CN103789769A - Method for recycling and regenerating PCB (Printed Circuit Board) acidic and alkaline etching waste liquid - Google Patents
Method for recycling and regenerating PCB (Printed Circuit Board) acidic and alkaline etching waste liquid Download PDFInfo
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- CN103789769A CN103789769A CN201410016262.7A CN201410016262A CN103789769A CN 103789769 A CN103789769 A CN 103789769A CN 201410016262 A CN201410016262 A CN 201410016262A CN 103789769 A CN103789769 A CN 103789769A
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Abstract
The invention provides a method for recycling and regenerating PCB (Printed Circuit Board) acidic and alkaline etching waste liquid. The method comprises the following steps: feeding acidic and alkaline etching waste liquid and an alkaline extracting agent into a centrifugal extraction system under the driving of power in a ratio of 1:4, and mixing, agitating and separating, wherein copper ions of the separated etching liquid are reduced to be lower than 50g/L and thus the acidic and alkaline etching waste liquid is regenerated; blending the regenerated acidic and alkaline etching waste liquid and returning back to a production line for cyclic utilization; after separating, feeding the extracting agent into a centrifuging water washing groove; after washing with water, feeding the extracting agent into a centrifugal backwashing groove, mixing with 190g/L dilute sulfuric acid and stirring so that the extracted copper ions are converted into copper sulfate; conveying the copper sulfate into a centrifugal electrolysis system, and producing a pipe type electrolysis copper pipe under the effect of direct current, wherein the copper content of the copper pipe is 99.95%; and after backwashing, conveying the extracting agent into an extracting agent chamber for cyclic utilization. With the adoption of the method, the problems in the prior art that the extracting agent is easy to lose, sulfate ions easily enter regenerated liquid, an electrolytic bath is likely to generate short circuit in the operation process, the occupied area of equipment is large can be solved.
Description
Technical field:
The present invention relates to the recycling technology of a kind of printed circuit board manufacturing enterprise acid-basicity etching waste liquor, be specifically related to a kind of PCB acid-basicity etching waste liquor resource recovery and the method for regeneration.
Background technology
Printed circuit board is the basis of electronics and information industry, semi-conductor, and modern high-new technology products all be unable to do without printed circuit board.Along with the enhancing of global environmental consciousness, various countries cause prevention electronics manufacturing in process of production baneful influence to human body and the eubiosis is mentioned important agenda.In China, protect environment and could realize sustained economic development, Business Economic Benefit, environmental benefit also could synchronized development.Printed circuit board can produce a large amount of copper-containing wastewaters in the middle of production process, as soda acid etching solution, and chromium and copper waste water, micro-etching solution, the waste water such as alligatoring all contain a large amount of cupric ions.Wherein spent etching solution processing is the problem of puzzlement enterprise always.Have at present the method for much extracting copper from spent etching solution, but all there is following shortcoming in these methods: extraction agent demand is large, and regenerated liquid quality is unstable, current efficiency is not high, occupation area of equipment is large, and equipment fluctuation of service has extraction agent loss, the easy short circuit of electrolyzer etc. in operational process.Be badly in need of now a kind of novel treatment technology and process this problem.
Summary of the invention
The above-mentioned shortcoming existing in order to overcome prior art, the invention provides a kind of method that PCB acid-basicity etching waste liquor resource is reclaimed and regenerated, this system can solve that conventional art is in operation that extraction agent easily runs off, sulfate ion enters in a large number and in regenerated liquid, causes quality abnormal, and the easy short circuit of the electrolyzer that is in operation, occupation area of equipment is large, and electrolyzer drops into the problems such as high.
