CN103966607A - Method for recovering copper and hydrochloric acid from acid etching solution - Google Patents
Method for recovering copper and hydrochloric acid from acid etching solution Download PDFInfo
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- CN103966607A CN103966607A CN201310038564.XA CN201310038564A CN103966607A CN 103966607 A CN103966607 A CN 103966607A CN 201310038564 A CN201310038564 A CN 201310038564A CN 103966607 A CN103966607 A CN 103966607A
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- Prior art keywords
- copper
- hydrochloric acid
- etching liquid
- acidic etching
- water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
A purpose of the present invention is to provide a method for recovering copper and hydrochloric acid from a treatment acid etching solution, wherein the method has characteristics of high comprehensive resource utilization rate, environmental protection and high economic benefits. The method is characterized in that heating distillation is performed on an acid etching solution to recover hydrochloric acid and the heating distillation residue of the acid etching solution is subjected to neutralization and copper precipitation to recover electrolytic copper, and the method comprises processes of boiling volatilization to recover hydrochloric acid, neutralization and copper precipitation, washing and chlorine removing, filtrate crystallization and sodium chloride recovery, filter residue dissolving, and dissolving solution electrowinning. According to the present invention, the hydrochloric acid in the etching solution can be effectively recovered, the electrolytic copper with the content of more than 99.95% is obtained, the comprehensive recovery utilization of the solution is efficiently increased, and high economic benefits are obtained; and the salt-containing wastewater produced during the whole process can be reasonably treated to obtain the sodium chloride crystal salt so as to increase the value utilization and provide good ecological benefits.
Description
Technical field
The invention belongs to the technical field that reclaims useful resources from industrial effluent, relate to a kind of method that reclaims copper and dilute hydrochloric acid from acidic etching liquid.
Background technology
In recent years, along with the steady growth of electronic industry, China's printed circuit board (PCB) fast development, to produce every year a large amount of acidic etching liquids, in this liquid, contain a large amount of acid and copper, if effectively do not processed, will environment be caused and be had a strong impact on, process this kind of waste liquid, the valuable resource of efficient recovery the inside has good economic worth, ecological benefits and social benefit.
At present, processing in the application of acidic etching liquid, be to be generally made into copper sulfate or copper sponge by reaction, do not adopt the application of similar flow processing scheme.
There were a lot of methods etching solution recycling aspect in the past.The first be in acidic etching liquid, add in alkaline matter and etching solution in acid, and then generate copper sulfate by reaction, the operation process of this method is complexity comparatively, economic benefit is poor; The second is in acidic etching liquid, to add in cupric oxide and the acid of the inside, then generate copper sulfate by reaction, but the price of cupric oxide is higher, and this method economic benefit is lower; The third method is to add alkaline matter, in and acid in etching solution, then adopt reductibility higher, the lower metal of price is replaced, and obtains copper sponge, and this method can make metal ion water solution-treated become difficulty, obtaining copper sponge also needs to be further processed, and economic benefit is lower.
Can find out that by above analysis the method for current processing acidic etching liquid exists following shortcoming: 1, need the alkali number of consumption too high, process sour cost higher; 2, the hydrochloric acid in acidic etching liquid is not comprehensively reclaimed; 3, processing rear liquid also needs to process, otherwise can pollute; 4, metallic copper can not reach the recovery of largeizationr of value.
Summary of the invention
The object of the invention is the deficiency existing for above-mentioned prior art, provide one can make comprehensive utilization of resources rate high, environmental friendliness, reclaims the method for copper and dilute hydrochloric acid in the high processing acidic etching liquid of economic benefit.
To achieve these goals, the technical solution used in the present invention is:
A method that reclaims copper and dilute hydrochloric acid from acidic etching liquid, is characterized in that, adds thermal distillation acidic etching liquid and reclaims the heating distillation residue of hydrochloric acid and the heavy copper acidic etching liquid of neutralization and reclaim electrolytic copper.
