Method and system for reclaiming valuable resource in acidic etching waste liquid

A technology of acidic etching waste liquid and etching waste liquid, applied in chemical instruments and methods, copper sulfate, chlorine/hydrogen chloride, etc., can solve problems such as difficulty in completely replacing hydrogen chloride, low copper recovery rate, etc.

Inactive Publication Date: 2008-07-09
郝屿
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method cannot release cuprous ions in the form of complexes, and the recovery rate of copper is low
In addition, the amount of concentrated sulfuric acid added is based on copper ions, and the excess is 5% to 15%. The excess of sulfuric acid is small, and it is difficult to completely replace the hydrogen chloride in the distillation and etching waste liquid.

Method used

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  • Method and system for reclaiming valuable resource in acidic etching waste liquid
  • Method and system for reclaiming valuable resource in acidic etching waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040]2000L etching waste solution (9.2wt% same content, 14.5wt% chlorine content, 1.3g / mL density) was oxidized by bubbling air under stirring conditions until the solution was transparent. Mix 400L of 98wt% concentrated sulfuric acid with the oxidized etching waste liquid and keep stirring to form the etching waste liquid. Heat the etching waste liquid with 0.07MPa saturated water vapor, then carry out negative pressure evaporation, the pressure is 0.06MPa, discharge the residue, and filter, then wash the copper sulfate crystal with saturated copper sulfate aqueous solution and absolute ethanol to obtain CuSO 4 .5H 2 O 939.1Kg, the purity is 99%. The recovery rate is 99.5%. Produced water vapor and hydrogen chloride were condensed to obtain 1542.7Kg of 25wt% hydrochloric acid with a recovery rate of 99.5%.

Embodiment 2

[0042] Add 30% hydrogen peroxide to 2500 L of the same waste etching solution as in Example 1 under agitation until the solution is transparent. Mix 750L of 95wt% concentrated sulfuric acid with the above solution and keep stirring. Heat the etching waste liquid with 0.08MPa saturated water vapor, then evaporate under negative pressure, discharge the residue, and obtain CuSO by filtration 4 .3H 2 O and CuSO 4 .5H 2 The mixture of O was 1092.6Kg, and the recovery rate was 99.2%. The generated water vapor and hydrogen chloride were condensed to obtain 1848.6Kg of 26wt% hydrochloric acid with a recovery rate of 99.2%.

Embodiment 3

[0044] Under stirring conditions, air was blown into 300 L of the etching waste liquid of Example 1 for oxidation treatment until the solution was transparent. Mix 120L of 98% concentrated sulfuric acid with the above clear solution and keep stirring. Heat the etching waste liquid with 0.08MPa saturated water vapor, then carry out negative pressure evaporation, discharge the residue, obtain copper sulfate crystals by filtration, then wash with saturated copper sulfate aqueous solution and absolute ethanol, and perform purification treatment to obtain 140.3Kg CuSO 4 .5 H 2O with a purity of 99.2% and a recovery of 99.3%. Produced water vapor and hydrogen chloride were condensed to obtain 224.4Kg of 25wt% hydrochloric acid with a recovery rate of 99.2%.

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Abstract

Provided are system of value resource in acidic corrosion waste fluid and a recycling method. The recycling method of the invention includes the following steps that adding oxidation agent and concentrated sulfuric acid into the corrosion waste fluid, pre-heating and heating the corrosion waste fluid, evaporating out water vapor and hydrogen chloride under negative pressure and recycling hydrochloric acid, the residue separates hydric sulphate from blue copperas crystal via centrifugal filtration and recycle hydric sulphate, washing blue copperas crystal by blue copperas crystal solution and absolute ethyl alcohol and recycling blue copperas. The recycling system comprises an oxidation ditch, a dosage bunker, a pre-heater, a heat booster, an evaporation tank, a filter, a cooler, a spraying and absorbing device and the like. The recycling method of the invention increases the recovery rate of metal copper and hydrogen chloride, with both recovery rates more than 99%. The method can employ scheme of batch operation or continuous recycling, which is adapted for industry utilization.

Description

technical field [0001] The invention relates to a recovery method and recovery system for valuable resources in acidic industrial waste water, in particular to a recovery method and recovery system for valuable resources in acidic etching waste liquid. Background technique [0002] Acidic etching waste liquid is a kind of industrial waste water produced in the process of making the inner layer circuit pattern of multilayer printed board, the main component is Cu 2+ 、H + , CuCl, [CuCl 3 ] 2- and [CuCl 4 ] 2- , the copper content is 120-160g / L, and the density is 1.2-1.4g / mL. my country is a big producer of printed boards second only to Japan, and the copper in the form of copper clad laminates consumed has accounted for 30% of the country's total. During the etching process of printed boards, more than 60% to 70% of the copper in the copper-clad laminates is etched and enters the etching solution, thus producing a large amount of high-concentration copper-containing aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C02F1/72C02F1/04C01B7/01C01G3/10
CPCC23F1/46
Inventor 郝屿蒋玉思
Owner 郝屿
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