CN1782132A - Method and device for controlling copper concentration in decayed copper liquid - Google Patents
Method and device for controlling copper concentration in decayed copper liquid Download PDFInfo
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- CN1782132A CN1782132A CN 200410047003 CN200410047003A CN1782132A CN 1782132 A CN1782132 A CN 1782132A CN 200410047003 CN200410047003 CN 200410047003 CN 200410047003 A CN200410047003 A CN 200410047003A CN 1782132 A CN1782132 A CN 1782132A
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Abstract
The present invention relates to method and apparatus for controlling the copper concentration in copper etching liquid. The control method includes proper pre-treatment of copper etching liquid, such as temperature regulation, turbidity control, oxidation-reduction potential regulation, pH regulation, etc.; and setting the copper etching liquid inside a membrane-electric deposition set with membrane separated cathode and anode for copper ion to penetrate through the membrane and deposit on the cathode as metal copper or insoluble copper compound. The copper etching liquid pre-treating apparatus includes filter, temperature controller, oxidation-reduction potential regulator and pH regulator. The copper separating apparatus includes DC power source, membrane-electric deposition set, etc. The copper concentration in copper etching liquid is controlled in 0.5-160 g/l and is suitable for use circularly.
Description
Technical field
The present invention relates to a kind of equipment of controlling method and this method of realization of copper concentration in the rotten copper liquid.
Background technology
Rotten copper liquid is solution widely used in the industries such as printed-wiring board (PWB) (etching work procedure), metal cleaning and surface treatment, sign manufacturing, copper hydrometallurgy, come dissolved copper or copper mineral by chemistry or galvanic corrosion, be called mashed plate liquid, etching solution, etching reagent etc. again, as printed-wiring board (PWB) (PCB) the online use of industry etching work procedure or face the etching solution that (replacing) scraps, the latter is used to be called spent etching solution.Rotten copper liquid also can be further divided into acid and alkaline two classes by its acid-basicity, as the acidic etching liquid and the alkaline etching liquid of online use in the industry of printed circuit boards, or faces acidic etching liquid and the alkaline etching liquid that (replacing) scraps.In use, the copper concentration of rotten copper liquid is controlled in certain scope, as 40-150g/L, with obtain the user at this operation desired application index such as industry of printed circuit boards in the desired etching index of etching work procedure, it comprises etching speed, etching capacity and lateral erosion (factor) coefficient etc.As its span of control of copper deviation of concentration in the rotten copper liquid such as Tai Gao or when too low, the etching index of its application indexes such as industry of printed circuit boards etching work procedure will worsen, and rotten copper liquid faces (replacing) at this moment and scraps.Change is exactly with cupric (as the so-called fresh etching solution of PCB industry) or the lower solution of cupric concentration do not remove partly or entirely to change those rotten copper liquid because of the higher application indexes variation of copper concentration (as the so-called spent etching solution of PCB industry), in the rotten copper liquid that changes except cupric, also contain other material, just contain a large amount of muriates in the so-called spent etching solution as the PCB industry, oxymuriate, tensio-active agent, biodegradable organic compounds etc., therefore the replacing process is exactly the process that rotten copper liquid is scrapped, the i.e. process of output industrial waste; Because its high toxicity and complicacy, the so-called spent etching solution that the PCB industry is discharged by State Environmental Protection Administration qualitative be the dangerous liquid refuse, forbid transboundary movement.For this class dangerous liquid refuse, serious environment pollution directly discharges in the small-sized PCB enterprise that has; It is that the recycling of starting point is as processing copper sulfate etc. that bigger PCB enterprise or waste treatment unit have then carried out to carry copper, but the further output number of course of processing meeting decuples the trade effluent of Liquid wastes amount, copper concentration wherein generally is higher than the wastewater discharge standard of State Bureau of Environmental Protection, and the non-copper component in the Liquid wastes is not more taked control measures targetedly.Therefore, processing after rotten copper liquid (replacing) is scrapped or governance process are one makes the further process of diffusion of source of pollution, and water resources and ecotope are damaged.