Further, specifically comprise the following steps:
(1) reclaim hydrochloric acid;
Acidic etching liquid is added in corrosion-resistant water distilling apparatus, be heated to boiling state, distill off-gas recovery hydrochloric acid by recovery;
(2) reclaim electrolytic copper;
(2.1) distillation residue of acidic etching liquid are dissolved in water, the cupric chloride in residue is fully dissolved, add sodium carbonate neutralization solution acidity;
(2.2) in (2.1) neutralizer, add sodium carbonate or sodium hydroxide, adjust pH, make the copper in solution generate cupric oxide or basic copper;
(2.3) after liquid-solid separation, obtain copper oxide mud or basic copper mud and brackish water, oxidation copper ashes mud or basic copper slag mud are added to washing water and carry out three countercurrent washings, after washing finishes, ore pulp is carried out to press filtration, filtrate is washing water, and filter residue is washing copper oxide mud;
(2.4) brackish water is added in crystallization axe, pass into steam and distill crystallization, the cooling rear recovery water of condensation of steam to acidic etching liquid distillation residue dissolve water, crystallization residue is entered to strumbox and filter, and filter residue carries out sodium-chlor recovery;
(2.5) add electrolysis cycle liquid, copper sulfate to dissolve three washing copper oxide muds, obtain copper-bath; Copper-bath is sent into and in electrolyzer, carried out electrolysis, output cathode copper.
Preferably, step (1) joins acidic etching liquid in corrosion-resistant distillation plant and distills, and volatilization flue gas is dilute hydrochloric acid after condensation absorbs.
Further, acidic etching liquid volatilization process temperature need to be more than 108 DEG C, in volatilization hydrochloric acid process, will stir slowly, prevent that the dense cupric chloride that melts from splashing.
Preferably, step (2.2) is precipitated out the cupric ion in solution by the mode of adding calcium carbonate or sodium hydroxide.
Preferably, step (2.3) can be cleaned the sodium-chlor being mingled with in copper sludge to remove by repeatedly being washed.
Preferably, step (2.4) concentrates by volume the sodium-chlor crystallization making in hydrochloric acid and washes out.
Preferably, step (2.5) is dissolved copper sludge slag by adding electrolysis cycle liquid and suitable sulfuric acid.
Compared with prior art, the invention has the beneficial effects as follows:
1, can reclaim the hydrochloric acid in acidic etching liquid;
2, effectively reduce the alkali consumption of acidic etching liquid N-process;
3, can comprehensively reclaim the salt in the waste water of output in operation process, avoid environmental pollution;
4, can obtain 99.95% electrolytic copper, economic worth is high;
5, reduce the consumption of water resources, improve the utilization ratio of water resources.
Brief description of the drawings
Fig. 1 is production technological process of the present invention.
Embodiment
In order to further illustrate the present invention, describe below in conjunction with embodiment and accompanying drawing:
1, reclaim hydrochloric acid
Acidic etching liquid is added in corrosion-resistant water distilling apparatus, be heated to boiling state, distill off-gas recovery hydrochloric acid by recovery.
Hydrochloric acid is colourless liquid, be corrosive, for the aqueous solution of hydrogenchloride, concentrated hydrochloric acid has volatility, in acidic etching liquid, concentration of hydrochloric acid is generally 20% left and right, and its volatilization temperature is 108 DEG C, and heating acidic etching liquid is to boiling state, HCl in solution evaporates together with steam, condenses into dilute hydrochloric acid by HCl after condensation together with water vapour.
2, neutralization oxidation
The distillation residue of acidic etching liquid are dissolved in water, the cupric chloride in residue is fully dissolved, add sodium carbonate neutralization solution acidity.
In neutralizer, add sodium hydroxide and sodium carbonate, adjust pH, make the copper in solution generate cupric oxide.
Neutralization precipitation cupric oxide reaction equation is as follows:
Na
2CO
3+2HCl＝2NaCl+2CO
2↑+H
2O………①
CuCl
2+2NaOH＝CuO+2NaCl+H
2O………②
Ore pulp after oxidation is carried out to press filtration, and filtrate is brackish water, and filter residue is oxidation copper ashes mud.
Neutralization precipitation basic copper reaction equation is as follows:
NaOH+HCl＝NaCl+H
2O………③
2Cu
2++CO
3 2-+2OH
-+nH
2O＝CuCO
3·Cu(OH)
2·nH
2O…·④
3, washing dechlorination
Oxidation copper ashes mud is added to second wash water and carry out pulping and washing one time, after washing finishes, ore pulp is carried out to press filtration, filtrate is once washing water, and filter residue is once washing copper oxide mud.The control of pulping and washing liquid-solid ratio is 3～6: 1.
