CN102303917B - Method for mixed treatment of waste liquid from acid etching and micro etching of printed circuit boards - Google Patents
Method for mixed treatment of waste liquid from acid etching and micro etching of printed circuit boards Download PDFInfo
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- CN102303917B CN102303917B CN201110244786.8A CN201110244786A CN102303917B CN 102303917 B CN102303917 B CN 102303917B CN 201110244786 A CN201110244786 A CN 201110244786A CN 102303917 B CN102303917 B CN 102303917B
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Abstract
The invention provides a method for the mixed treatment of waste liquid from acid etching and micro etching of printed circuit boards, which comprises the following steps of: 1, adding 40-50-mass/volume-percent sodium hydroxide solution serving as an auxiliary material into waste liquid to be treated from acid etching in a reaction kettle, keeping the PH value between 8.0 and 10.0, uniformly stirring, discharging into a solid-liquid separation press filter system after the reaction is finished completely and obtaining copper oxide; 2, dissolving the prepared copper oxide into micro etching waste liquid to be treated to obtain copper-containing copper sulfate electrolyte; and 3, electrolyzing copper-containing copper sulfate electrolyte and producing high-purity metal copper. When the method for the mixed treatment of waste liquid from acid etching and micro etching of printed circuit boards is used, the copper content in the treated waste water reaches a standard and the waste water can be discharged; and the purity of the produced metal copper product is over 99.5 percent. Thus, the method can create obvious economic and social benefit.
Description
[technical field]
The present invention relates to print the manufacturing technology field, especially relate to a kind of acidic etching waste solution of printed circuit board and micro-etched waste liquid mixed processing method.
[background technology]
In recent years along with the fast development of electron trade, keep the annual growth rate of 10-20% as electronic industry basic link-printed electronic circuit board industry always, current domestic family more than 3500 of printed circuit board manufacturing enterprise that multiple scale is arranged, monthly output reaches 1.2 hundred million square metres.
In the manufacturing processed of printed circuit board, need to consume a large amount of smart copper, domestic printed circuit board manufacturing enterprise essence copper consumption is more than 60,000 tons/month according to statistics, in the copper waste etching solution of output, total copper amount is more than 50,000 tons/month, and copper is a kind of heavy metal element be present in soil and people's carcass, in soil, content is generally in about 0.2ppm, excessive copper can with people's carcass in precipitate/complex reaction of enzyme, generation poisoning by enzyme and lose physiological function.The copper of occurring in nature is transferred in people's carcass by water body, plant etc., if intake is too high, will the Equilibrium of Trace Elements in people's carcass be destroyed, and causes heavy metal undesired accumulation in vivo, produces the results such as sex change, carinogenicity of causing a disease.Like this, a large amount of copper waste etching solutions that produce in the manufacturing processed of printed circuit board, as effectively processed not in time, can cause severe contamination hidden danger to water resources and the soil of environment especially printed circuit board factory surrounding area undoubtedly.
In the industrial wastewater discharge standard of China, the monitor control index of copper is 0.5ppm, and drinking water standard is 0.03ppm, and American-European relevant criterion is severeer.In copper scrap etching solution due to printed circuit board processing generation, copper content is tens supreme hundred grams per liters, and therefore, State Environmental Protection Administration orientates printed circuit board copper scrap etching solution (useless copper etching liquor) as the dangerous liquid refuse, regulation is processed on the spot, forbids transboundary movement.
The recovery copper of acidic etching waste liquid has following several method:
1, substitution method: this method is generally with acidic etching liquid and a small amount of alkaline etching liquid or ammonia neutralization, acidity in acidic etching liquid is reduced, then drop into wherein industrial iron plate, utilize the activity of iron that copper is cemented out, this method is understood heat release and is produced a large amount of water vapour, chlorine and hydrogen chloride gas in the production reaction process, must discharge a large amount of waste water after having replaced, contain a large amount of Cl-, ammonia nitrogen and Fe3+ in the waste water of its discharge, not only in contaminate environment but also etching solution, active princlple can't regeneration.
