CN102418099A - Process for recovering copper by processing acidic copper chloride etchant through rotational flow electrolysis - Google Patents
Process for recovering copper by processing acidic copper chloride etchant through rotational flow electrolysis Download PDFInfo
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- CN102418099A CN102418099A CN2011104110952A CN201110411095A CN102418099A CN 102418099 A CN102418099 A CN 102418099A CN 2011104110952 A CN2011104110952 A CN 2011104110952A CN 201110411095 A CN201110411095 A CN 201110411095A CN 102418099 A CN102418099 A CN 102418099A
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Abstract
The invention relates to a process for recovering copper by processing an acidic copper chloride etchant through rotational flow electrolysis, belonging to the technical field of copper-containing waste liquid treatment. The process comprises the following steps of: taking acidic copper chloride etching wastewater as a raw material; obtaining a copper sulfate crystal at a temperature of 120-180 DEG C through using an acid replacement conversion system; dissolving the copper sulfate crystal by diluting with distilled water to obtain a copper sulfate solution; filtering the copper sulfate solution through precise filtering equipment to obtain a filtrate; de-coppering the filtrate through the rotational flow electrolysis; and scalding an obtained copper pipe with little acid. According to the process provided by the invention, a rotational flow electrolytic cell and assorted equipment are convenient to mount, dismount and move through a portable or modular assembly; the solution is circulated in a closed loop without emission of harmful gases; electrolytic deposition is selectively carried out on metal, and the copper can be purified in a better manner by using the rotational flow electrolysis technology; due to higher current density and efficiency, the reagent consumption is reduced, the production cost is reduced and the enterprise benefit is improved; and an effective and highly-pure electroextraction is carried out on the solution, therefore, the recovered copper is standard cathode copper with a total recovery rate of more than 96%.
Description
Technical field
The invention belongs to the contained waste liquid processing technology field, be specifically related to that a kind of flow process is short, cost is low, the eddy flow electrolysis treatment acid chlorization copper etchant solution of high-efficiency environment friendly reclaims process for copper.
Background technology
In recent years, China's electronic industry development is rapid, and the production of PC board has formed industrial scale in China gradually, and in etching process, acidic etching liquid commonly used has CuCl
2Etching solution and FeCl
3Etching solution.Because CuCl
2Etching solution has advantages such as high etching capacity, high etching efficiency, low cost and environmental pollution be less relatively concurrently, is widely used by PCB factory.Therefore, the etching waste liquor that the PC board etching process produces all is a large amount of copper-containing etching waste solution, on average produces spent etching solution daily more than 6000 tons.By 120g/L, can reclaim 600 tons of copper every day from spent etching solution, and the whole nation is annual from 200,000 tons of the recyclable copper of circuit card etching process.The recovery copper method that uses at present is following:
1) traditional electrolysis method of reproduction
Though tradition electrolysis method of reproduction has effectively reclaimed the copper in the acidic copper chloride waste etching solution; But in electrolytic process, can produce a large amount of chlorine; Polluted environment and added that the severe corrosive of chlorine and hypertoxicity have huge harm to human body, so in industry, can't promote the use of.
2) metal replacement method
Be easy to get though the metal replacement method has raw material, also there is insufficient place in simple operation and other advantages, and it is big to be mainly reflected in the metal powder consumption, and cost copper products high and that obtain can only be a copper sponge, and added value is not high.
3) SX electrodeposition method
For the mode of the general slective extraction of solution of most of complicated components with the metals ion that will obtain obtain through the extraction agent extraction.But because the acidity of acidic etching waste liquid is too high; Free acid concentration is at 150-250g/L, so before extraction, will adopt Lix series extraction agent extraction then earlier with sour with part in the alkali; And then use the diluted acid back extraction, also need alkaline matter adjustment acidity during electrolysis.So extraction electrodeposition method, the reagent of consumption is many, and is economical poor.
Summary of the invention
To the problems referred to above that exist in the prior art, the object of the present invention is to provide that a kind of flow process is short, cost is low, the eddy flow electrolysis treatment acid chlorization copper etchant solution of high-efficiency environment friendly reclaims process for copper.