Thereby how selective separation copper remains in the desirable scope of user its copper concentration from the spent etching solution of rotten copper liquid such as PCB industry, recycles to prolong its work-ing life even realization, is numerous scientific and technical personnel's target always.USP5524780 and USP5556553 have reported the method that adopts aluminium reducing copper and carry out the use of PCB copper etchant solution cyclic regeneration, USP5487842 and CN1154723 have then reported and have adopted solvent extraction to carry out the method that PCB copper etchant solution cyclic regeneration uses, equipment has high input, the process management difficulty is big, priming cost is high because they exist, the solution of separating copper is not easy to keep shortcomings such as its application performance when carrying out the cyclic regeneration use, uses and promote less.
Summary of the invention
The present invention is from pollution prevention (being cleaner production) rather than does not hold the thinking of administering, the higher rotten copper liquid of copper content such as the spent etching solution of PCB industry are carried out selective separation copper, thereby its copper concentration is remained in the desired scope of user, reach the purpose of stablizing its application performance (as etch copper) and recycling.
An object of the present invention is, a kind of method of controlling copper concentration in the rotten copper liquid is provided.Rotten copper liquid is a kind of solution of energy dissolved copper, be called mashed plate liquid, etching solution, etching reagent etc. again in fields such as printed-wiring board (PWB) (PCB) manufacturing, metal cleaning and surface treatment, sign manufacturings, online use or face the etching solution that (replacing) scraps in the preferred industry of printed circuit boards etching machine, the latter is used to be called spent etching solution.
Another object of the present invention is, a kind of equipment and flow process thereof of controlling copper concentration in the rotten copper liquid is provided, and it is suitable for realizing the method for copper concentration in the rotten copper liquid of control of the present invention.
By first aspect of the present invention, the method for controlling the copper concentration in the rotten copper liquid is achieved through the following channels:
(1) rotten copper liquid (as the spent etching solution of PCB industry) is carried out suitable pre-treatment earlier, comprise the physical-chemical parameters such as its temperature, turbidity, redox potential, pH are regulated;
Rotten copper liquid is carried out pretreated the physical-chemical parameters scope to be should be: temperature: 1.5-90 ℃; Turbidity: TSS (total suspended solid)≤10mg/L; Redox potential :-1.0V is to+1.0V; PH:0.5-11.Can adjust the temperature to 1.5-95 ℃ by heating, the type of cooling of routine, optimum range 20-55 ℃; Can adopt conventional removal suspended substance method such as sand filtration, MF (micro-filtration) to control TSS (total suspended solid)≤10mg/L, best TSS scope≤2mg/L; The method of concentration that can be by reducing or increase oxidizing substance in the solution or reducing substances or regulate redox potential to-1.0V to+1.0V with electrochemical method, optimum range-0.5V is to+0.5V; Regulating the pH value is the most conventional technological operation in this area, those of ordinary skills can learn employed material and operation steps fully easily, the pH value is adjusted to 0.5-11 and is advisable, and generally is to control pH at 0.5-3 at acidic etching liquid, and alkaline etching liquid is then controlled its pH at 7.5-10.
(2) will more than carried out the rotten copper liquid that the physical-chemical parameters regulates and place a negative and positive polar region by the isolated film-electric deposition device of a kind of film spacer, make cupric ion in the rotten copper liquid see through the film spacer and migrate on the negative electrode and deposit out with the form of metallic copper or insoluble copper compound; The result is that part copper is come out by galvanic deposit optionally from rotten copper liquid at least, and other composition keeps, and copper concentration is controlled in the desirable scope of user, in the scope as 0.5-160g/L (grams per liter) in the rotten copper liquid.
Film spacer in film-electric deposition device can adopt ceramic membrane common on the market, asbestos diaphragm and organic high molecular layer etc., and organic high molecular layer comprises anion-exchange membrane and cationic exchange membrane; The bath voltage of film-electrodeposition process is advisable with 1-6V, can with more than carried out polar region that rotten copper liquid that the physical-chemical parameters regulates places electrolyzer, another polar region then is equipped with close electrolyte solution such as vitriol-sulphuric acid soln or the ammoniacal liquor-ammonium salt solution etc. with rotten copper liquid pH, the liquid level of negative and positive polar region can be the same or different, and can adopt conventional detection means to monitor parameters such as its temperature, copper concentration, bath voltage, pH.
