Method for recovering brownification waste liquid

A recovery method and technology of browning liquid, applied in the direction of improving process efficiency, etc., can solve the problems of lack of effective components, unfavorable growth and reproduction of microorganisms, and high cost of oxidative degradation method.

Active Publication Date: 2021-05-18
深圳星河环境股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the browning waste liquid has strong film-forming ability, strong complexing ability, stable existence under strong acidic and weak oxidant conditions and is not easy to be oxidized and degraded, the above treatment methods have their own defects.
In the process of electrolysis and electroosmosis, the browning waste liquid is easy to form a film on the surface of the electrode and the ion exchange membrane, and the treatment efficiency is low; in the extraction and resin adsorption treatment, the organic matter and copper ions cannot be separated well; after adding NaOH, Na 2 In the sedimentation treatment of browning waste liquid by reagents such as S, the purity of the precipitate produced is low and difficult to separate, which is not an ideal copper precipitation method; the cost of oxidation degradation method is too high; distillation method will decompose part of the low boiling point additives or some additives in the place Interaction under controlled temperature, resulting in the loss of some active ingredients in the browning solution and the imbalance of the effective component distribution of the original browning solution; the use of chemical precipitation method, that is, the acid-base neutralization method, this method is simple in process and consumes a lot of alkali , waste water is difficult to discharge, and the degree of copper resource utilization is low; because the content of inorganic salts such as copper sulfate in the waste browning liquid is too high, which is not conducive to the growth and reproduction of microorganisms, it is not suitable to use biological degradation

Method used

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  • Method for recovering brownification waste liquid
  • Method for recovering brownification waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Before recycling, the content of the main components of the used browning waste liquid is determined. Through EDTA titration, the copper content in the browning waste liquid was measured to be 25g / L; through acid-base titration, the sulfuric acid concentration in the browning waste liquid was measured to be 1mol / L; the chemical oxygen demand measured by the dichromate method The content (COD) is 10000ppm, which means that browning waste liquid contains a lot of organic matter.

[0034] Add alkaline substances such as copper hydroxide or copper oxide to 1L browning waste liquid, adjust the pH to 0-2; stir and dissolve, and then pass SO into the solution 2 Gas, the solution began to be turbid and precipitated. After 1-2 hours of aeration reaction, a large amount of precipitates appeared in the solution. After stopping the aeration, filter to obtain the precipitate and the first filtrate.

[0035] The above-mentioned first filtrate is fully aerated for 1-2 hours to obtain...

Embodiment 2

[0039] The difference from Example 1 is: in the preparation step of the regenerated browning liquid, the quality of the additive sub-liquid is 15g, and the added sulfuric acid is 107mL (the concentration is 50%, and the density is 1.4g / cm 3 ), the added hydrogen peroxide is 17mL (concentration is 50%, density is 1.2g / cm 3 ); that is, the mass volume ratio of the additive sub-liquid accounting for the regenerated browning solution is 1.5%; the added sulfuric acid quality is 75g, and the added sulfuric acid accounts for 7.5% of the mass volume ratio of the regenerated browning solution; the added hydrogen peroxide The mass is 10g, and the mass volume ratio of the added hydrogen peroxide to the regenerated browning solution is 1%. The rest of the conditions are exactly the same as in Example 1, and will not be repeated here.

Embodiment 3

[0041] The difference from Example 1 is: in the preparation step of the regenerated browning liquid, the quality of the additive sub-liquid is 80g, and the added sulfuric acid is 214mL (the concentration is 50%, and the density is 1.4g / cm 3 ), the added hydrogen peroxide is 50mL (concentration is 50%, density is 1.2g / cm 3 ); That is, the mass volume ratio of the additive sub-liquid accounting for the regenerated browning solution is 8%; the added sulfuric acid quality is 150g, and the added sulfuric acid accounts for 15% of the mass volume ratio of the regenerated browning solution; the added hydrogen peroxide The mass is 30g, and the mass volume ratio of the added hydrogen peroxide to the regenerated browning solution is 3%. The rest of the conditions are exactly the same as in Example 1, and will not be repeated here.

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Abstract

The invention provides a method for recovering brownification waste liquid. The method comprises the following steps: complexation and impurity removal: adding alkaline substances into the brownification waste liquid, adjusting the pH value to be 0-2, introducing SO2 gas to react to generate a precipitate, and filtering to obtain the precipitate and first filtrate; metal copper reduction: adding deionized water into the precipitate, stirring and slurrying, adding an alkaline solution to adjust the pH value to obtain a neutral solution, then adding hydrazine hydrate, fully stirring, reacting to generate copper sponge and nitrogen, and filtering to obtain the copper sponge and second filtrate; and preparation of regenerated brownification liquid: adding an additive into the second filtrate to obtain additive sub-liquid, and adding sulfuric acid, hydrogen peroxide and a stabilizer into the additive sub-liquid to obtain the regenerated brownification liquid. By means of the method, the problem that a large amount of brownification waste liquid in a PCB factory needs to be treated in an outsourced mode can be solved, meanwhile, the purpose of recycling part of the waste liquid can be achieved, and implementation of circular economy is facilitated.

Description

technical field [0001] The invention relates to the technical field of waste liquid treatment, in particular to a recovery method of browning waste liquid. Background technique [0002] In the manufacturing process of PCB (Printed circuit board, printed circuit board) multilayer board, the browning process of inner layer board is more and more widely used. The browning treatment process is a chemical copper corrosion reaction process. When the amount of copper dissolved in the browning solution exceeds the standard and the browning effect fails, browning waste liquid is produced. The main components of browning waste liquid are high-concentration sulfuric acid, hydrogen peroxide, copper microetching agent, stabilizer and a large amount of copper ions and other complex compounds and reaction products. Browning waste liquid contains a large amount of harmful substances, which can be directly Emissions will destroy the ecological balance and endanger human health. And these w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B15/00C23F1/46C23F1/18
CPCC22B7/006C22B15/0089C23F1/46C23F1/18Y02P10/20
Inventor 宋传京邹毅芳叶自洁陆严宏乔贞
Owner 深圳星河环境股份有限公司
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