Method for continuously preparing high-purity low-chloride electroplating copper oxide

An electroplating grade copper oxide, high-purity technology, used in copper oxide/copper hydroxide and other directions

Inactive Publication Date: 2013-04-03
TAIXING SMELTING PLANT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regarding the production process of copper oxide, it is also involved in some invention patents disclosed at present. The application number is 01127175.2, which uses copper sulfate and copper material as raw materials, undergoes low-temperature oxidation at 80-85°C, obtains copper sulfate through crystallization, and then mixes it with Sodium hydroxide reaction, and then through ball milling, pressure filtration, washing, drying, and pulverization to obtain active copper oxide. Waste water; Application number is the technique that 200710076208.1 discloses to produce copper oxide through distilling ammonia with alkaline etching waste liquid, owing to be to make by distilling ammonia for a long time under high temperature, strong alkali state with alkaline etching waste liquid, so copper oxide activity is relatively Low; the application number is 200710071896.2, which discloses the reaction of copper nitrate and sodium hydroxide through pressure filtration, drying, and roasting to produce copper oxide, which will produce nitrogen dioxide or nitrogen monoxide waste gas, which will cause certain pollution to the environment; application number is 200810067243.1 The production process of synthesizing basic copper chloride as a precursor, and then reacting with sodium hydroxide to produce monoclinic copper oxide, but its activity has not been verified experimentally
At present, copper oxide for horizontal electroplating is also prepared from basic copper carbonate as raw material, but first, basic copper carbonate is mostly obtained by traditional technology, and the content of impurities such as iron and lead is high. Second, most manufacturers use pusher kiln calcining equipment for calcination. Basic copper carbonate prepares electroplating-grade copper oxide. This method has the following problems: (1) Due to the uneven temperature distribution in the kiln, the physical properties of the reaction material are not uniform enough, and the low-temperature part of the basic copper carbonate has not enough fire-through content, while the high-temperature part is oxidized. The copper has been burnt to death and loses its activity; (2) The slag from the charging sagger brings impurities such as silicon, aluminum, calcium and other contaminated products into the material, making the chemical composition of the electroplating grade copper oxide unable to meet the target requirements; (3) Because the material is fixed Bed, uneven temperature distribution, long production time and high energy consumption; (4) manual operation, labor-intensive, can not be automated

Method used

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  • Method for continuously preparing high-purity low-chloride electroplating copper oxide
  • Method for continuously preparing high-purity low-chloride electroplating copper oxide
  • Method for continuously preparing high-purity low-chloride electroplating copper oxide

Examples

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Effect test

Embodiment 1

[0049] Using standard cathode copper, liquid ammonia, and carbon dioxide with a purity of ≥99.9% as raw materials, the production process using HZD-80 rotary electric furnace calcination is as follows:

[0050] At 20m 3 Pump 15 meters into the concentrated ammonia preparation tank with cooling coil 3 Deionized water, open the liquid ammonia cylinder valve, make the liquid ammonia pressure into the preparation tank 0.2MPa, and pass ammonia gas for 6 hours to prepare a concentrated ammonia water with a concentration of 135g / L. Close the liquid ammonia cylinder valve; open the preparation tank The valve of the cooling water pipe, which is not connected to the concentrated ammonia water, is fed with cooling water whose temperature is less than 15℃, and then the carbon dioxide cylinder valve is opened to control the carbon dioxide pressure to 0.2MPa and the carbonization degree to 80% to produce carbonic acid. The carbonized ammonia water with the ammonium concentration of 3.18mol / L is...

Embodiment 2

[0055] Using standard cathode copper, liquid ammonia, and carbon dioxide with a purity of ≥99.9% as raw materials, the production process using HZD-80 rotary electric furnace calcination is as follows:

[0056] At 20m 3 Of concentrated ammonia preparation tank with cooling coil, pumped 15 meters 3 Deionized water, open the liquid ammonia cylinder valve, make the liquid ammonia pressure into the preparation tank 0.15MPa, and pass ammonia gas for 7 hours to prepare a concentrated ammonia water with a concentration of 120g / L. Close the liquid ammonia cylinder valve; open the preparation tank The valve of the cooling water pipe, which is not connected to the concentrated ammonia water, is fed with cooling water with a temperature of less than 15℃, and then the carbon dioxide cylinder valve is opened to control the pressure of the fed carbon dioxide at 0.15MPa and the degree of carbonization at 100% to produce ammonium carbonate. The carbonized ammonia water with the concentration of 3...

Embodiment 3

[0061] Using standard cathode copper, liquid ammonia, and carbon dioxide with a purity of ≥99.9% as raw materials, the production process using HZD-80 rotary electric furnace calcination is as follows:

[0062] At 20m 3 Of concentrated ammonia preparation tank with cooling coil, pumped 15 meters 3 Deionized water, open the liquid ammonia cylinder valve, make the liquid ammonia pressure into the preparation tank 0.1MPa, and pass ammonia gas for 7 hours to prepare a concentrated ammonia water with a concentration of 85g / L. Close the liquid ammonia cylinder valve; open the preparation tank The valve of the cooling water pipe, which is not connected to the concentrated ammonia water, is fed with cooling water with a temperature of less than 15℃, and then the carbon dioxide cylinder valve is opened to control the pressure of the carbon dioxide to be fed at 0.1MPa and the degree of carbonization at 140% to produce carbonic acid Carbonized ammonia water with a concentration of ammonium s...

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Abstract

The invention discloses a method for continuously preparing high-purity low-chloride electroplating copper oxide. According to the method, pure copper, liquid ammonia and high-purity carbon dioxide are taken as raw materials for producing high-purity basic cupric carbonate, so that the problem of impurities such as chlorine and the like in the conventional method for producing the raw materials of the basic cupric carbonate is avoided and the purity of the basic cupric carbonate is improved; and the high-purity basic cupric carbonate is calcined through a rotary electric furnace without scale on the inner wall for continuously preparing the electroplating copper oxide, so that the shortcomings of low content of the basic cupric carbonate due to no complete combustion of the basic cupric carbonate at the low-temperature part and complete combustion of the copper oxide at the high-temperature part in the static calcining process of a pushed slab kiln, loss of activity, high impurity content, high labor intensity, discontinuity in production, long cycle, high energy consumption, high cost and the like are overcome, the product activity is guaranteed, the product quality is high, the energy consumption is low, the cost is low, and the environment is more protected.

Description

technical field [0001] The invention belongs to the field of copper oxide production, and in particular relates to a method for continuously preparing high-purity low-chlorine electroplating-grade copper oxide using high-purity basic copper carbonate produced in an external coil tube internal stirring reactor as a raw material. Background technique [0002] In the PCB manufacturing process, the traditional electroplating process uses a copper plate as the anode plate and supplements the copper source. Due to the complex shape of the electronic components, there are holes, concave-convex surfaces and other shapes. In the holes, the electroplating solution cannot penetrate, so the plating Less than copper, the protruding part has a high current density and a thick coating, while the concave part has a low current density and a thin coating, resulting in unqualified products. [0003] At present, the horizontal electroplating process is common in the PCB manufacturing industry ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G3/02
Inventor 徐金章刘后传许明才
Owner TAIXING SMELTING PLANT
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