By another aspect of the present invention, the equipment of implementing the method for copper concentration in the rotten copper liquid of control comprises following device unit:
(1) device that the physical-chemical parameters such as temperature, turbidity, redox potential and the pH of rotten copper liquid regulated and control, and for realizing the physico-chemical parameter monitoring device of these regulation and control purposes;
(2) copper in the rotten copper liquid is deposited film-electric deposition device of coming out with the form of metallic copper or insoluble copper compound in galvanic deposition cell.
In the device of regulating physico-chemical parameter, the device of said attemperation comprises heating and the cooling apparatus that shell-and-tube heat exchanger, tubular heat exchanger, plate-type heat exchanger etc. are conventional; Regulate the device such as the conventional suspended substance removal devices such as sand filtering device, micro-filtration (MF) device of turbidity; The device of adjusting redox potential comprises the adding apparatus of oxygenant and reductive agent etc.; Regulate the soda acid adding apparatus of pH etc.
In film-electric deposition device that the copper in the rotten copper liquid is deposited out with the form of metallic copper or insoluble copper compound, said film-electrodeposition apparatus comprises direct supply, solution transfer pump, diaphragm sell or ion-exchange membrane electrolyzer, insoluble anode (DSA) and electroconductibility negative electrode such as copper coin, titanium plate, stainless steel plate, copper starting sheet etc.They can individually be bought from the market or order from specialized factory is whole, as the Asahi Glass company of Japan, Beijing chemical machinery head factory of China etc.
The equipment that carries out in pre-treatment and the selective copper removal process various physico-chemical parameters being monitored at rotten copper liquid comprises:
PH meter, turbidometer, cupric ion detector, thermometer and ORP conventional sense equipment such as (redox electrodes), they can buy very easily from the market.
See Fig. 1 and Fig. 2 about the further graphic extension of controlling the method and apparatus flow process of copper concentration in the rotten copper liquid.
Description of drawings:
Fig. 1 is the process flow diagram of copper concentration in the rotten copper liquid of control;
Fig. 2 is the equipment flowsheet synoptic diagram of copper concentration in the rotten copper liquid of control.
Embodiment 1:
The Hunan used etching solution of circuit board plant etching work procedure is an alkaline etching liquid, requires its copper concentration to be the 80-100 grams per liter when normally using, cupric 162 grams per liters after measured when scrapping.Get 50 liters of this waste liquids, earlier its physical-chemical parameters is adjusted to: temperature: 20-30 ℃; Turbidity: TSS (total suspended solid)≤2mg/L; Redox potential :-0.2V is to+0.5V; PH:8.5-10.Then it being sent into a cumulative volume is that 110L, membrane area are 0.75m
2The positive column (ionic membrane is the Nafion film of Du Pont company) of ionic membrane-electric deposition device, it is ammoniacal liquor-ammoniumsulphate soln of 8-9 that pH is placed in the cathodic area, and anode adopts Graphite Electrodes, and negative electrode adopts copper starting sheet, the temperature of maintenance system is at 20-45 ℃, pH8-11; Groove at 4V is pressed and 350A/M
2Electrolysis is after 15 hours under the current density, and the copper concentration that records etching waste liquor becomes 82 grams per liters, can return etching work procedure and use; 4 kilograms of negative plate weightening finishes simultaneously are metallic copper after testing.
Embodiment 2:
The Hunan used etching solution of circuit board plant etching work procedure is an acidic etching liquid, requires its copper concentration to be the 85-110 grams per liter when normally using, cupric 151 grams per liters after measured when scrapping.Get 100 liters of this waste liquids, earlier its physical-chemical parameters is adjusted to: temperature: 20-30 ℃; Turbidity: TSS (total suspended solid)≤2mg/L; Redox potential :-0.2V is to+0.5V; PH:0.5-2.Then it being sent into a cumulative volume is that 210L, membrane area are 1.25m
2The positive column (barrier film is an asbestos diaphragm) of diaphragm-electric deposition device, it is sulfuric acid-ammoniumsulphate soln of 0.5-1.5 that pH is placed in the cathodic area, anode adopts insoluble titanium anode, negative electrode adopts stainless steel plate, the temperature that keeps system is at 25-40 ℃, pH0.5-2; Groove at 4.5V is pressed and 400A/M
2Electrolysis is after 14 hours under the current density, and the copper concentration that records this etching waste liquor becomes 91 grams per liters, can return former etching work procedure and use; 6 kilograms of negative plate weightening finishes simultaneously are metallic copper after testing.