2. membrane electrolysis: this method is to adopt the anode with anti-active Cl-to carry out diaphragm electrolysis to acidic etching waste liquid, but because Cl-is higher, the electrolytic metal copper produced after electrolysis is powdery, electrolysis is easily to produce a large amount of chlorine and hydrogen, dangerous high, and anode and ionic membrane consumption are very fast, and the production run cost is high.Adopt electrolysis with ion-exchange film to carry out the method for copper waste etching solution recycling utilization, often due to the high requirement of ionic membrane to environment for use, along with the carrying out of process, worsen, cause film properties unstable, the cathode-anode plate interpole gap is little simultaneously, current density is more than 600A/ square metre, negative plate surface easily long fastener is stabbed ionic membrane that anode and cathode liquid is altered is logical, cause systemic breakdown, produce extremely unstable, ionic membrane expensive (every square metre Renminbi 8000～15000 yuan) work-ing life short (average out to half a year) simultaneously, the existence of chlorion and some metal ion during electrolysis, produce and have unavoidably chlorine to produce, and the copper powdering of output, the easy oxidation purity of product copper-base is low, value is lower than 30% of standard electrolytic copper.Power consumption is also often because ionic membrane is former thereby higher than more than three times of standard electrolytic copper, therefore its industrial applications exists certain economy, environmental protection and technical difficulty to the accumulation existence of some metal ion in the resistance of copper ion migration, electrolytic solution etc.After waste liquid enters electrolytic tank electrolysis, remaining liquid can not need efflux in reuse, has caused the wasting of resources to bring pressure to environmental protection.
2, sulfuric acid distillation electrodeposition method: this method is in acidic etching liquid, to add sulfuric acid to carry out underpressure distillation, utilize sulfuric acid fractionation by distillation different from volatility the boiling point of hydrochloric acid reclaim HCl and produce copper sulfate, this method need add a large amount of sulfuric acid that cupric chloride is replaced as to copper sulfate, and cupric chloride can not be replaced as copper sulfate by sulfuric acid fully, produce chlorine while causing electrolysis, complex manufacturing is dangerous high.
3, straight run distillation extraction process: this method is at first to utilize underpressure distillation, and the HCl in acidic etching liquid is separated, and still residue reclaims metallic copper by the method for solution extraction-electrodeposition.But, because straight run distillation separates the HCl weak effect, the still residue acid concentration is still very high, causes extraction efficiency low, without actual promotional value.
4, acid system extraction process: acidic etching liquid water and alkaline matter adjust to 1～3 by pH value, use under acid system and be applicable to the extraction agent extracting copper-back extraction extracted under acid system, produce electrolytic copper, it is low that the acidic etching liquid pH value is adjusted under 1～3 o'clock acid system extracting power, after the copper extraction is a certain amount of, raffinate pH value decline extraction was lost efficacy, need be added a large amount of tap water dilution adjustment pH value to 1～3 and repeatedly extracted, ten times of increments of raffinate contain a large amount of dilute hydrochloric acid discharges and cause the wasting of resources and new environmental pollution, to enterprise, have increased the environmental protection treatment difficulty.
[summary of the invention]
The technical problem to be solved in the present invention is, defect for prior art, provide that a kind of not only the Cu in waste water content of discharge can qualified discharge after this processes, more can produce acidic etching waste solution of printed circuit board and the micro-etched waste liquid mixed processing method of highly purified metallic copper.
In order to solve the problems of the technologies described above, the invention provides a kind of acidic etching waste solution of printed circuit board and micro-etched waste liquid mixed processing method, said method comprising the steps of:
Step S1: in reactor, to adding the auxiliary material sodium hydroxide solution of mass volume ratio 40%-50% in pending acidic etching waste liquid, control pH value 8.0～10.0, stir, the fully rear discharging of question response is to the filter press system of solid-liquid separation, prepare cupric oxide, be collected in the heat energy produced when adding sodium hydroxide solution in described acidic etching waste liquid;
Step S2: add pending micro-etched waste liquid to dissolve the cupric oxide of described preparation, obtain the copper sulfate electrolyte of high cupric;
Step S3: once electrolytic: utilize the heat energy produced in step S1, the copper sulfate electrolyte of the high cupric that step S2 is obtained continues electrolysis with the current density of 1.5～3.0ASD, and described electrolyte temperature is controlled at 45 ℃～50 ℃, generates high purity metal copper;
Re-electrolysis: the copper concentration in described electrolytic solution is during lower than 10 grams per liter, utilize the heat energy produced in step S1, by concentration of copper sulfate in the concentrated electrolytic solution of electrolytic solution continuous heating to 50 ℃～70 ℃, and continue electrolysis with the high current density of 0.5～1.0ASD, generate high purity metal copper.
Further, in above-mentioned acidic etching waste solution of printed circuit board and micro-etched waste liquid mixed processing method, described step S3 also comprises: liquid after the electricity after electrolysis is added in the micro-etched waste liquid in described step S2, is cycled to repeat described step S2, S3.
Further, in above-mentioned acidic etching waste solution of printed circuit board and micro-etched waste liquid mixed processing method, described step S1 produces the copper content of efflux wastewater lower than 0.5ppm.
