CN101792220A - Comprehensive treatment method of acidic etching waste liquid - Google Patents
Comprehensive treatment method of acidic etching waste liquid Download PDFInfo
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- CN101792220A CN101792220A CN 201010125454 CN201010125454A CN101792220A CN 101792220 A CN101792220 A CN 101792220A CN 201010125454 CN201010125454 CN 201010125454 CN 201010125454 A CN201010125454 A CN 201010125454A CN 101792220 A CN101792220 A CN 101792220A
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Abstract
The invention relates to a comprehensive treatment method of acidic etching waste water. Tail water treated by the existing treatment method can not conform to the standard. The method comprises the following steps: firstly adding oxydol to an acidic etching waste liquid to be treated for breaking and regeneration; then adding 98% concentrated sulfuric acid, distilling by heating, and absorbing the distilled steam with clean water to obtain dilute hydrochloric acid; dissolving residues after the distillation in a solution to generate a mother solution, throwing nano filter membranes and reverse osmosis membranes for concentration and separation, cooling and crystallizing the condensed mother solution, rinsing with water, and drying to obtain a copper sulfate crystal product. The method comprehensively uses the resources of the acidic etching waste liquid, produces the industrial dilute hydrochloric acid and copper sulfate products, ensures that the discharged waste water conform to the standard, improves the resource recovery rate of copper, and also raises the distillation speed.
Description
Technical field
The present invention relates to a kind of comprehensive recovery and treatment method of industrial effluent, be specifically related to a kind of treatment process of acidic etching waste liquid, utilize this method can from acidic etching waste liquid, reclaim hydrochloric acid and copper sulfate, and realize qualified discharge.
Background technology
Acidic etching liquid is mainly adopted in present domestic single side printed wiring board production.Acidic etching liquid is the etching solution that a kind of suitable fine-line plate is made, and its system is abundanter, and modal is hydrochloric acid/cupric chloride system.Etching waste liquor is an omplicated solution system that contains multiple complexing ion, contains the cupric ion and the acidity of high density, belongs to Hazardous wastes, must adopt special-purpose method or technology to handle.At present to the following several treatment processs of the normal employing of acidic etching waste liquid: remove unnecessary hydrochloric acid with copper scrap, cupric oxide etc. and hydrochloric acid reaction, or directly use a large amount of alkali neutralizing acids, again with substitution method, in and extraction process, membrane electrolysis produce copper coin or copper sulfate product, also have and adopt sulfuric acid distillation substitution method to reclaim hydrochloric acid and copper sulfate synchronously.200610038080.5), take the patent of invention (patent No.: of technology as the leading factor with electrolysis 200610062086.6) and the utility model patent (patent No.: 200520067901.9) patent of invention of handling at the etching waste liquor that the contains oxalic acid (patent No.: 200510080937.5), reclaim the patent of invention of hydrochloric acid and the copper sulfate (patent No.: for example to add sulfuric acid displacement distillation.
The problem maximum is that tail water can not qualified discharge in the present acidic etching waste liquid treatment process.Add in the alkali and do not accomplish the resource recycling, and increased the saltiness of waste water with the method for remaining acid.The substitution method input is economized most, but contains a large amount of salt in the tail water and the cupric ion that exceeds standard, and administers to bother most; The extraction agent cost height of extraction process, run off greatly, the rate of recovery of copper is limited; Be easy to generate hydrogen and chlorine during diaphragm electrolysis, dangerous high, production cost is big; Sulfuric acid extractive distillation method is not improved solution to the tail water cupric ion problem of exceeding standard.
Summary of the invention
Purpose of the present invention is exactly at the deficiencies in the prior art, and a kind of integrated conduct method that can make acidic etching waste liquid comprehensive utilization, tail water qualified discharge is provided.
For achieving the above object, the inventive method realizes by following steps:
(1) contact break regeneration
Hydrogen peroxide is joined in the pending acidic etching waste liquid of concentration of hydrochloric acid 2～4N, copper ion concentration 120～160g/L, stirring reaction 20～40 seconds makes that the cupric ion of complexing is divalent ion in the acidic etching waste liquid; The hydrogen peroxide that adds and the volume ratio of pending acidic etching waste liquid are 0.005～0.008: 1.
(2) vacuum distillation
The vitriol oil with 98% joins in the acidic etching waste liquid after the contact break, adds thermal distillation then; The vitriol oil that adds and the volume ratio of pending acidic etching waste liquid are 0.08～0.13: 1, and distillation temperature is 100～120 ℃; The steam utilization water sprayer that distills out carries out clear water and absorbs, and the dilute hydrochloric acid that obtains is inserted in the storage tank, and the water sprayer vacuum pressure is 1～3kPa.