The technical scheme that a kind of method PCB acid-basicity etching waste liquor resource being reclaimed and regenerate of the present invention adopts is:
The method that PCB acid-basicity etching waste liquor resource is reclaimed and regenerated, the method comprises following step:
(1) acid-basicity etching waste liquor being sent into Centrifugical extraction separation system by power in 1:4 ratio with a kind of basic extractant carries out mix and blend and separates;
(2) separate after etching liquid cupric ion and be reduced to 50g/L and regenerated below, after allotment, return to production line and recycle;
(3) separate rear extraction agent and enter centrifugal water washing trough;
(4) after washing, extraction agent enters centrifugal anti-wash tank and 190g/L dilute sulphuric acid mix and blend, makes its cupric ion extracting be converted to copper sulfate;
(5) copper sulfate enters centrifugal electrolytic system, produces cast electrolysis copper pipe, copper content 99.95% under direct current effect;
(6) extraction agent after backwash enters extraction agent chamber and recycles.
Preferably, in above-mentioned Centrifugical extraction system, pending spent etching solution and extraction agent are pressed to throughput ratio 1:4 suction extraction cell by magnetic drive pump, after extraction, carrying out etching solution by pumping suction centrifugation chamber separates with extraction agent, wherein centrifugation adopts high speed centrifugation power to make mixed solution at internal rotating, and the liquid of different densities flows out the difference outlet by centrifugal chamber at a high speed.
Preferably, above-mentioned centrifugal electrolytic system main body is by managing dress negative electrode casing wall, anode bar, the centrifugal jet orifice of initial plate, liquid outlet, Waste gas outlet, flange in the bottom dish, the top flange dish composition be close to the negative electrode inside wall of cylinder are installed, copper sulfate liquid enters centrifugal jet orifice by high pressure pumping, and centrifugal jet orifice is injected electrolyzer inwall by oblique miter angle by copper sulfate and made its high speed rotating, is flowed out by the outlet of electrolyzer overhead stream, cyclic electrolysis, by high direct current at the initial plate face copper that produces electrolysis.Pipe dress negative electrode casing wall material can be processed into by stainless steel, titanium material.
The invention still further relates to a kind of novel process that adopts aforesaid method to recycle printed circuit board manufacturing enterprise alkaline etching waste liquid for producing, this technique comprises following several step:
(1) waste liquid is from producer's spent etching solution storage pool suction system spent etching solution hold-up vessel, by spent etching solution from spent etching solution hold-up vessel suction system Centrifugical extraction separation system; Extraction after etching liquid enters regeneration etching solution hold-up vessel by etching solution transferring system, from regeneration etching hold-up vessel, regeneration etching solution suction regeneration etching solution make-up tank is carried out to component adjustment, after adjusting, regeneration etching solution recycles by the sub-liquid add-on system of etching line suction etching production line;
(2) after extraction, enter centrifugal water wash system containing copper extractant and carry out circulating water wash, centrifugal washing enters copper sulfate generation system containing copper extractant afterwards and reacts generation copper sulfate liquid with dilute sulphuric acid, enters extraction agent circulation groove and recycle after extraction agent separates with cupric ion after washing;
(3) water of circulating water wash after completing enters recirculated water transferring system after centrifugation, recycles after returning to whose hold-up vessel of circulating water wash;
(4) copper sulfate generation system generates after copper sulfate liquid and to enter centrifugal electrolyzer through persulfuric acid copper transferring system and carry out centrifugal electrolysis and do and fall copper processing, the wherein pipe of cupric ion production purity 99.95% under the effect of electric field dress electrolytic copper, the sulfuric acid falling after copper continues to enter copper sulfate production system through copper sulfate circulation groove, recycles.
Accompanying drawing explanation:
Fig. 1 is alkali etching copper recovery system schema of the present invention;
Fig. 2 is the process flow sheet that PCB acid-basicity etching waste liquor resource of the present invention reclaims and regenerates;
In figure: 1-etching solution Centrifugical extraction groove, 2-centrifuge separator, 3-circulating water rinsing tank, 4-centrifuge separator, 5-copper sulfate generates groove, 6-centrifuge separator.
