to be continuously used. Thus, effective components in the spent alkaline etching solution are fully and effectively utilized; secondary pollution is avoided; operation is simple and convenient; environmental friendliness is achieved; the alkaline CuC12 spent etching solution copper removal regeneration method is suitable for industrial application of spent alkaline etching solution copper removal regeneration.

Description

technical field [0001] The invention belongs to the field of chemical metallurgy, and in particular relates to a method for decopper regeneration of an alkaline etching solution. Background technique [0002] Alkaline copper chloride etchant (CuCl 2 -NH 4 Cl-NH 3 ·H 2 O) Because of its fast etching speed, small side erosion, large copper-dissolving ability, and easy control of etching rate, it is widely used in the etching of electroplated and anti-corrosion printed boards. With the progress of etching, the copper content in the etching solution increases continuously, and the specific gravity gradually increases. When the concentration of copper in the etching solution reaches a certain height, it must be adjusted in time. In industrial production, the etching solution with too high discharge specific gravity is used, and new supplementary liquid is added to control the specific gravity of the etching solution within the allowable range. The discharged high specific gr...

Claims

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Application Information

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IPC IPC(8): C23F1/46C22B7/00
CPCY02P10/20
Inventor 王学文王明玉刘学辉
Owner CENT SOUTH UNIV
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