(3) mother liquor concentrates
Residue behind the vacuum distillation is added lysate be dissolved into mother liquor, the lysate of adding and the weight ratio of residue are 1: 0.3～0.6, and the first lysate that adds is a water; With high-pressure pump mother liquor is squeezed into nanofiltration membrane, under the pressure of 0.9～1.9MPa, carry out concentrating and separating; If content of copper ion surpasses emission standard in the clear liquid that leaches, then the clear liquid that leaches is squeezed into reverse osmosis membrane with high-pressure pump, under the pressure of 0.9～1.9MPa, carry out concentrating and separating, content of copper ion reaches emission standard in the clear liquid that leaches; Mother liquor after concentrating utilizes distillatory steam to heat.
(4) crystallisation by cooling
Mother liquor after concentrated and the heating is carried out crystallisation by cooling,, obtain the crystalline sulfuric acid copper products after the drying the xln water wash.
(5) washing lotion refluxes
Incorporate crystallization raffinate and leacheate into the mother liquor enrichment step, replace water as lysate.
The inventive method has been carried out comprehensive utilization of resources to acidic etching waste liquid, output industrial dilute hydrochloric acid and copper sulfate product, guaranteed the qualified discharge of efflux wastewater, improved the resource recovery of copper, also improved distillation speed simultaneously.The present invention is particularly suitable for the construction of middle-size and small-size set treatment device.
Description of drawings
Fig. 1 is the equipment synoptic diagram of the inventive method.
Embodiment
Describe the inventive method in detail below in conjunction with accompanying drawing.
As shown in Figure 1, the equipment of the inventive method employing comprises: still kettle S1, relay tank S2, high-pressure pump S3, membrane module S4, interchanger S5, water sprayer S6, product storage tank S7, low-pressure pump S8, crystallizer S9, leaching device S10, moisture eliminator S11.
The connection of each equipment is as follows: the import of still kettle S1 is connected with auxiliary agent pipeline L2 with acidic etching waste liquid pipeline L1, the vapour outlet of still kettle S1 is connected by the interior hot-fluid tube inlet of vapour line L3 and interchanger S5, and the outlet of hot-fluid pipe is connected with the vacuum liquid-absorbing mouth of water sprayer S6 by pipeline.The cold fluid pipeline inlet of interchanger S5 is connected with the mother liquor outlet of membrane module S4 by pipeline, the outlet of cold fluid pipeline is connected by the feed entrance of pipeline with crystallizer S9, the raffinate outlet of crystallizer S9 is connected with the end of raffinate return line L5, the products export of crystallizer S9 directly connects leaching device S10, the leacheate inlet of leaching device S10 connects the clear water pipeline, the products export of leaching device S10 directly connects moisture eliminator S11, the products export of moisture eliminator S11 is the discharge outlet of solid phase prod, and the leacheate outlet of leaching device S10 is connected with the end of leacheate return line L6.After the other end of the other end of raffinate return line L5 and leacheate return line L6 converges, converge with the outlet at bottom pipeline of still kettle S1, and be connected with the opening for feed of relay tank S2.The outlet of relay tank S2 is connected with the import of high-pressure pump S3, and the outlet of high-pressure pump S3 is connected with the opening for feed of membrane module S4, and the liquid outlet that sees through of membrane module S4 is connected with cleaner liquid pipeline L4.The outlet of water sprayer S6 is connected by the inlet of pipeline with product storage tank S7, and the outlet at bottom of product storage tank S7 is connected with the inlet of low-pressure pump S8, and the outlet of low-pressure pump S8 is connected by the water-in of pipeline with water sprayer S6.
System operation method: pending acidic etching waste liquid is pumped into acidic etching waste liquid pipeline L1 enter still kettle S1, reaction promoter (is added hydrogen peroxide earlier, add the vitriol oil again) squeeze into auxiliary agent pipeline L2 with pump respectively and enter still kettle S1, energising heating or adopt steam heating.Inject simultaneously the clear water (to middle liquid level) of half in the product storage tank S7 in advance, start low-pressure pump S8, make water sprayer S6 work, be the vacuum distillation state in the drive still kettle.The distillation back that finishes adds an amount of clear water dissolved residue in still kettle, end liquid is entered relay tank S2, starts high-pressure pump S3, controls the operating pressure of membrane module well, makes membrane module S4 works better.Close the outlet valve of still kettle S1 after the material emptying in the still S1 to be distilled, in still kettle S1, add new a collection of stock liquid and reaction promoter again, move continuously with method.The operating pressure of membrane module S4 required cleaner liquid Flow-rate adjustment during according to system stable operation, and guarantee to be operated within the safe pressure scope of membrane module.Start crystallizer S9 when having material liquid to enter among the device S9 to be crystallized, when material to be had enters leaching device S10, open the clear water drip washing valve of leaching device S10 again, start moisture eliminator S11 at last, dry intact product is solid-state, uses packaging bags.The product storage tank is taked the work of compartment discharge opeing water supplementing method, promptly opens tapping valve when the liquid level in the storage tank attains to a high place, and liquid level is closed tapping valve after dropping to lowest order, opens water intaking valve moisturizing to mid water levels again and stops to get final product.