Not only copper content can qualified discharge in processed waste water for acidic etching waste solution of printed circuit board of the present invention and micro-etched waste liquid mixed processing method, it is product up to the metallic copper more than 99.5% that the purity of generation is more arranged, the thick copper sulfate that value produces far above common neutralization precipitation method, have obvious economic benefit and social benefit.
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is the schematic flow sheet of acidic etching waste solution of printed circuit board of the present invention and micro-etched waste liquid mixed processing method.
Refer to Fig. 1, Fig. 1 is the schematic flow sheet of acidic etching waste solution of printed circuit board of the present invention and the preferred embodiment of micro-etched waste liquid mixed processing method.
[accompanying drawing explanation]
Acidic etching waste solution of printed circuit board of the present invention and micro-etched waste liquid mixed processing method can be widely used in the manufacture course of processing of modern printed circuit board, the acidic etching waste liquid of its producible a large amount of high cuprics and micro-etched waste liquid.
Acidic etching waste solution of printed circuit board of the present invention and micro-etched waste liquid mixed processing method comprise the following steps:
[embodiment]
Step S1: in reactor, to adding the auxiliary material sodium hydroxide solution of mass volume ratio 40%-50% in pending acidic etching waste liquid, control pH value 8.0～10.0, stir, the fully rear discharging of question response, to the filter press system of solid-liquid separation, is prepared cupric oxide;
Step S2: add pending micro-etched waste liquid to dissolve the cupric oxide of described preparation, obtain the copper sulfate electrolyte of high cupric;
Step S3: the copper sulfate electrolyte to described high cupric carries out electrolysis, generates high purity metal copper.
Described step S1 also comprises: be collected in the heat energy produced when adding the auxiliary material sodium hydroxide solution in described acidic etching waste liquid.
Described thermal energy collecting can adopt the water circulating pipe mode.
Method of the present invention only described step S1 will produce efflux wastewater, and this Cu in waste water content effluxed is lower than 0.5ppm.
In step S2, in described pending micro-etched waste liquid, contain sulphuric acid soln and the cupric ion that can effectively utilize in a large number, utilize this waste liquid to dissolve the cupric oxide be prepared from by acidic etching waste liquid in dissolving tank, make the copper sulfate electrolyte of high cupric.
Described step S3 specifically comprises:
Once electrolytic: utilize the heat energy produced in step 1, the copper sulfate electrolyte of the high cupric that step S2 is obtained continues electrolysis with the current density of 1.5～3.0ASD, and described electrolyte temperature is controlled at 45 ℃～50 ℃, generates high purity metal copper;
Re-electrolysis: the copper concentration in described electrolytic solution is during lower than 10 grams per liter, utilize the heat energy produced in step 1, by concentration of copper sulfate in the concentrated electrolytic solution of electrolytic solution continuous heating to 50 ℃～70 ℃, and continue electrolysis with the high current density of 0.5～1.0ASD, generate high purity metal copper.
In the re-electrolysis step of described step S3, will produce oxygen and a small amount of sulfuric acid fog, but after alkalify gas tower is processed qualified discharge.
In order to reach the purpose of energy-saving and environment friendly, described step S3 also comprises: liquid after the electricity after electrolysis is added in the micro-etched waste liquid in described step S2, is cycled to repeat described step S2, S3.
Due to liquid after the electricity after re-electrolysis in described step 3, still contain available sulfuric acid and trace copper ion, therefore liquid after described electricity can be added in the micro-etched waste liquid in step S2, participate in the production process of step 2, supplement sulfuric acid and electrolytic solution liquid medicine amount, circulation participates in the flow process of whole treatment process.
Below in conjunction with specific embodiment, acidic etching waste solution of printed circuit board of the present invention and micro-etched waste liquid mixed processing method are described.
Embodiment 1:
In reactor, to adding the auxiliary material sodium hydroxide solution of mass volume ratio 40% in pending acidic etching waste liquid, control pH value 8.0～10.0, stir, the fully rear discharging of question response is to the filter press system of solid-liquid separation, prepare cupric oxide, and be collected in the heat energy produced when adding the auxiliary material sodium hydroxide solution in described acidic etching waste liquid.Add pending micro-etched waste liquid to dissolve the cupric oxide of described preparation, obtain the copper sulfate electrolyte of high cupric;
Once electrolytic: utilize the heat energy produced in above-mentioned steps, the copper sulfate electrolyte of the high cupric that obtains is continued to electrolysis with the current density of 1.5ASD, described electrolyte temperature is controlled at 45 ℃, generates high purity metal copper; Re-electrolysis: the copper concentration in described electrolytic solution is during lower than 10 grams per liter, utilize the heat energy produced in above-mentioned steps, by concentration of copper sulfate in electrolytic solution continuous heating to 50 ℃ concentrated electrolytic solution, and continue electrolysis with the high current density of 0.5ASD, generate high purity metal copper.Liquid after electricity after electrolysis is added in the micro-etched waste liquid in described above-mentioned steps, is cycled to repeat described step S2, S3.
