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Preparation method for electronic grade high-purity copper sulfate pentahydrate

A technology of copper sulfate pentahydrate, electronic grade, applied in copper sulfate and other directions, can solve the problems of complex process, high price, reducing the activity of plating solution, etc., and achieve the effect of high copper ion concentration, low production cost and high product purity

Inactive Publication Date: 2013-04-24
GUANGDONG GUANGHUA SCI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, when electronic components such as printed circuit boards are electroless plated, the plating solution is very sensitive to impurities; organic and non-metallic impurities will reduce the activity of the plating solution, resulting in reduced electroless plating speed and missing plating, and even lead to electroless plating in severe cases. The process is completely stopped; and various metal impurities will also cause the phenomenon of chemical plating speed reduction and missing plating, and will cause the coating to become dark, and the deposition of metal impurities on the coating will also cause the coating to be unstable and make the coating rough ; Therefore, the purity and cleanliness of copper sulfate have a very important impact on the yield, electrical performance and reliability of IC products
[0003] At present, the high-purity copper sulfate suitable for chemical plating of IC products is mainly imported, and the price is expensive.
The main factor that restricts the localization of high-purity copper sulfate is that the content of impurities such as iron, nickel, lead, and zinc in the raw materials is too high, while the traditional purification method is to remove impurities by hydrolysis precipitation by adjusting the pH value of the solution, and the iron ion hydrolysis precipitation The pH value is lower than that of copper ions, but copper ions will also partially precipitate while removing iron ions, while the pH values ​​of zinc, nickel and lead hydrolysis are all greater than copper, so it is difficult to remove; if conventional extraction methods are used to remove impurities, the reverse The concentration of copper ions in the extract is not high enough, and a subsequent concentration process is required to prepare ideal copper sulfate crystals, so there are problems of complex process and high energy consumption

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Dissolve 500.0 g of industrial-grade copper sulfate pentahydrate to prepare a solution with a copper ion concentration of 35 g / l. At this time, the concentration of each metal impurity in the solution is 0.015 g / l of iron, 0.014 g / l of nickel, and 0.014 g / l of zinc. 0.006g / l, lead 0.0022g / l, use an appropriate amount of sulfuric acid to adjust the pH value of the solution to 1.5, add an appropriate amount of activated carbon to filter;

[0021] (2) Extract copper from the filtrate obtained in step (1) with extractant M5640, the concentration of extractant M5640 in kerosene is 40%, compared to O / A is 2 / 1, the equilibrium pH value is 1.5, and the extraction time is 2min , the number of extraction stages is 4, which separates copper from metal impurities such as iron, nickel, zinc, and lead;

[0022] (3) The extraction agent M5640 in step (2) is loaded with copper organic phase at 55°C for stripping with a stripping agent. The stripping agent is a mixture of sulfuric a...

Embodiment 2

[0025] (1) Dissolve 500.0 g of industrial-grade copper sulfate pentahydrate to prepare a solution with a copper ion concentration of 45 g / l. At this time, the concentration of each metal impurity in the solution is 0.016 g / l of iron, 0.0145 g / l of nickel, and 0.0145 g / l of zinc. 0.0063g / l, lead 0.0025g / l, use an appropriate amount of sulfuric acid to adjust the pH value of the solution to 2.0, add an appropriate amount of activated carbon to filter;

[0026] (2) Extract copper from the filtrate obtained in step (1) with extractant M5640, the concentration of extractant M5640 in kerosene is 45%, compared to O / A is 2 / 1, the equilibrium pH value is 2.0, and the extraction time is 2min , the number of extraction stages is 5, which separates copper from iron, nickel, zinc, lead and other metal impurities;

[0027] (3) Extract the copper-loaded organic phase of extractant M5640 in step (2) at 55°C with a stripping agent for stripping. The stripping agent is a mixture of sulfuric aci...

Embodiment 3

[0030] (1) Dissolve 500.0 g of industrial-grade copper sulfate pentahydrate to prepare a solution with a copper ion concentration of 55 g / l. At this time, the concentration of each metal impurity in the solution is 0.017 g / l of iron, 0.015 g / l of nickel, and 0.0068 g / l of zinc g / l, lead 0.0027g / l, use an appropriate amount of sulfuric acid to adjust the pH value of the solution to 2.5, add an appropriate amount of activated carbon to filter;

[0031] (2) Extract copper from the filtrate obtained in step (1) with extractant M5640, the concentration of extractant M5640 in kerosene is 50%, the ratio O / A is 2 / 1, the equilibrium pH value is 2.5, and the extraction time is 2min , the number of extraction stages is 5, which separates copper from nickel, zinc, iron and other impurities;

[0032] (3) Extract the copper-loaded organic phase of extractant M5640 in step (2) at 55°C with a stripping agent for stripping. The stripping agent is a mixture of sulfuric acid and the mother liquo...

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Abstract

The invention provides a method for preparing electronic grade high-purity copper sulfate pentahydrate through purifying with industrial grade copper sulfate pentahydrate as a raw material. According to the method, after the industrial grade copper sulfate pentahydrate is prepared to the solution with a certain concentration and a certain pH value, the copper extraction is implemented for the solution by adopting extractant M5640; then back extraction is executed by adopting back extractant at a higher temperature; and the direct cooling crystallization, the centrifugation and the drying are implemented to obtain the product. The preparation method adopts the extractant M5640 to extract the copper, so that impurities, such as iron, nickel, lead, zinc and the like in industrial copper sulfate raw materials can be removed more efficiently, and the back extraction temperature is heated up; copper ions in the obtained copper sulfate solution have high concentration; the direct cooling crystallization can be implemented after the oil removing purification, so that the concentration crystallization technique in the conventional extraction method can be avoided; compared with the traditional technique for removing impurities and purifying copper sulfate through hydrolytic precipitation method and the conventional extraction method, the preparation method has the characteristics of simple technique, high product purity, low energy consumption and low production cost; and the prepared copper sulfate pentahydrate is suitable for IC (Integrated Circuit) products.

Description

technical field [0001] The present invention relates to a method for preparing copper salt, in particular to a method for preparing high-purity copper salt suitable for use in the electronics industry, and more particularly to a method for preparing electronic grade high Method for pure copper sulfate pentahydrate. Background technique [0002] Copper sulfate generally exists in the form of five crystal waters. Copper sulfate pentahydrate is also known as bile alum, blue alum, and copper alum. In traditional industrial fields, copper sulfate is mainly used as a mordant, insecticide, Water fungicides, wood preservatives, and also widely used in the preparation of Bordeaux mixture, copper electroplating solution, non-ferrous metal beneficiation (flotation) industry, ship paint industry and the manufacture of other chemical raw materials. With the rapid development of high-tech electronic components, integrated circuits, printed circuit boards and related enterprises in Chin...

Claims

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Application Information

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IPC IPC(8): C01G3/10
Inventor 谭泽李明黄司平
Owner GUANGDONG GUANGHUA SCI TECH
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