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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, which is applied in the field of environmental engineering, can solve problems such as factory troubles, high copper ion concentration, affecting 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: 2011-05-04
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
  • 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] Example 1: Small test

[0051] The acid chlorine type copper etching solution wastewater is provided by Guangdong Meixian Qiaoyun Wastewater Treatment Plant. The appearance is dark blue and thick, with a brown-black oil layer floating on it. After analysis, the copper content is 100.1g / L, the chloride ion content is 1033.3g / L, and the acidity is 1.5mol / L HCl. Take a certain amount of wastewater after flotation and degreasing for the following test. The concentration of the formulated lix984 extractant is 25%. Take 25ml of oil-removed waste liquid, adjust the pH to 2.5 with NaOH, absorb the filtered waste liquid, put it into a 500ml separatory funnel, add the above-mentioned extracting agent, and perform extraction. The ratio is O:W=4:1. Shake for 5 minutes, stand for 7 minutes, and separate the phases. The raffinate is added with the new extractant for the second extraction, the method is the same as the first extraction. The chloride ion content of the loaded organic ...

Embodiment 2

[0052] Example 2: Pilot test

[0053] The source of waste liquid is the same as the small test. The test device is a bacterial leaching-extraction-electrowinning pilot test laboratory of the Key Laboratory of Biometallurgy of the Ministry of Education. It performs the second-stage countercurrent extraction of wastewater that has been degreasing by flotation and adjusted to pH 2.5 with lime water. The agglomerated baffle plates are made of two polypropylene porous plates with a spacing of 5 cm. The two baffles are filled with glass fiber and resin. The wastewater 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 with a pH of 2.5, and the ratio is 1:1. Then use 180g / L H 2 SO 4 The reverse extraction,...

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 wastewater flows into the pH adjustment tank, the lime water is adjusted to pH 2.0-2.5, and the flow rate is 3m 3 / h of wastewater is subjected to flotation, adsorption, filtration and degreasing, and then a secondary countercurrent extraction operation; the flow rate of lix984 extractant (concentration is still 25%) is 12m 3 / h, mixing time is 5min, stirring speed is 150rpm, clarification time is 7min. The 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 ratio and flow ratio are both 1:1. Then use 180g / LH 2 SO 4 Reverse extraction, the comparison ratio is 2.5:1, the copper sulfate solution obtained after the reverse extraction is fi...

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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 etchingsolution. 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 acid chloride copper etching solution waste water and preparing high-purity cathode copper. The method can be applied to printed circuit boards (PCBs) using acid chlorine copper etching solution ) Enterprises or related wastewater professional treatment enterprises. Background technique [0002] The etching process of corroding the non-patterned part of copper with copper etching solution is one of the basic processes of printed circuit board (PCB) companies. Common types of copper etching solutions are ammonia (alkaline) chlorine etching solution and acid chlorine type copper etching solution. If the etching waste liquid cannot be recycled well, it will lead to a large loss of copper resources and serious environmental pollution. Traditional methods include using waste liquid to directly recover CuS, copper chloride, copper ox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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