Once washing copper oxide mud is added to three washing water and carry out secondary pulping and washing, after washing finishes, ore pulp is carried out to press filtration, filter residue is secondary washing copper oxide mud, and filtrate is second wash water.The control of pulping and washing liquid-solid ratio is 3～6: 1.
Add production water to carry out pulping and washing three times secondary washing copper oxide mud, after washing finishes, ore pulp is carried out to press filtration, filter residue is three washing copper oxide muds, and filtrate is three washing water.The control of pulping and washing liquid-solid ratio is 3～6: 1.
Its principle is: sodium-chlor (NaCl) is colourless cube of crystallization or white crystals.Water-soluble, the lower every 100g water soluble of normal temperature (25 DEG C) 36.2g that terminates an agreement.Cupric oxide (CuO) is a kind of black oxide of copper, and slightly water absorbability is water insoluble.Ventilation breather chemical formula is CuCO
3cu (OH)
2nH
2o, (main component is Cu
2(OH)
2cO
3, non-pure substance), belong to subcarbonate, be the one of salt, water insoluble.Washing process utilizes cupric oxide, and the solvability in water is different from sodium-chlor with basic copper, washing dechlorination.
4, brackish water crystallization
Brackish water is added in crystallization axe, pass into steam and distill crystallization, the cooling rear recovery water of condensation of steam to acidic etching liquid distillation residue dissolve water.
Crystallization residue is entered to strumbox and filter, filter residue carries out sodium-chlor recovery.
5, copper sludge dissolves
Add electrodeposition circulation fluid, sulfuric acid to dissolve three washing copper oxide muds, obtain copper-bath.
Reaction equation is as follows:
CuO+H
2SO
4＝CuSO
4+H
2O………⑤
CuCO
3·Cu(OH)
2·nH
2O+2H
2SO
4＝2CuSO
4+CO
2+(3+n)H
2O…⑥
6, copper sulfate electrodeposition
Copper-bath is sent into and in electrolyzer, carried out electrodeposition, output cathode copper.
Electrolytic deposition process, using stainless steel as negative electrode, using anticorrosion titanium material as anode, passes into direct current and copper-bath, separates out cathode copper, precipitated oxygen on anode on negative electrode.
Reaction equation is as follows:
Cathodic reaction: Cu
2++ 2e
-=Cu ... 7.
Anodic reaction: H
2o+2e
-=1/2O
2+ 2H
+8.
In such scheme, acidic etching liquid need can volatilize in a large number below boiling state, and heating medium can be steam, power supply, burning things which may cause a fire disaster.In reaction process, along with acidic etching liquid volume reduces, the etching solution in reactor becomes thickness gradually, and whipping appts need be installed in reactor.
In such scheme, after boiling volatilization finishes, need add water residue is dissolved, for carrying out lower step operation, the add-on of water is equal to the add-on of the acidic etching liquid of boiling volatilization, and suitably heating for dissolving temperature to 40～50 DEG C, dissolve rapidly residue.
In such scheme, Na
2cO
3there are two kinds with the mode that adds of NaOH, first, first add sodium carbonate neutralization solution acidity, then adjust solution temperature more than 80 DEG C, (according to equipment anticorrosion layer Temperature Setting upper temperature limit) adds NaOH to adjust solution endpoint pH is again 10～11, and the copper in solution is precipitated with the form of cupric oxide; While utilizing sodium carbonate neutralization solution acidity, the CO in soda ash
3 -have CO with the acid-respons in solution
2generate, the acidity of etching solution is higher, needs the soda ash amount of consumption larger, the CO of output
2also more, bubble lies prostrate on liquid level, causes reaction difficulty, now can be by adding NaOH to adjust pH.NaCO
3with the add-on of NaOH be that 1～1.1 times of Theoretical Calculation amount adds.The second, add NaOH neutralization solution acidity, and then add Na
2cO
3the terminal pH that adjusts solution is 6.5～7.5, and temperature of reaction control is below 75 DEG C, and the copper in solution is precipitated with the form of ventilation breather.NaCO
3the mole number of add-on be equal to the mole number of copper content in solution.