Below specify the inventive method by three embodiment.
With 1m
3The pending acidic etching waste liquid of concentration of hydrochloric acid 2N, copper ion concentration 120g/L pumps into still kettle, adds hydrogen peroxide 5L, adds 98% vitriol oil 80L behind the stirring reaction 20s and adds thermal distillation, adopts the saturated vapo(u)r heating, and 100 ℃ of still temperature are until evaporate to dryness.The clear water that adds 300L in the product storage tank in advance, the steam utilization water sprayer that distills out carry out clear water and absorb, and the water sprayer vacuum pressure is 1kPa, and the dilute hydrochloric acid volume became 1350L after distillation was finished, and concentration is 15%.In still kettle, add clear water more while hot, as the lysate dissolved residue, with high-pressure pump mother liquor is squeezed into nanofiltration membrane, under the pressure of 0.9MPa, carry out concentrating and separating, discharge filtrate 40L and utilize distillatory steam to heat, behind the crystallisation by cooling, with the xln water wash, obtain cupric sulfate pentahydrate 370kg after the drying, the copper ion concentration of discharging clear liquid is lower than 0.5mg/L, reaches emission standard.Crystallization raffinate and leacheate are joined in the still kettle, and as the lysate dissolved residue, the weight ratio of lysate in the dissolved residue process (crystallization raffinate and leacheate or clear water) and residue remains between 1: 0.3～0.6.
Embodiment 2
With 1m
3The pending acidic etching waste liquid of concentration of hydrochloric acid 3N, copper ion concentration 140g/L pumps into still kettle, adds hydrogen peroxide 6.5L, adds 98% vitriol oil 100L behind the stirring reaction 30s and adds thermal distillation, adopts electrically heated, and 110 ℃ of still temperature are until evaporate to dryness.The clear water that adds 250L in the product storage tank in advance, the steam utilization water sprayer that distills out carry out clear water and absorb, and the water sprayer vacuum pressure is 2kPa, and the dilute hydrochloric acid volume became 1360L after distillation was finished, and concentration is 17%.In still kettle, add clear water more while hot, as the lysate dissolved residue, select the combination of nanofiltration membrane and reverse osmosis membrane for use, working pressure is discharged filtrate 70L and is utilized distillatory steam to heat under 1.9MPa, behind the crystallisation by cooling,, obtain cupric sulfate pentahydrate 460kg after the drying with the xln water wash, the copper ion concentration of discharging clear liquid is lower than 0.5mg/L, reaches emission standard.Crystallization raffinate and leacheate are joined in the still kettle, and as the lysate dissolved residue, the weight ratio of lysate in the dissolved residue process (crystallization raffinate and leacheate or clear water) and residue remains between 1: 0.3～0.6.
With 1m
3The pending acidic etching waste liquid of concentration of hydrochloric acid 4N, copper ion concentration 160g/L pumps into still kettle, adds hydrogen peroxide 8L, adds 98% vitriol oil 130L behind the stirring reaction 40s and adds thermal distillation, adopts electrically heated, and 120 ℃ of still temperature are until evaporate to dryness.The clear water that adds 200L in the product storage tank in advance, the steam utilization water sprayer that distills out carry out clear water and absorb, and the water sprayer vacuum pressure is 3kPa, and the dilute hydrochloric acid volume became 1380L after distillation was finished, and concentration is 20%.In still kettle, add clear water more while hot, as the lysate dissolved residue, select the combination of nanofiltration membrane and reverse osmosis membrane for use, working pressure is discharged filtrate 100L and is utilized distillatory steam to heat under 1.5MPa, behind the crystallisation by cooling,, obtain cupric sulfate pentahydrate 540kg after the drying with the xln water wash, the copper ion concentration of discharging clear liquid is lower than 0.5mg/L, reaches emission standard.Crystallization raffinate and leacheate are joined in the still kettle, and as the lysate dissolved residue, the weight ratio of lysate in the dissolved residue process (crystallization raffinate and leacheate or clear water) and residue remains between 1: 0.3～0.6.
