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Method for preparing copper oxide based on acidic etching liquid as raw material

An acid etching solution, copper oxide technology, applied in copper oxide/copper hydroxide and other directions, can solve the problems of increased liquid volume, uneven stirring and temperature rise, increased waste water discharge, etc., to achieve easy control, uniform particle size, and economical The effect of production costs

Active Publication Date: 2012-01-04
昆山德阳新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing problems are: the Cu(OH) 2 produced in the first stage is a viscous jelly, the stirring and heating are uneven, and the acid etching solution used needs to be diluted before it can be operated, and the diluted Undoubtedly lead to an increase in the volume of the liquid, resulting in an increase in the discharge of wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The present embodiment provides a kind of preparation method of high-purity copper oxide, and it comprises the steps:

[0018] (1) Take 200mL of acidic etching waste liquid, add 25wt% sodium hydroxide aqueous solution under the condition of constant stirring, until the pH is 11, continue stirring at a stirring speed of 500 rpm for 10 minutes, and then let it stand for about 8 minutes;

[0019] (2) Transfer the solution treated in step (1) into a stainless steel reaction kettle lined with polytetrafluoroethylene, add pure water to 75% of the total volume of the kettle, and hydrothermally synthesize it at 150°C for 5 hours. , naturally cooled to room temperature, collected the material at the bottom of the kettle, washed with deionized water first, then washed with alcohol, and then dried at 90°C for 8 hours to obtain 20.5g of copper oxide. The tested copper oxide content is 99.5%, the average particle size is 15nm, the maximum particle size is 30nm, and the minimum...

Embodiment 2

[0021] The present embodiment provides a kind of preparation method of high-purity copper oxide, and it comprises the steps:

[0022] (1) Take 500mL of acidic etching waste liquid, add 15wt% sodium hydroxide aqueous solution under the condition of constant stirring, until the pH is 10, continue to stir at 650 rpm for 15 minutes, and then let it stand for about 8 minutes;

[0023] (2) Transfer the solution treated in step (1) into a stainless steel reaction kettle lined with polytetrafluoroethylene, add pure water to 75% of the total volume of the kettle, and hydrothermally synthesize it at 180°C for 4 hours. , naturally cooled to room temperature, collected the material at the bottom of the kettle, first washed with deionized water, then washed with alcohol, and then dried at 90°C for 8 hours to obtain 53g of copper oxide. The tested copper oxide content is 99.6%, the average particle size is 18nm, the maximum particle size is 30nm, and the minimum particle size is 11nm....

Embodiment 3

[0025] The present embodiment provides a kind of preparation method of high-purity copper oxide, and it comprises the steps:

[0026] (1) Take 400mL of acidic etching waste liquid, add 50wt% sodium hydroxide aqueous solution under the condition of constant stirring, until the pH is 12, continue to stir at 800 rpm for 25 minutes, and then let it stand for about 8 minutes;

[0027] (2) Transfer the solution treated in step (1) into a stainless steel reaction kettle lined with polytetrafluoroethylene, add pure water to 75% of the total volume of the kettle, and hydrothermally synthesize it at 180°C for 6 hours. , cooled naturally to room temperature, collected the material at the bottom of the kettle, washed with deionized water first, then washed with alcohol, and then dried at 95°C for 8 hours to obtain 39g of copper oxide. The tested copper oxide content is 99.3%, the average particle size is 15nm, the maximum particle size is 26nm, and the minimum particle size is 10nm....

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PUM

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Abstract

The invention relates to a method for preparing copper oxide based on an acidic etching liquid as a raw material. The method comprises the following steps: (1) regulating the pH of the acidic etching liquid to 10-13 with sodium hydroxide or potassium hydroxide; (2) transferring the etching liquid obtained in the step (1) into a stainless steel reaction kettle with a teflon lining, adding pure water to 70%-80% of total kettle volume, and carrying out hydrothermal synthesis for 2-10 hours at the temperature of 120-200 DEG C; and (3) after the reaction is finished, naturally cooling to room temperature, collecting materials at the kettle bottom, and successively washing with deionized water and alcohol, and then drying so as to obtain copper oxide. According to the invention, copper oxide isprepared from the acidic etching liquid by using the hydrothermal synthesis method, and obtained copper oxide has the advantages of high purity, high activity and uniform particle diameter. In addition, the method has no secondary pollution and low production cost.

Description

technical field [0001] The invention relates to a method for preparing copper oxide by using an acid etching solution as a raw material. Background technique [0002] Copper oxide is a very important metal oxide material, which has a wide range of applications in the fields of catalysis, superconductivity, organic synthesis, and printed circuit board electroplating. [0003] With the annual growth rate of my country's electronics industry exceeding 20%, it has driven the development of printed circuit board (PCB) and related industries, and my country has become the world's largest PCB production center. Acid etching circuit board is the main direction of etching development, the main component of acid etching solution is CuCl 2 , HCl, NaCl, etc., so it is imperative to recover copper ions in acidic etching waste at low cost. At present, the main treatment methods for etching waste liquid include electrolysis, solvent extraction, chemical precipitation, etc., but ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G3/02
Inventor 廖奕坤徐佳琦朱婷柏琳
Owner 昆山德阳新材料科技有限公司
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