Embodiment 2:
In reactor, to adding the auxiliary material sodium hydroxide solution of mass volume ratio 45% in pending acidic etching waste liquid, control pH value 8.0～10.0, stir, the fully rear discharging of question response is to the filter press system of solid-liquid separation, prepare cupric oxide, and be collected in the heat energy produced when adding the auxiliary material sodium hydroxide solution in described acidic etching waste liquid.Add pending micro-etched waste liquid to dissolve the cupric oxide of described preparation, obtain the copper sulfate electrolyte of high cupric;
Once electrolytic: utilize the heat energy produced in above-mentioned steps, the copper sulfate electrolyte of the high cupric that obtains is continued to electrolysis with the current density of 2.0ASD, described electrolyte temperature is controlled at 47 ℃, generates high purity metal copper; Re-electrolysis: the copper concentration in described electrolytic solution is during lower than 10 grams per liter, utilize the heat energy produced in above-mentioned steps, by concentration of copper sulfate in electrolytic solution continuous heating to 60 ℃ concentrated electrolytic solution, and continue electrolysis with the high current density of 0.7ASD, generate high purity metal copper.Liquid after electricity after electrolysis is added in the micro-etched waste liquid in described above-mentioned steps, is cycled to repeat described step S2, S3.
Embodiment 3:
In reactor, to adding the auxiliary material sodium hydroxide solution of mass volume ratio 50% in pending acidic etching waste liquid, control pH value 8.0～10.0, stir, the fully rear discharging of question response is to the filter press system of solid-liquid separation, prepare cupric oxide, and be collected in the heat energy produced when adding the auxiliary material sodium hydroxide solution in described acidic etching waste liquid.Add pending micro-etched waste liquid to dissolve the cupric oxide of described preparation, obtain the copper sulfate electrolyte of high cupric;
Once electrolytic: utilize the heat energy produced in above-mentioned steps, the copper sulfate electrolyte of the high cupric that obtains is continued to electrolysis with the current density of 3.0ASD, described electrolyte temperature is controlled at 50 ℃, generates high purity metal copper; Re-electrolysis: the copper concentration in described electrolytic solution is during lower than 10 grams per liter, utilize the heat energy produced in above-mentioned steps, by concentration of copper sulfate in electrolytic solution continuous heating to 70 ℃ concentrated electrolytic solution, and continue electrolysis with the high current density of 1.0ASD, generate high purity metal copper.Liquid after electricity after electrolysis is added in the micro-etched waste liquid in described above-mentioned steps, is cycled to repeat described step S2, S3.
Embodiment 4:
In reactor, to adding the auxiliary material sodium hydroxide solution of mass volume ratio 42% in pending acidic etching waste liquid, control pH value 8.0～10.0, stir, the fully rear discharging of question response is to the filter press system of solid-liquid separation, prepare cupric oxide, and be collected in the heat energy produced when adding the auxiliary material sodium hydroxide solution in described acidic etching waste liquid.Add pending micro-etched waste liquid to dissolve the cupric oxide of described preparation, obtain the copper sulfate electrolyte of high cupric;
Once electrolytic: utilize the heat energy produced in above-mentioned steps, the copper sulfate electrolyte of the high cupric that obtains is continued to electrolysis with the current density of 2.5ASD, described electrolyte temperature is controlled at 48 ℃, generates high purity metal copper; Re-electrolysis: the copper concentration in described electrolytic solution is during lower than 10 grams per liter, utilize the heat energy produced in above-mentioned steps, by concentration of copper sulfate in electrolytic solution continuous heating to 65 ℃ concentrated electrolytic solution, and continue electrolysis with the high current density of 1.0ASD, generate high purity metal copper.Liquid after electricity after electrolysis is added in the micro-etched waste liquid in described above-mentioned steps, is cycled to repeat described step S2, S3.