In such scheme, the heavy copper filtered liquid of neutralization can be by carrying out filtered and recycled sodium-chlor wherein to crystallization slag after volatilization crystallization.
In such scheme, heavy copper ashes dechlorination need, after 3 washings, can be carried out slag and dissolve operation, in actual production, can determine slag washing times by detecting chloride ion content in washed-residue, if chloride ion content, lower than 0.2%, can no longer wash, otherwise also need washing.Be CuO mutually if sink to the bottom slag thing,, wash temperature can be more than 35 DEG C, if precipitation slag thing is basic copper mutually, wash temperature need be controlled at below 35 DEG C.
In such scheme, be further saving water resource, three wash waters are returned to secondary washing use, secondary wash water is back to once washing and uses.
Slag after having washed in such scheme adds electrolysis cycle liquid to dissolve, and is added to sulfuric acid according to the output quantity of slag and slag thing.Output slag thing is the CuO add-on of electrolysis waste solution=(1.35～1.5) × m (CuO) ÷ C (electrolyte acidity) mutually. can be by reducing electrolytic solution add-on, and add the mode of the vitriol oil and add the required sulfuric acid of reaction.
The hydrochloric acid of the present invention in can efficient recovery etching solution, obtaining content is more than 99.95% electrolytic copper, has effectively improved the comprehensive reutilization of solution, obtains high economic benefit; In whole process, the brine waste of output also can rationally be processed and obtain sodium-chlor crystal salt, improves to be worth and utilizes, and has good ecological benefits.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (8)
1. a method that reclaims copper and dilute hydrochloric acid from acidic etching liquid, is characterized in that, adds thermal distillation acidic etching liquid and reclaims the heating distillation residue of hydrochloric acid and the heavy copper acidic etching liquid of neutralization and reclaim electrolytic copper.
2. a kind of method that reclaims copper and dilute hydrochloric acid from acidic etching liquid as claimed in claim 1, is characterized in that, specifically comprises the following steps:
(1) reclaim hydrochloric acid;
Acidic etching liquid is added in corrosion-resistant water distilling apparatus, be heated to boiling state, distill off-gas recovery hydrochloric acid by recovery;
(2) reclaim electrolytic copper;
(2.1) distillation residue of acidic etching liquid are dissolved in water, the cupric chloride in residue is fully dissolved, add sodium carbonate neutralization solution acidity;
(2.2) in (2.1) neutralizer, add sodium carbonate or sodium hydroxide, adjust pH, make the copper in solution generate cupric oxide or basic copper;
(2.3) after liquid-solid separation, obtain copper oxide mud or basic copper mud and brackish water, oxidation copper ashes mud or basic copper slag mud are added to washing water and carry out three countercurrent washings, after washing finishes, ore pulp is carried out to press filtration, filtrate is washing water, and filter residue is washing copper oxide mud;
(2.4) brackish water is added in crystallization axe, pass into steam and distill crystallization, the cooling rear recovery water of condensation of steam to acidic etching liquid distillation residue dissolve water, crystallization residue is entered to strumbox and filter, and filter residue carries out sodium-chlor recovery;
(2.5) add electrolysis cycle liquid, copper sulfate to dissolve three washing copper oxide muds, obtain copper-bath; Copper-bath is sent into and in electrolyzer, carried out electrolysis, output cathode copper.
3. a kind of method that reclaims copper and dilute hydrochloric acid from acidic etching liquid as claimed in claim 2, it is characterized in that, step (1) joins acidic etching liquid in corrosion-resistant distillation plant and distills, and volatilization flue gas is dilute hydrochloric acid after condensation absorbs.
4. a kind of method that reclaims copper and dilute hydrochloric acid from acidic etching liquid as claimed in claim 3, it is characterized in that, acidic etching liquid volatilization process temperature need to be more than 108 DEG C, in volatilization hydrochloric acid process, will stir slowly, prevent that the dense cupric chloride that melts from splashing.
5. a kind of method that reclaims copper and dilute hydrochloric acid from acidic etching liquid as claimed in claim 2, is characterized in that, step (2.2) is precipitated out the cupric ion in solution by the mode of adding calcium carbonate or sodium hydroxide.