Claims (1)
1. the integrated conduct method of an acidic etching waste liquid is characterized in that these method concrete steps are:
Step (1) contact break regeneration
Hydrogen peroxide is joined in the pending acidic etching waste liquid of concentration of hydrochloric acid 2～4N, copper ion concentration 120～160g/L, stirring reaction 20～40 seconds makes that the cupric ion of complexing is divalent ion in the acidic etching waste liquid; The hydrogen peroxide that adds and the volume ratio of pending acidic etching waste liquid are 0.005～0.008: 1;
Step (2) vacuum distillation
The vitriol oil with 98% joins in the acidic etching waste liquid after the contact break, adds thermal distillation then; The vitriol oil that adds and the volume ratio of pending acidic etching waste liquid are 0.08～0.13: 1, and distillation temperature is 100～120 ℃; The steam utilization water sprayer that distills out carries out clear water and absorbs, and the dilute hydrochloric acid that obtains is inserted in the storage tank, and the water sprayer vacuum pressure is 1～3kPa;
Step (3) mother liquor concentrates
Residue behind the vacuum distillation is added lysate be dissolved into mother liquor, the lysate of adding and the weight ratio of residue are 1: 0.3～0.6, and the first lysate that adds is a water; With high-pressure pump mother liquor is squeezed into nanofiltration membrane, under the pressure of 0.9～1.9MPa, carry out concentrating and separating; If content of copper ion surpasses emission standard in the clear liquid that leaches, then the clear liquid that leaches is squeezed into reverse osmosis membrane with high-pressure pump, under the pressure of 0.9～1.9MPa, carry out concentrating and separating, content of copper ion reaches emission standard in the clear liquid that leaches; Mother liquor after concentrating utilizes distillatory steam to heat;
Step (4) crystallisation by cooling
Mother liquor after concentrated and the heating is carried out crystallisation by cooling,, obtain the crystalline sulfuric acid copper products after the drying the xln water wash;
Step (5) washing lotion refluxes
Incorporate crystallization raffinate and leacheate into step (3) and carry out mother liquor and concentrate, replace water as lysate.
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| CN 201010125454 CN101792220A (en) | 2010-03-16 | 2010-03-16 | Comprehensive treatment method of acidic etching waste liquid |
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| CN 201010125454 CN101792220A (en) | 2010-03-16 | 2010-03-16 | Comprehensive treatment method of acidic etching waste liquid |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102978567A (en) * | 2012-12-21 | 2013-03-20 | 合肥工业大学 | Method for preparing photoetching-free high-precision mask for evaporated electrodes |
| CN103787400A (en) * | 2013-12-30 | 2014-05-14 | 广州科城环保科技有限公司 | Method for treating microetching liquid waste and copper sulfate liquid waste |
| CN104085911A (en) * | 2014-06-28 | 2014-10-08 | 南通久信石墨科技开发有限公司 | Process device for generating copper sulfate by replacing copper etchant |
| CN104176871A (en) * | 2014-09-04 | 2014-12-03 | 北京赛科康仑环保科技有限公司 | Recovery treatment method of acidic etching waste liquor |
| CN105174219A (en) * | 2015-10-19 | 2015-12-23 | 湖州森诺膜技术工程有限公司 | System for concentrating dilute hydrochloric acid by adopting vacuum type membrane distillation system |
| CN105540975A (en) * | 2015-12-30 | 2016-05-04 | 北京赛科康仑环保科技有限公司 | Recycling method and system of PCB (printed circuit board) etching waste liquid |
| CN106185810A (en) * | 2016-07-27 | 2016-12-07 | 方亚飞 | A kind of joint disposal technique of acidic copper chloride waste etching solution |
| CN106587317A (en) * | 2016-12-30 | 2017-04-26 | 江门市崖门新财富环保工业有限公司 | Concentrated acid fractional distillation treatment process for copper ammonia concentrated liquid of circuit board |
| CN107099802A (en) * | 2017-06-16 | 2017-08-29 | 深圳市新锐思环保科技有限公司 | A kind of novel acid etching solution resource recycling method and recycling system |