Embodiment:
Now by reference to the accompanying drawings the present invention is described further.Large in order to solve the extraction agent demand existing in prior art in the present invention, regenerated liquid quality is unstable, current efficiency is not high, occupation area of equipment is large, equipment fluctuation of service, in operational process, have the shortcomings such as extraction agent loss, the easy short circuit of electrolyzer, invent a kind of method that PCB acid-basicity etching waste liquor resource is reclaimed and regenerated, as shown in Figure 1, 2, for the technical process figure of PCB acid-basicity etching waste liquor resource recovery of the present invention and renovation process, the main following step of the method as we can see from the figure:
1, acid-basicity etching waste liquor being sent into Centrifugical extraction separation system by power in 1:4 ratio with a kind of basic extractant carries out mix and blend and separates;
2, separate after etching liquid cupric ion and be reduced to 50g/L and regenerated below, after allotment, return to production line and recycle;
3, separate rear extraction agent and enter centrifugal water washing trough;
4, after washing, extraction agent enters centrifugal anti-wash tank and 190g/L dilute sulphuric acid mix and blend, makes its cupric ion extracting be converted to copper sulfate;
5, copper sulfate enters centrifugal electrolytic system, produces cast electrolysis copper pipe, copper content 99.95% under direct current effect;
6, the extraction agent after backwash enters extraction agent chamber and recycles.
In above-mentioned steps, Centrifugical extraction system extracts (by pending spent etching solution and extraction agent by magnetic drive pump by throughput ratio 1:4 suction extraction cell) by extraction cell, carries out etching solution separate with extraction agent after extraction by pumping suction centrifugation chamber.(centrifugation adopts high speed centrifugation power to make mixed solution at internal rotating, and the liquid of different densities flows out the difference outlet by centrifugal chamber at a high speed); Washing is same as above with backwash function.Adopt above-mentioned Centrifugical extraction system, due to its separating effect at a high speed, compare traditional horizontal gravity stratification, release etch liquid and extraction agent faster, that when increasing treatment capacity, has reduced extraction agent stays the groove time, has lowered the consumption of extraction agent.Centrifugical extraction system separates mixed solution by centrifugal force, Gu separate more thorough, the generation that can greatly reduce sulfate ion and enter etching solution, thus guarantee the quality of etching regenerated liquid.
Centrifugal electrolytic system main body is by managing dress negative electrode casing wall (material can be made up of metal material processing such as stainless steel, titanium materials), anode bar, the centrifugal jet orifice of initial plate (install with the negative electrode inside wall of cylinder and be close to), liquid outlet, Waste gas outlet, flange in the bottom dish, top flange dish composition.Copper sulfate liquid enters centrifugal jet orifice by high pressure pumping, and centrifugal jet orifice is injected electrolyzer inwall by oblique miter angle by copper sulfate and made its high speed rotating, is flowed out cyclic electrolysis by the outlet of electrolyzer overhead stream.By high direct current at the initial plate face copper that produces electrolysis.Adopt this centrifugal electrolytic system, each electrolyzer can bear 400A electric current, relatively with traditional rectilinear electrolyzer, has reduced the quantity of anode, has guaranteed current efficiency.Thereby its internal structure is effectively stopped the probability of anode and cathode short circuit and is reduced maintenance cost.Improve economic benefit.
As shown in Figure 2, mainly comprise following several step at the recovery processing technique that this method by the recovery of PCB acid-basicity etching waste liquor resource and regeneration is applied to printed circuit board manufacturing enterprise alkaline etching waste liquid for producing:
1. waste liquid is from producer's spent etching solution storage pool suction system spent etching solution hold-up vessel, by spent etching solution from spent etching solution hold-up vessel suction system Centrifugical extraction separation system.Extraction after etching liquid (, regenerated liquid) enters regeneration etching solution hold-up vessel by etching solution transferring system.From regeneration etching hold-up vessel, regeneration etching solution suction regeneration etching solution make-up tank is carried out to component adjustment.After adjusting, regeneration etching solution recycles by the sub-liquid add-on system of etching line suction etching production line.
2. after extraction, enter centrifugal water wash system containing copper extractant and carry out circulating water wash, centrifugal washing enters copper sulfate generation system containing copper extractant afterwards and reacts generation copper sulfate liquid with dilute sulphuric acid.After extraction agent separates with cupric ion, after washing, entering extraction agent circulation groove recycles.