Described eddy flow electrolysis treatment acid chlorization copper etchant solution reclaims process for copper, it is characterized in that may further comprise the steps:
1) the industrial vitriol oil of 96%-98% is poured in the reactor drum; Again with acidic copper chloride waste etching solution pour into separating funnel with 1-3 drip/it is to carry out sour replacement(metathesis)reaction under 120 ℃-180 ℃ that the speed of s slowly is added drop-wise in the reactor drum in temperature of reaction; The volume ratio that feeds intake of the described industrial vitriol oil and acidic copper chloride waste etching solution is 0.1-0.3:1, obtains the solution of sulfur acid copper crystal;
2) adding distil water dilution in the solution of the sulfur acid copper crystal that step 1) obtains, the copper-bath after obtaining diluting, copper ion concentration is 60-80g/L in the solution, chlorine ion concentration is 5-30g/L;
3) with step 2) copper-bath that obtains filters with pumping and filtering device, removes suspended substance, organic matter and particulate contamination, and the filtrating that obtains changes in the circulation groove subsequent use;
4) filtrating that step 3) is obtained flows into from circulation groove as electrolytic solution carries out eddy flow electrolysis decopper(ing) in the eddy flow electrolyzer, obtain negative electrode copper pipe and electrolytic solution, described current density 220-800A/m
2, electrolyte flow rate is 200-600L/h;
5) the negative electrode copper pipe that step 4) is obtained is put into and is scalded board slot, scalds with what contain dilute sulphuric acid that liquid washs, drying treatment, obtains clean negative electrode copper pipe;
6) electrolytic solution behind the step 4) decopper(ing) is back to step 1) as displacement acid, is used for obtaining copper-bath, reuse with the acidic copper chloride waste etching solution reaction.
Described eddy flow electrolysis treatment acid chlorization copper etchant solution reclaims process for copper, it is characterized in that copper ion concentration is 100-130g/L in the described acidic copper chloride waste etching solution of step 1), and chlorine ion concentration is 180-200g/L.
Described eddy flow electrolysis treatment acid chlorization copper etchant solution reclaims process for copper, it is characterized in that the volume ratio of the described industrial vitriol oil of step 1) and acidic copper chloride waste etching solution is 0.2:1.
Described eddy flow electrolysis treatment acid chlorization copper etchant solution reclaims process for copper, it is characterized in that the described pumping and filtering device of step 3) is a blade vacuum filtration pump, described suction filtration speed 0.9-1.1L/s.
Described eddy flow electrolysis treatment acid chlorization copper etchant solution reclaims process for copper, it is characterized in that the described eddy flow electrolyzer of step 4) number is 1-3.
Described eddy flow electrolysis treatment acid chlorization copper etchant solution reclaims process for copper, it is characterized in that the described electrolyte flow rate of step 4) is 220-550L/h;
Described eddy flow electrolysis treatment acid chlorization copper etchant solution reclaims process for copper, it is characterized in that step 5) is described to scald the dilute sulfuric acid solution that liquid is PH 2.0-3.0, and the temperature of scalding board slot is 90-150 ℃, and the time of scalding is 15-20 minute.
Described eddy flow electrolysis treatment acid chlorization copper etchant solution reclaims process for copper; It is characterized in that copper ion concentration is 2-7.5g/L in the electrolytic solution behind the described decopper(ing) of step 6); Return the acid displacement operation of step 1) and use, react with acidic copper chloride waste etching solution as displacement acid.
Described eddy flow electrolysis treatment acid chlorization copper etchant solution reclaims process for copper, it is characterized in that the described electrolyte flow rate of step 4) is 400-500L/h.