| CN107354461A (en) * | 2017-09-13 | 2017-11-17 | 田成 | A kind of printed circuit board acidic etching waste liquor process for regenerating, recovering and reutilizing |
| CN108793095A (en) * | 2018-09-26 | 2018-11-13 | 高频美特利环境科技（北京）有限公司 | Solution impurity-removing method and solution impurity removed system |
| CN111020633A (en) * | 2019-12-23 | 2020-04-17 | 广东臻鼎环境科技有限公司 | Treatment method of acidic etching waste liquid |
| CN113336259A (en) * | 2021-08-06 | 2021-09-03 | 清大国华环境集团股份有限公司 | Method for recycling acidic copper sulfate waste liquid |
| CN114561669A (en) * | 2022-03-03 | 2022-05-31 | 无锡中天固废处置有限公司 | Method for recycling acidic copper-containing ammonium-containing etching waste liquid |
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| CN101113013A (en) * | 2007-06-26 | 2008-01-30 | 深圳市万山红环保实业有限公司 | Method and device for preparing cupric oxide/cupric sulfate by reclaiming wiring board etching waste liquor |
| CN101215062A (en) * | 2007-12-26 | 2008-07-09 | 郝屿 | Method and system for reclaiming valuable resource in acidic etching waste liquid |
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Patent Citations (2)
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| CN101113013A (en) * | 2007-06-26 | 2008-01-30 | 深圳市万山红环保实业有限公司 | Method and device for preparing cupric oxide/cupric sulfate by reclaiming wiring board etching waste liquor |
| CN101215062A (en) * | 2007-12-26 | 2008-07-09 | 郝屿 | Method and system for reclaiming valuable resource in acidic etching waste liquid |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102978567A (en) * | 2012-12-21 | 2013-03-20 | 合肥工业大学 | Method for preparing photoetching-free high-precision mask for evaporated electrodes |
| CN103787400A (en) * | 2013-12-30 | 2014-05-14 | 广州科城环保科技有限公司 | Method for treating microetching liquid waste and copper sulfate liquid waste |
| CN103787400B (en) * | 2013-12-30 | 2015-08-05 | 广州科城环保科技有限公司 | The treatment process of a kind of microetch waste liquid and bluestone waste |
| CN104085911A (en) * | 2014-06-28 | 2014-10-08 | 南通久信石墨科技开发有限公司 | Process device for generating copper sulfate by replacing copper etchant |
| CN104176871A (en) * | 2014-09-04 | 2014-12-03 | 北京赛科康仑环保科技有限公司 | Recovery treatment method of acidic etching waste liquor |
| CN104176871B (en) * | 2014-09-04 | 2016-05-18 | 北京赛科康仑环保科技有限公司 | A kind of recycling processing method for acidic etching waste liquid |
| CN105174219A (en) * | 2015-10-19 | 2015-12-23 | 湖州森诺膜技术工程有限公司 | System for concentrating dilute hydrochloric acid by adopting vacuum type membrane distillation system |
| CN105540975A (en) * | 2015-12-30 | 2016-05-04 | 北京赛科康仑环保科技有限公司 | Recycling method and system of PCB (printed circuit board) etching waste liquid |
| CN106185810A (en) * | 2016-07-27 | 2016-12-07 | 方亚飞 | A kind of joint disposal technique of acidic copper chloride waste etching solution |
| CN106587317A (en) * | 2016-12-30 | 2017-04-26 | 江门市崖门新财富环保工业有限公司 | Concentrated acid fractional distillation treatment process for copper ammonia concentrated liquid of circuit board |
| CN107099802A (en) * | 2017-06-16 | 2017-08-29 | 深圳市新锐思环保科技有限公司 | A kind of novel acid etching solution resource recycling method and recycling system |
| CN107354461A (en) * | 2017-09-13 | 2017-11-17 | 田成 | A kind of printed circuit board acidic etching waste liquor process for regenerating, recovering and reutilizing |
| CN108793095A (en) * | 2018-09-26 | 2018-11-13 | 高频美特利环境科技（北京）有限公司 | Solution impurity-removing method and solution impurity removed system |
| CN111020633A (en) * | 2019-12-23 | 2020-04-17 | 广东臻鼎环境科技有限公司 | Treatment method of acidic etching waste liquid |
| CN113336259A (en) * | 2021-08-06 | 2021-09-03 | 清大国华环境集团股份有限公司 | Method for recycling acidic copper sulfate waste liquid |
| CN114561669A (en) * | 2022-03-03 | 2022-05-31 | 无锡中天固废处置有限公司 | Method for recycling acidic copper-containing ammonium-containing etching waste liquid |
| WO2023165021A1 (en) * | 2022-03-03 | 2023-09-07 | 无锡中天固废处置有限公司 | Method for recycling acidic copper-containing and ammonium-containing waste etching solution |
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Open date: 20100804 |