3. the water of circulating water wash after completing enters recirculated water transferring system after centrifugation, recycles after returning to circulating water wash water store tank.
4. copper sulfate generation system generates after copper sulfate liquid and to enter centrifugal electrolyzer through persulfuric acid copper transferring system and carry out centrifugal electrolysis and do and fall copper processing, the wherein pipe of cupric ion production purity 99.95% under the effect of electric field dress electrolytic copper.The sulfuric acid falling after copper continues to enter copper sulfate production system through copper sulfate circulation groove, recycles.
PCB acid-basicity etching waste liquor resource of the present invention reclaims and the method for regeneration adopts Centrifugical extraction technology, utilizes efficient centrifugal machine that treatment capacity in its unit time is improved greatly, and centrifugation is thorough rapidly, regenerated liquid stay in grade.Reduce the consumption of extraction agent; Adopt centrifugal electrolysis tech, reduce the problems such as the polarization that produces in electrolytic process, passivation, short circuit.Centrifugical extraction, centrifugal electrolysis are for I take charge of the Novel waste etching solution treatment technology of independent research and development, and Whole Equipment floor space reduces more than 50% with respect to conventional process equipment, and equipment moves can realize unmanned automatic management.Operating safety is stable.
Finally it should be noted that, above embodiment is only in order to describe technical scheme of the present invention rather than this technological method is limited, the present invention can extend to other modification, variation, application and embodiment in application, and therefore thinks that all such modifications, variation, application, embodiment are in spirit of the present invention and teachings.
Claims (5)
1. a method that PCB acid-basicity etching waste liquor resource is reclaimed and regenerated, is characterized in that, the method comprises following step:
(1) acid-basicity etching waste liquor being sent into Centrifugical extraction separation system by power in 1:4 ratio with a kind of basic extractant carries out mix and blend and separates;
(2) separate after etching liquid cupric ion and be reduced to 50g/L and regenerated below, after allotment, return to production line and recycle;
(3) separate rear extraction agent and enter centrifugal water washing trough;
(4) after washing, extraction agent enters centrifugal anti-wash tank and 190g/L dilute sulphuric acid mix and blend, makes its cupric ion extracting be converted to copper sulfate;
(5) copper sulfate enters centrifugal electrolytic system, produces cast electrolysis copper pipe, copper content 99.95% under direct current effect;
(6) extraction agent after backwash enters extraction agent chamber and recycles.
2. method according to claim 1, it is characterized in that: in Centrifugical extraction system, pending spent etching solution and extraction agent are pressed to throughput ratio 1:4 suction extraction cell by magnetic drive pump, after extraction, carrying out etching solution by pumping suction centrifugation chamber separates with extraction agent, wherein centrifugation adopts high speed centrifugation power to make mixed solution at internal rotating, and the liquid of different densities flows out the difference outlet by centrifugal chamber at a high speed.
3. method according to claim 1 and 2, it is characterized in that: centrifugal electrolytic system main body is by managing dress negative electrode casing wall, anode bar, the centrifugal jet orifice of initial plate, liquid outlet, Waste gas outlet, flange in the bottom dish, the top flange dish composition be close to the negative electrode inside wall of cylinder are installed, copper sulfate liquid enters centrifugal jet orifice by high pressure pumping, centrifugal jet orifice is injected electrolyzer inwall by oblique miter angle by copper sulfate and is made its high speed rotating, flowed out by the outlet of electrolyzer overhead stream, cyclic electrolysis, by high direct current at the initial plate face copper that produces electrolysis.
4. method according to claim 3, is characterized in that, pipe dress negative electrode casing wall material can be processed into by stainless steel, titanium material.