Embodiment 3:
The Hunan used etching solution of circuit board plant etching work procedure is an acidic etching liquid, requires its copper concentration to be the 80-105 grams per liter when normally using, cupric 148 grams per liters after measured when scrapping.Get 70 liters of this waste liquids, earlier its physical-chemical parameters is adjusted to: temperature: 20-30 ℃; Turbidity: TSS (total suspended solid)≤2mg/L; Redox potential :-0.2V is to+0.5V; PH:0.5-2.Then it being sent into a cumulative volume is that 150L, membrane area are 0.95m
2The positive column (barrier film is the ceramic membrane in 1.5 μ m apertures) of barrier film-electric deposition device, it is sulfuric acid-ammoniumsulphate soln of 0.5-1.5 that pH is placed in the cathodic area, and anode adopts insoluble titanium anode, and negative electrode adopts the titanium plate, the temperature of maintenance system is at 25-40 ℃, pH0.5-2; Groove at 4.1V is pressed and 400A/M
2Electrolysis is after 10 hours under the current density, and the copper concentration that records this etching waste liquor becomes 95 grams per liters, can return former etching work procedure and use; 3.7 kilograms of negative plate weightening finishes simultaneously are metallic copper after testing.
Claims (11)
1. method of controlling copper concentration in the rotten copper liquid is characterized in that may further comprise the steps:
(1) rotten copper liquid is carried out the physical-chemical parameters such as suitable pre-treatment such as attemperation, turbidity, redox potential, pH;
(2) will pass through pretreated rotten copper liquid and place a negative and positive polar region, and make cupric ion in the rotten copper liquid see through the film spacer and migrate on the negative electrode and deposit out with the form of metallic copper or insoluble copper compound by the isolated film-electric deposition device of a kind of film spacer; Copper concentration remaining in the rotten copper liquid is controlled in the scope of 0.5-160g/L (grams per liter).
2. according to the method for claim 1, it is characterized in that: said rotten copper liquid is a kind of solution of energy dissolved copper, be called mashed plate liquid, etching solution, etching reagent etc. again in fields such as printed-wiring board (PWB) manufacturing, metal cleaning and surface treatment, sign manufacturings, online use or face acidity or the alkaline etching liquid that (replacing) scraps in the preferred industry of printed circuit boards etching machine, the latter is used to be called spent etching solution.
3. according to the method for claim 2, it is characterized in that: the physical-chemical parameters scope through pretreated rotten copper liquid is: 1.5 to 90 ℃ of temperature; TSS (total suspended solid)≤10mg/L; Redox potential-1.0V is to+1.0V; PH value 0.5 to 11.
4. according to claim 1, each method in 2 and 3, it is characterized in that: said film-electric deposition device comprises barrier film and electrochemical apparatus at least, and the cupric ion in the rotten copper liquid finally can the form with metallic copper or insoluble copper compound deposit out on the negative electrode of electrochemical apparatus.
5. according to claim 1,2, each method in 3 and 4, it is characterized in that: said film spacer is a kind of solids that solution can be isolated but can allow ion pass through, it keeps apart positive column and cathodic area, makes that its character of solution of placing in positive column and the cathodic area can be identical or different.
6. according to the method for claim 5, it is characterized in that: the film spacer is selected from ceramic membrane, asbestos diaphragm and organic high molecular layer.
7. according to the method for claim 5, it is characterized in that: organic high molecular layer is selected from anion-exchange membrane and cationic exchange membrane.
8. realize the equipment of each method among the claim 1-7, it is characterized in that: the device that rotten copper liquid is carried out suitable pretreated device and copper is come out by galvanic deposit from rotten copper liquid.