Through adopting above-mentioned technology, compared with prior art, beneficial effect of the present invention is following:
1) the present invention uses the industrial vitriol oil and effectively converts the cl ions in the system to HCl, avoids producing a large amount of chlorine, contaminate environment and personnel safety;
2) the eddy flow electrolyzer of the present invention's use is to be assembled through portable or module by eddy flow electrolyzer and support equipment, makes things convenient for installing/dismounting to relocate; And the solution closed cycle, there is not discharge of harmful gases; Optionally metal is carried out electrolytic deposition, use the eddy flow electrolysis tech copper of can better purifying; Higher current density and current efficiency, reagent consumption is few, reduces production costs, and improves the performance of enterprises;
3) the cupric acid solution of the present invention after through eddy flow electrolysis decopper(ing) can turn back to acid displacement operation and use as displacement acid, and raw material consumption is few, has reduced cost;
4) recovery copper method of the present invention, flow process is short, cost is low, high-efficiency environment friendly, and acidic copper chloride waste etching solution is carried out efficient, highly purified electrowinning, and the negative electrode copper pipe purity of recovery is 99.95%, and total yield is more than 96%.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment 1:
96% the industrial vitriol oil of 500ml is poured in the beaker of 5L, and the copper ions concentration with 3L is 100g/L again, and chlorine ion concentration is that the acidic copper chloride waste etching solution of 200g/L is poured separating funnel into and slowly is added drop-wise in the beaker of 5L with the speed of 1/s; In temperature of reaction is to carry out sour replacement(metathesis)reaction under 180 ℃; Obtain the solution of sulfur acid copper crystal, add the distilled water diluting of 1800ml, the copper-bath copper ions concentration after the dilution is 56g/L; Chlorine ion concentration is 20g/L; Remove by filter suspended substance, organic matter and particulate contamination with pumping and filtering device, suction filtration speed is 1.1L/s, and the filtrating electrolytic solution that obtains flows into from circulation groove and carries out eddy flow electrolysis decopper(ing) in the eddy flow electrolyzer; The electrolytic solution volume is 5.2L, current density 1000A/m
2, electrolyte flow rate is 400L/h, electrolysis 5 hours; The negative electrode copper pipe that obtains is put into and is scalded board slot, under 105 ℃ of temperature, scalds liquid with the dilute sulphuric acid of PH 2.0 and washs 20 minutes, drying treatment, obtains clean negative electrode copper pipe 287 grams; The recovery is 96%, purity 99.95%; Copper ion concentration is 4g/L in the electrolytic solution, is back in the beaker of 5L as displacement acid, is used for obtaining copper-bath with the acidic copper chloride waste etching solution reaction, reuses.
Embodiment 2:
98% the industrial vitriol oil of 300ml is poured in the beaker of 5L, and the copper ions concentration with 3L is 130g/L again, and chlorine ion concentration is that the acidic copper chloride waste etching solution of 180g/L is poured separating funnel into and slowly is added drop-wise in the beaker of 5L with the speed of 3/s; In temperature of reaction is to carry out sour replacement(metathesis)reaction under 120 ℃; Obtain the solution of sulfur acid copper crystal, add the distilled water diluting of 1500ml, the copper-bath copper ions concentration after the dilution is 81g/L; Chlorine ion concentration is 30g/L; Remove by filter suspended substance, organic matter and particulate contamination with pumping and filtering device, suction filtration speed is 0.9L/s, and the filtrating electrolytic solution that obtains flows into from circulation groove and carries out eddy flow electrolysis decopper(ing) in the eddy flow electrolyzer; The electrolytic solution volume is 4.8L, current density 800A/m
2, electrolyte flow rate is 550L/h, electrolysis 4 hours; The negative electrode copper pipe that obtains is put into and is scalded board slot, under 115 ℃ of temperature, scalds liquid with the dilute sulphuric acid of PH 3.0 and washs 18 minutes, drying treatment, obtains clean negative electrode copper pipe 355 grams; The recovery is 91%, purity 99.95%; Copper ion concentration is 7.29g/L in the electrolytic solution, is back in the beaker of 5L as displacement acid, is used for obtaining copper-bath with the acidic copper chloride waste etching solution reaction, reuses.