Embodiment 5:
In reactor, to adding the auxiliary material sodium hydroxide solution of mass volume ratio 48% in pending acidic etching waste liquid, control pH value 8.0～10.0, stir, the fully rear discharging of question response is to the filter press system of solid-liquid separation, prepare cupric oxide, and be collected in the heat energy produced when adding the auxiliary material sodium hydroxide solution in described acidic etching waste liquid.Add pending micro-etched waste liquid to dissolve the cupric oxide of described preparation, obtain the copper sulfate electrolyte of high cupric;
Once electrolytic: utilize the heat energy produced in above-mentioned steps, the copper sulfate electrolyte of the high cupric that obtains is continued to electrolysis with the current density of 2.5ASD, described electrolyte temperature is controlled at 50 ℃, generates high purity metal copper; Re-electrolysis: the copper concentration in described electrolytic solution is during lower than 10 grams per liter, utilize the heat energy produced in above-mentioned steps, by concentration of copper sulfate in electrolytic solution continuous heating to 65 ℃ concentrated electrolytic solution, and continue electrolysis with the high current density of 0.8ASD, generate high purity metal copper.Liquid after electricity after electrolysis is added in the micro-etched waste liquid in described above-mentioned steps, is cycled to repeat described step S2, S3.
Than prior art, not only copper content can qualified discharge in processed waste water for acidic etching waste solution of printed circuit board of the present invention and micro-etched waste liquid mixed processing method, it is product up to the metallic copper more than 99.5% that the purity of generation is more arranged, the thick copper sulfate that value produces far above common neutralization precipitation method, have obvious economic benefit and social benefit.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (3)
1. an acidic etching waste solution of printed circuit board and micro-etched waste liquid mixed processing method is characterized in that: said method comprising the steps of:
Step S1: in reactor, to adding the sodium hydroxide solution of mass volume ratio 40%-50% in pending acidic etching waste liquid, control the pH value 8.0～10.0, stir, the fully rear discharging of question response is to the filter press system of solid-liquid separation, prepare cupric oxide, be collected in the heat energy produced when adding sodium hydroxide solution in described acidic etching waste liquid;
Step S2: add pending micro-etched waste liquid to dissolve the cupric oxide of described preparation, obtain the copper sulfate electrolyte of high cupric;
Step S3: once electrolytic: utilize the heat energy produced in step S1, the copper sulfate electrolyte of the high cupric that step S2 is obtained continues electrolysis with the current density of 1.5～3.0ASD, and described electrolyte temperature is controlled at 45 ℃～50 ℃, generates high purity metal copper;
Re-electrolysis: the copper concentration in described electrolytic solution is during lower than 10 grams per liter, utilize the heat energy produced in step S1, by concentration of copper sulfate in the concentrated electrolytic solution of electrolytic solution continuous heating to 50 ℃～70 ℃, and continue electrolysis with the high current density of 0.5～1.0ASD, generate high purity metal copper.
2. acidic etching waste solution of printed circuit board according to claim 1 and micro-etched waste liquid mixed processing method is characterized in that:
Described step S3 also comprises: liquid after the electricity after electrolysis is added in the micro-etched waste liquid in described step S2, is cycled to repeat described step S2, S3.
3. acidic etching waste solution of printed circuit board according to claim 1 and micro-etched waste liquid mixed processing method is characterized in that: described step S1 produces the copper content of efflux wastewater lower than 0.5ppm.
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| 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 |
| CN103979625A (en) * | 2014-04-25 | 2014-08-13 | 昆山市益民环保技术开发有限公司 | Mixing method for treating acid and alkaline etching waste liquid and nitric acid stripping waste liquid of printed-circuit boards |
| CN104313653A (en) * | 2014-09-22 | 2015-01-28 | 梅县金象铜箔有限公司 | Method for preparing electrolyte for copper foil electrolysis by using regenerated copper oxide |
| CN104711636B (en) * | 2015-02-11 | 2018-09-25 | 昆山市益民环保技术开发有限公司 | Method for processing acidic etching waste solution of printed circuit board |
| CN107662988A (en) * | 2016-07-30 | 2018-02-06 | 湖北永绍科技股份有限公司 | A kind of processing method of acidic etching waste liquid |
| CN111925026A (en) * | 2020-07-03 | 2020-11-13 | 昆山中环实业有限公司 | Treatment process of acidic copper-containing etching waste liquid |
| CN112209543B (en) * | 2020-09-03 | 2022-12-20 | 深圳市环保科技集团股份有限公司 | Composite treatment method of complex copper waste liquid and microetching waste liquid |
| CN112808742B (en) * | 2020-12-31 | 2022-05-20 | 深圳星河环境股份有限公司 | Method and system for treating printed circuit board waste |
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| CN100385023C (en) * | 2006-09-29 | 2008-04-30 | 黄慎宗 | Copper recovering treatment process |
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