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Method of preparing high pure cathode copper by using PCB acid chlorine copper etching solution sewage

A high-purity cathode copper and copper etching technology, applied in the field of environmental engineering, can solve problems such as factory troubles, high copper ion concentration, influence extraction and impurity entrainment, etc., to reduce investment costs and operating costs, reduce investment and operating costs, Reduces the effect of extraction entrained impurities

Inactive Publication Date: 2009-10-07
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This leads to the storage and operation of highly toxic and dangerous chlorine gas, causing great trouble to the factory;
[0008] (3) There is inevitably a certain amount of ferric ions in the acidic etching solution, which leads to a decrease in the electrical efficiency during electrowinning;
[0009] (4) Although insoluble anodes are used, the chloride ion corrosion is serious and the plates are easy to burn; the electrode plates have a large investment and high cost;
[0010] (5) The composition of the etching solution is complex, the cathode copper quality is poor, and the operation stability is poor
[0014] (2) Wastewater from various processes in PCB manufacturing is inevitably mixed with each other. The actual source of etching waste liquid is complicated, and contains a small amount of organic components such as ink, which affects extraction and impurity entrainment;
[0015] (3) Due to the high concentration of copper ions in the etching waste liquid, the recovery rate of copper extraction is only about 80%;
[0016] (4) The quality of the prepared cathode copper is generally between 97% and 99%, which does not meet the national standard for cathode copper

Method used

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  • Method of preparing high pure cathode copper by using PCB acid chlorine copper etching solution sewage
  • Method of preparing high pure cathode copper by using PCB acid chlorine copper etching solution sewage

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1: small test test

[0051] The acid chlorine-type copper etching solution wastewater is provided by Guangdong Meixian Qiaoyun Wastewater Treatment Plant. It is dark blue in appearance and thick, with a brown and black oil slick on it. After analysis, the copper content was 100.1g / L, the chloride ion content was 1033.3g / L, and the acidity was 1.5mol / L HCl. Take a certain amount of waste water for the following test after degreasing by flotation. The concentration of the prepared lix984 extractant is 25%. Get 25ml of oil-removing waste liquid, adjust the pH value to 2.5 with NaOH, absorb and filter the waste liquid, put it into a 500ml separating funnel, add the above-mentioned extractant, and extract, compared to O:W=4:1, manual Shake for 5 minutes, let stand for 7 minutes, and separate the phases. The raffinate is added with the above-mentioned new extractant to carry out the second extraction, and the method is the same as the first extraction. The chlo...

Embodiment 2

[0052] Embodiment 2: pilot test

[0053] The source of waste liquid is the same as that of the small test. The test device is the bacterial leaching-extraction-electrowinning pilot laboratory of the key laboratory of the Ministry of Education of Biometallurgy. The second-stage countercurrent extraction is performed on the waste water that has been degreased by flotation and adjusted to a pH value of 2.5 with lime water. Condensation and baffles are two polypropylene perforated plates with a distance of 5 cm, and glass fiber and resin are filled between the two baffles. The waste water flow rate is 1L / h; the flow rate of lix984 extractant (concentration is still 25%) is 4L / h, the mixing time is 5min, the stirring speed is 150rpm, and the clarification time is 7min. By measuring and analyzing the copper content of the raffinate, the extraction recovery rate was calculated to be 95.7%. Wash twice with sulfuric acid at pH 2.5 in a ratio of 1:1. Then use 180g / L H 2 SO 4 Back-e...

Embodiment 3

[0055] The waste liquid comes from various acid etching liquid waste water collected by Guangdong Qiaoyun Wastewater Treatment Plant from various PCB factories. The waste water flows into the pH adjustment tank, and the lime water adjusts the pH to 2.0-2.5, with a flow rate of 3m 3 After the waste water of / h carries out flotation adsorption filtration to remove oil, carry out secondary countercurrent extraction operation; The flow rate of lix984 extraction agent (concentration is still 25%) is 12m 3 / h, the mixing time is 5min, the stirring speed is 150rpm, and the clarification time is 7min. The phase ratio is 1:1, and the two-phase flow ratio is 4:1. By measuring and analyzing the copper content of the raffinate, the extraction recovery rate was calculated to be 95.6%. Wash twice with sulfuric acid with a pH value of 2.0, and the phase and flow ratios are both 1:1. Then use 180g / LH 2 SO 4 Back-extraction, the ratio is 2.5:1, the copper sulfate solution obtained after b...

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Abstract

The present invention disclose a method of preparing high pure cathode copper by using PCB acid chlorine copper etching solution sewage, the main technical characteristics include applying sewage preprocess procedure to satisfy extraction need better, programming multi-extraction to improve extraction recovery rate of cooper, applying extractant with high selectivity avoid extraction entrainment design, washing procedure etc. to reduce carried impurity and dispel affect of chloride ion to electrodeposition. The electrodeposition applies additive to improve copper crystallinity, simultaneity, utilize residual useful ingredient in raffinate to prepare copper etching solution, arriving the objective of both prepare high pure cathode copper effectively and regenerative cycle use of the etching solution. The purity of the prepared cathode copper reaches 99.99%.

Description

technical field [0001] The invention belongs to the technical field of environmental engineering, and relates to a method for recovering copper from PCB acidic chlorine-type copper etching solution wastewater and preparing high-purity cathode copper. The method can be applied to printed circuit boards (PCBs) using acidic chlorine-type copper etching solution ) enterprises or related professional wastewater treatment enterprises. Background technique [0002] The etching process of etching away the copper in the non-graphic part with copper etching solution is one of the basic processes of printed circuit board (PCB) enterprises. Common types of copper etching solutions are ammoniacal (alkaline) chlorine-type etching solutions and acidic chlorine-type copper etching solutions. If the waste etching solution cannot be recycled well, it will lead to a large loss of copper resources and serious pollution of the environment. Traditional methods include using waste liquid to dire...

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B3/40C25C1/12
CPCY02P10/20
Inventor 余润兰陈涌达邱冠周覃文庆
Owner CENT SOUTH UNIV
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