Embodiment 3:
98% the industrial vitriol oil of 900ml is poured in the beaker of 5L, is 120g/L with 3L copper ions concentration again, and chlorine ion concentration is that the acidic copper chloride waste etching solution of 200g/L is poured separating funnel into and slowly is added drop-wise in the beaker of 5L with the speed of 2/s; In temperature of reaction is to carry out sour replacement(metathesis)reaction under 150 ℃; Obtain the solution of sulfur acid copper crystal, add the distilled water diluting of 1500ml, the copper-bath copper ions concentration after the dilution is 66.67g/L; Chlorine ion concentration is 10g/L; Remove by filter suspended substance, organic matter and particulate contamination with pumping and filtering device, suction filtration speed is 1.0L/s, and the filtrating electrolytic solution that obtains flows into from circulation groove and carries out eddy flow electrolysis decopper(ing) in the eddy flow electrolyzer; The electrolytic solution volume is 5.3L, current density 550A/m
2, electrolyte flow rate is 400L/h, electrolysis 3.5 hours; The negative electrode copper pipe that obtains is put into and is scalded board slot, under 90 ℃ of temperature, scalds liquid with the dilute sulphuric acid of PH 2.5 and washs 15 minutes, drying treatment, obtains clean negative electrode copper pipe 320 grams; The recovery is 88.89%, purity 99.95%; Copper ion concentration is 7.4g/L in the electrolytic solution, is back in the beaker of 5L as displacement acid, is used for obtaining copper-bath with the acidic copper chloride waste etching solution reaction, reuses.
Embodiment 4:
98% the industrial vitriol oil of 600ml is poured in the beaker of 5L, is 110g/L with 3L copper ions concentration again, and chlorine ion concentration is that the acidic copper chloride waste etching solution of 170g/L is poured separating funnel into and slowly is added drop-wise in the beaker of 5L with the speed of 2/s; In temperature of reaction is to carry out sour replacement(metathesis)reaction under 150 ℃; Obtain the solution of sulfur acid copper crystal, add the distilled water diluting of 1500ml, the copper-bath copper ions concentration after the dilution is 64.7g/L; Chlorine ion concentration is 18g/L; Remove by filter suspended substance, organic matter and particulate contamination with pumping and filtering device, suction filtration speed is 1.0L/s, and the filtrating electrolytic solution that obtains flows into from circulation groove and carries out eddy flow electrolysis decopper(ing) in the eddy flow electrolyzer; The electrolytic solution volume is 5L, current density 550A/m
2, electrolyte flow rate is 400L/h, electrolysis 3.5 hours; The negative electrode copper pipe that obtains is put into and is scalded board slot, under 150 ℃ of temperature, scalds liquid with the dilute sulphuric acid of PH 3.0 and washs 18 minutes, drying treatment, obtains clean negative electrode copper pipe 350 grams; The recovery is 97.1%, purity 99.95%; Copper ion concentration is 2g/L in the electrolytic solution, is back in the beaker of 5L as displacement acid, is used for obtaining copper-bath with the acidic copper chloride waste etching solution reaction, reuses.
Embodiment 5:
98% the industrial vitriol oil of 800ml is poured in the beaker of 5L, and again with the copper ions 120g/L of 3L, the acidic copper chloride waste etching solution of cl ions 190g/L is poured separating funnel into and slowly is added drop-wise in the beaker of 5L with the speed of 2/s; In temperature of reaction is to carry out sour replacement(metathesis)reaction under 160 ℃; Obtain the solution of sulfur acid copper crystal, add the distilled water diluting of 1500ml, the copper-bath copper ions concentration after the dilution is 67.9g/L; Chlorine ion concentration is 10g/L; Remove by filter suspended substance, organic matter and particulate contamination with pumping and filtering device, suction filtration speed is 1.0L/s, and the filtrating electrolytic solution that obtains flows into from circulation groove and carries out eddy flow electrolysis decopper(ing) in the eddy flow electrolyzer; The electrolytic solution volume is 5.2L, current density 800A/m
2, electrolyte flow rate is 500L/h, electrolysis 4 hours; The negative electrode copper pipe that obtains is put into and is scalded board slot, under 110 ℃ of temperature, scalds liquid with the dilute sulphuric acid of PH 3.0 and washs 16 minutes, drying treatment, obtains clean negative electrode copper pipe 340 grams; The recovery is 94.4%, purity 99.95%; Copper ion concentration is 4g/L in the electrolytic solution, is back in the beaker of 5L as displacement acid, is used for obtaining copper-bath with the acidic copper chloride waste etching solution reaction, reuses.
