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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 - waste water, environmental protection pressure is high, and it is not an ideal method for copper recovery

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

Embodiment 2

[0032] Take 3m of etching solution containing Cu 142.3g / L with a pH of 8.8 3 , first deamination by evaporating under normal pressure at 105°C, the pH value of the solution dropped to 7.3 to stop evaporation, acidified to pH = 6.5 by adding phosphoric acid, and then frozen at -17°C for 8 hours, filtered to obtain 1696.5kg cupric ammonium chloride crystals and containing Cu 13.1 g / L crystallized liquid, the ammonia gas produced by evaporation is cooled and absorbed at 5°C to obtain ammonia water. After the obtained crystallization, the liquid was filled with ammonia until the pH value rose to 9.7, and returned to the etching process to continue to use; after the obtained cupric ammonium chloride crystal was stirred and dissolved with water, the copper was extracted with the P204-kerosene system as the organic phase, and the organic phase was loaded with 2mol / L H 2 SO 4 For the stripping solution of copper. The copper sulfate solution obtained by stripping is subjected to a ce...

Embodiment 3

[0034] Take 1m of etching solution containing Cu 126.8g / L with pH 8.3 3 , first undergo forced deamination by vacuum evaporation at 85°C to reduce the pH value of the solution to 6.8, then freeze at -12°C for 18 hours, and filter to obtain 448.6kg copper ammonium chloride double salt crystals and crystallized liquid containing Cu 24.5g / L . The resulting liquid after crystallization is added to the ammonia water obtained in Example 2 to adjust pH=9.5 and return to the etching process for continued use; after the obtained cupric chloride ammonium double salt crystals are dissolved in water, add 1 times the stoichiometric number of copper oxalate converted into copper oxalate in the solution 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, concentrated and crystallized to obtain ammonium...

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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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