5. adopt the arbitrary described method of claim 1-4 to recycle a novel process for printed circuit board manufacturing enterprise alkaline etching waste liquid for producing, it is characterized in that this technique comprises following several step:
(1) waste liquid is from producer's spent etching solution storage pool suction system spent etching solution hold-up vessel, by spent etching solution from spent etching solution hold-up vessel suction system Centrifugical extraction separation system; Extraction after etching liquid enters regeneration etching solution hold-up vessel by etching solution transferring system, from regeneration etching hold-up vessel, regeneration etching solution suction regeneration etching solution make-up tank is carried out to component adjustment, after adjusting, regeneration etching solution recycles by the sub-liquid add-on system of etching line suction etching production line;
(2) after extraction, enter centrifugal water wash system containing copper extractant and carry out circulating water wash, centrifugal washing enters copper sulfate generation system containing copper extractant afterwards and reacts generation copper sulfate liquid with dilute sulphuric acid, enters extraction agent circulation groove and recycle after extraction agent separates with cupric ion after washing;
(3) water of circulating water wash after completing enters recirculated water transferring system after centrifugation, recycles after returning to whose hold-up vessel of circulating water wash;
(4) copper sulfate generation system generates after copper sulfate liquid and to enter centrifugal electrolyzer through persulfuric acid copper transferring system and carry out centrifugal electrolysis and do and fall copper processing, the wherein pipe of cupric ion production purity 99.95% under the effect of electric field dress electrolytic copper, the sulfuric acid falling after copper continues to enter copper sulfate production system through copper sulfate circulation groove, recycles.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104532293A (en) * | 2014-12-22 | 2015-04-22 | 无锡市瑞思科环保科技有限公司 | Method of purifying nickel from chemical nickel-plating waste liquid and nickel purification device |
| 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 |
| CN106757182A (en) * | 2017-01-19 | 2017-05-31 | 昆山元天电子有限公司 | A kind of recycling technique of PCB surface metallic copper |
| CN107313069A (en) * | 2017-05-22 | 2017-11-03 | 广东省稀有金属研究所 | A kind of method by acid, the mashed up recovery copper of alkali spent etching solution |
| CN108301000A (en) * | 2017-05-17 | 2018-07-20 | 佛山鑫仁源环保科技有限公司 | Alkaline etching liquid indirect regeneration |
| CN109536725A (en) * | 2019-01-14 | 2019-03-29 | 北京康普锡威科技有限公司 | Printed plate board etching waste liquor processing method, copper nanoparticle and preparation method thereof |
| CN110042251A (en) * | 2019-05-27 | 2019-07-23 | 深圳市祺鑫天正环保科技有限公司 | The recovery method and recovery system of copper in alkaline etching waste liquid for producing |
| CN110144590A (en) * | 2019-05-31 | 2019-08-20 | 深圳市泓达环境科技有限公司 | Alkaline copper-containing etching waste solution regeneration and the ammonia nitrogen waste water circulatory system |
| CN114606497A (en) * | 2022-01-28 | 2022-06-10 | 斯瑞尔环境科技股份有限公司 | Process method for treating and regenerating cycle of ferric trichloride etching solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107313069A (en) * | 2017-05-22 | 2017-11-03 | 广东省稀有金属研究所 | A kind of method by acid, the mashed up recovery copper of alkali spent etching solution |
| CN109536725A (en) * | 2019-01-14 | 2019-03-29 | 北京康普锡威科技有限公司 | Printed plate board etching waste liquor processing method, copper nanoparticle and preparation method thereof |
| CN110042251A (en) * | 2019-05-27 | 2019-07-23 | 深圳市祺鑫天正环保科技有限公司 | The recovery method and recovery system of copper in alkaline etching waste liquid for producing |
| CN110144590A (en) * | 2019-05-31 | 2019-08-20 | 深圳市泓达环境科技有限公司 | Alkaline copper-containing etching waste solution regeneration and the ammonia nitrogen waste water circulatory system |
| CN114606497A (en) * | 2022-01-28 | 2022-06-10 | 斯瑞尔环境科技股份有限公司 | Process method for treating and regenerating cycle of ferric trichloride etching solution |
| CN114606497B (en) * | 2022-01-28 | 2024-03-19 | 斯瑞尔环境科技股份有限公司 | Ferric trichloride etching solution treatment and regeneration circulation process method |
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