Claims (9)
1. eddy flow electrolysis treatment acid chlorization copper etchant solution reclaims process for copper, it is characterized in that may further comprise the steps:
1) the industrial vitriol oil of 96%-98% is poured in the reactor drum; Again with acidic copper chloride waste etching solution pour into separating funnel with 1-3 drip/it is to carry out sour replacement(metathesis)reaction under 120 ℃-180 ℃ that the speed of s slowly is added drop-wise in the reactor drum in temperature of reaction; The volume ratio that feeds intake of the described industrial vitriol oil and acidic copper chloride waste etching solution is 0.1-0.3:1, obtains the solution of sulfur acid copper crystal;
2) adding distil water dilution in the solution of the sulfur acid copper crystal that step 1) obtains, the copper-bath after obtaining diluting, copper ion concentration is 60-80g/L in the solution, chlorine ion concentration is 5-30g/L;
3) with step 2) copper-bath that obtains filters with pumping and filtering device, removes suspended substance, organic matter and particulate contamination, and the filtrating that obtains changes in the circulation groove subsequent use;
4) filtrating that step 3) is obtained flows into from circulation groove as electrolytic solution carries out eddy flow electrolysis decopper(ing) in the eddy flow electrolyzer, obtain negative electrode copper pipe and electrolytic solution, described current density 220-800A/m
2, electrolyte flow rate is 200-600L/h;
5) the negative electrode copper pipe that step 4) is obtained is put into and is scalded board slot, scalds with what contain dilute sulphuric acid that liquid washs, drying treatment, obtains clean negative electrode copper pipe;
6) electrolytic solution behind the step 4) decopper(ing) is back to step 1) as displacement acid, is used for obtaining copper-bath, reuse with the acidic copper chloride waste etching solution reaction.
2. eddy flow electrolysis treatment acid chlorization copper etchant solution according to claim 1 reclaims process for copper, it is characterized in that copper ion concentration is 100-130g/L in the described acidic copper chloride waste etching solution of step 1), and chlorine ion concentration is 180-200g/L.
3. eddy flow electrolysis treatment acid chlorization copper etchant solution according to claim 1 reclaims process for copper, it is characterized in that the volume ratio of the described industrial vitriol oil of step 1) and acidic copper chloride waste etching solution is 0.2:1.
4. eddy flow electrolysis treatment acid chlorization copper etchant solution according to claim 1 reclaims process for copper, it is characterized in that the described pumping and filtering device of step 3) is a blade vacuum filtration pump, described suction filtration speed 0.9-1.1L/s.
5. eddy flow electrolysis treatment acid chlorization copper etchant solution according to claim 1 reclaims process for copper, it is characterized in that the described eddy flow electrolyzer of step 4) number is 1-3.
6. eddy flow electrolysis treatment acid chlorization copper etchant solution according to claim 1 reclaims process for copper, it is characterized in that the described electrolyte flow rate of step 4) is 220-550L/h.
7. eddy flow electrolysis treatment acid chlorization copper etchant solution according to claim 1 reclaims process for copper, it is characterized in that step 5) is described to scald the dilute sulfuric acid solution that liquid is PH 2.0-3.0, and temperature 90-150 ℃ of scalding board slot, the time of scalding is 15-20 minute.
8. eddy flow electrolysis treatment acid chlorization copper etchant solution according to claim 1 reclaims process for copper; It is characterized in that copper ion concentration is 2-7.5g/L in the electrolytic solution behind the described decopper(ing) of step 6); Return the acid displacement operation of step 1) and use, react with acidic copper chloride waste etching solution as displacement acid.