6. a kind of method that reclaims copper and dilute hydrochloric acid from acidic etching liquid as claimed in claim 2, is characterized in that, step (2.3) can be cleaned the sodium-chlor being mingled with in copper sludge to remove by repeatedly being washed.
7. a kind of method that reclaims copper and dilute hydrochloric acid from acidic etching liquid as claimed in claim 2, is characterized in that, step (2.4) concentrates by volume the sodium-chlor crystallization making in hydrochloric acid and washes out.
8. a kind of method that reclaims copper and dilute hydrochloric acid from acidic etching liquid as claimed in claim 2, is characterized in that, step (2.5) is dissolved copper sludge slag by adding electrolysis cycle liquid and suitable sulfuric acid.
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|---|---|---|---|
| CN201310038564.XA CN103966607A (en) | 2013-01-31 | 2013-01-31 | Method for recovering copper and hydrochloric acid from acid etching solution |
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|---|---|---|---|
| CN201310038564.XA CN103966607A (en) | 2013-01-31 | 2013-01-31 | Method for recovering copper and hydrochloric acid from acid etching solution |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106086403A (en) * | 2016-08-09 | 2016-11-09 | 成都虹华环保科技股份有限公司 | A kind of hydrometallurgy industry equipment for separating liquid from solid |
| CN106167250A (en) * | 2016-07-07 | 2016-11-30 | 中南大学 | A kind of acid CuCl2etching solution method of comprehensive utilization |
| CN106282567A (en) * | 2015-05-29 | 2017-01-04 | 陕西瑞凯环保科技有限公司 | A kind of method reclaiming metal from useless acidic etching liquid |
| CN106587105A (en) * | 2016-12-15 | 2017-04-26 | 明高电路版（赣州）有限公司 | Method for recovering copper chloride acid etching liquid in printed circuit board |
| 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 |
| CN107385445A (en) * | 2017-07-27 | 2017-11-24 | 四会富士电子科技有限公司 | A kind of method that circuitboard etching waste liquid recycles |
| CN108249670A (en) * | 2018-01-16 | 2018-07-06 | 张家港市佰坤物资有限公司 | A kind of acid etching liquid treatment acid solution and the technique for recycling copper |
| 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 |
| CN111101157A (en) * | 2019-12-27 | 2020-05-05 | 合肥恒力装备有限公司 | Zero-emission treatment process for PCB etching waste liquid |
| CN112093813A (en) * | 2020-08-11 | 2020-12-18 | 吉安共创机电工程有限公司 | System and method for treating high ammonia nitrogen acidic etching waste liquid |
| CN113373479A (en) * | 2021-06-09 | 2021-09-10 | 深圳市瑞盛环保科技有限公司 | Process for treating acid liquor and recovering copper by using acidic etching liquid |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106282567A (en) * | 2015-05-29 | 2017-01-04 | 陕西瑞凯环保科技有限公司 | A kind of method reclaiming metal from useless acidic etching liquid |
| CN106167250A (en) * | 2016-07-07 | 2016-11-30 | 中南大学 | A kind of acid CuCl2etching solution method of comprehensive utilization |
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| CN107385445A (en) * | 2017-07-27 | 2017-11-24 | 四会富士电子科技有限公司 | A kind of method that circuitboard etching waste liquid recycles |
| 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 |
| CN108249670A (en) * | 2018-01-16 | 2018-07-06 | 张家港市佰坤物资有限公司 | A kind of acid etching liquid treatment acid solution and the technique for recycling copper |
| 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 |
| CN111101157A (en) * | 2019-12-27 | 2020-05-05 | 合肥恒力装备有限公司 | Zero-emission treatment process for PCB etching waste liquid |
| CN112093813A (en) * | 2020-08-11 | 2020-12-18 | 吉安共创机电工程有限公司 | System and method for treating high ammonia nitrogen acidic etching waste liquid |
| CN112093813B (en) * | 2020-08-11 | 2023-05-02 | 吉安共创机电工程有限公司 | System and method for treating high ammonia nitrogen acid etching waste liquid |
| CN113373479A (en) * | 2021-06-09 | 2021-09-10 | 深圳市瑞盛环保科技有限公司 | Process for treating acid liquor and recovering copper by using acidic etching liquid |
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