9. eddy flow electrolysis treatment acid chlorization copper etchant solution according to claim 1 reclaims process for copper, it is characterized in that the described electrolyte flow rate of step 4) is 400-500L/h.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102808194A (en) * | 2012-07-04 | 2012-12-05 | 嘉兴科菲冶金科技股份有限公司 | Process for purifying cobalt by electro-depositing cobalt chloride solution through cyclone electrolysis technology and reclaiming residual chlorine |
| CN103693672A (en) * | 2013-12-25 | 2014-04-02 | 广州科城环保科技有限公司 | Method for preparing electroplating grade copper sulfate pentahydrate by copper-bearing acid waste liquid without containing ammonia nitrogen |
| CN104611703A (en) * | 2014-12-26 | 2015-05-13 | 锦州清源嘉华环保科技有限公司 | Device and method for regenerating PCB etching waste liquid and recycling heavy metal |
| CN105442032A (en) * | 2014-09-25 | 2016-03-30 | 深圳市洁驰科技有限公司 | Copper-containing nitric acid stripping hanging liquid regeneration treatment method |
| CN106011949A (en) * | 2016-08-01 | 2016-10-12 | 舒城联科表面处理有限公司 | Current density parameter gradient control method during copper cyclone electrolysis |
| CN106319564A (en) * | 2016-09-13 | 2017-01-11 | 广沣金源（北京）科技有限公司 | Metallic copper, method for treating wastewater containing copper ions and method for electrolyzing metal ions |
| CN108914128A (en) * | 2018-07-09 | 2018-11-30 | 南京舜业环保科技有限公司 | A kind of the regeneration cycle system and method for recycling of sulfuric acid copper etchant solution |
| CN109853002A (en) * | 2019-03-30 | 2019-06-07 | 深圳市泰兴和环保实业有限公司 | A kind of swirl electrolysis device |
| CN113088722A (en) * | 2021-03-17 | 2021-07-09 | 磨名言 | Method for electrolytically recovering copper from copper sulfide ore |
| CN114892221A (en) * | 2022-05-09 | 2022-08-12 | 惠州市华盈科技有限公司 | Cyclone electrolysis method for manufacturing cathode copper sheet |
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Cited By (12)
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| CN102808194A (en) * | 2012-07-04 | 2012-12-05 | 嘉兴科菲冶金科技股份有限公司 | Process for purifying cobalt by electro-depositing cobalt chloride solution through cyclone electrolysis technology and reclaiming residual chlorine |
| CN102808194B (en) * | 2012-07-04 | 2015-04-29 | 浙江科菲科技股份有限公司 | Process for purifying cobalt by electro-depositing cobalt chloride solution through cyclone electrolysis technology and reclaiming residual chlorine |
| CN103693672A (en) * | 2013-12-25 | 2014-04-02 | 广州科城环保科技有限公司 | Method for preparing electroplating grade copper sulfate pentahydrate by copper-bearing acid waste liquid without containing ammonia nitrogen |
| CN103693672B (en) * | 2013-12-25 | 2015-08-26 | 广州科城环保科技有限公司 | A kind of cupric acid waste liquid not containing ammonia nitrogen prepares the method for plating level cupric sulfate pentahydrate |
| CN105442032A (en) * | 2014-09-25 | 2016-03-30 | 深圳市洁驰科技有限公司 | Copper-containing nitric acid stripping hanging liquid regeneration treatment method |
| CN104611703A (en) * | 2014-12-26 | 2015-05-13 | 锦州清源嘉华环保科技有限公司 | Device and method for regenerating PCB etching waste liquid and recycling heavy metal |
| CN106011949A (en) * | 2016-08-01 | 2016-10-12 | 舒城联科表面处理有限公司 | Current density parameter gradient control method during copper cyclone electrolysis |
| CN106319564A (en) * | 2016-09-13 | 2017-01-11 | 广沣金源（北京）科技有限公司 | Metallic copper, method for treating wastewater containing copper ions and method for electrolyzing metal ions |
| CN108914128A (en) * | 2018-07-09 | 2018-11-30 | 南京舜业环保科技有限公司 | A kind of the regeneration cycle system and method for recycling of sulfuric acid copper etchant solution |
| CN109853002A (en) * | 2019-03-30 | 2019-06-07 | 深圳市泰兴和环保实业有限公司 | A kind of swirl electrolysis device |
| CN113088722A (en) * | 2021-03-17 | 2021-07-09 | 磨名言 | Method for electrolytically recovering copper from copper sulfide ore |
| CN114892221A (en) * | 2022-05-09 | 2022-08-12 | 惠州市华盈科技有限公司 | Cyclone electrolysis method for manufacturing cathode copper sheet |
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