9. according to the equipment of claim 8, it is characterized in that: saidly rotten copper liquid is carried out suitable pretreated device comprise: device such as the sand filtering device and the micro-filtration of suspended substance promptly removed in turbidity control; Carry out temperature controlled routine and heat-reach cooling apparatus such as shell-and-tube heat exchanger, plate-type heat exchanger etc.; Carry out the oxygenant of redox potential adjusting and the adding apparatus of reductive agent; Carry out the soda acid adding apparatus of pH regulator; And these the physical-chemical parameters are carried out the detecting instrument such as the pH meter of on-line monitoring, thermometer and ORP (redox electrode).
10. according to the equipment of claim 8 or 9, it is characterized in that: the said device that copper is come out by galvanic deposit from rotten copper liquid comprises direct supply, solution transfer pump, membrane module (film device), insoluble anode (DSA) and electroconductibility negative electrode at least.
11. the equipment according to claim 10 is characterized in that: said electroconductibility negative electrode is selected from copper coin, stainless steel plate, titanium plate, copper starting sheet; Film in the membrane module (film device) can be ceramic membrane or asbestos diaphragm or organic high molecular layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410047003 CN1782132A (en) | 2004-12-03 | 2004-12-03 | Method and device for controlling copper concentration in decayed copper liquid |
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| CN 200410047003 CN1782132A (en) | 2004-12-03 | 2004-12-03 | Method and device for controlling copper concentration in decayed copper liquid |
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| CN 200410047003 Pending CN1782132A (en) | 2004-12-03 | 2004-12-03 | Method and device for controlling copper concentration in decayed copper liquid |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101988200A (en) * | 2009-08-04 | 2011-03-23 | 章晓冬 | Cyclic regeneration and metal reclamation equipment for acid chloride-containing etchant |
| CN103663803A (en) * | 2012-09-17 | 2014-03-26 | 武汉环材科技有限公司 | Efficient electro-deposited heavy metal cleaning system |
| CN104087938A (en) * | 2014-06-18 | 2014-10-08 | 京东方科技集团股份有限公司 | Etching-liquid storing apparatus and wet-method etching equipment |
| CN104535636A (en) * | 2014-12-16 | 2015-04-22 | 宇宙电路板设备(深圳)有限公司 | Oxidizing agent inductor, oxidizing agent adding control circuit and controller |
| CN104894562A (en) * | 2015-05-06 | 2015-09-09 | 信利（惠州）智能显示有限公司 | Method for prolong service life of Mo/Al etching soup |
| CN105862040A (en) * | 2016-06-20 | 2016-08-17 | 深圳市华星光电技术有限公司 | Copper-etching solution additive and production method of copper-etching solution |
| CN107626207A (en) * | 2017-09-28 | 2018-01-26 | 昆明理工大学 | The method and apparatus for synchronously reclaiming metal using conductivity ceramics film enrichment spent acid |
| CN110468279A (en) * | 2019-09-09 | 2019-11-19 | 赵坤 | A method of recycling lead from the lead plaster material of waste lead storage battery |
-
2004
- 2004-12-03 CN CN 200410047003 patent/CN1782132A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101988200A (en) * | 2009-08-04 | 2011-03-23 | 章晓冬 | Cyclic regeneration and metal reclamation equipment for acid chloride-containing etchant |
| CN103663803A (en) * | 2012-09-17 | 2014-03-26 | 武汉环材科技有限公司 | Efficient electro-deposited heavy metal cleaning system |
| CN104087938A (en) * | 2014-06-18 | 2014-10-08 | 京东方科技集团股份有限公司 | Etching-liquid storing apparatus and wet-method etching equipment |
| CN104535636A (en) * | 2014-12-16 | 2015-04-22 | 宇宙电路板设备(深圳)有限公司 | Oxidizing agent inductor, oxidizing agent adding control circuit and controller |
| CN104894562A (en) * | 2015-05-06 | 2015-09-09 | 信利（惠州）智能显示有限公司 | Method for prolong service life of Mo/Al etching soup |
| CN104894562B (en) * | 2015-05-06 | 2017-06-16 | 信利（惠州）智能显示有限公司 | A kind of extension Mo/Al etches the service life method of liquid |
| CN105862040A (en) * | 2016-06-20 | 2016-08-17 | 深圳市华星光电技术有限公司 | Copper-etching solution additive and production method of copper-etching solution |
| US10246783B2 (en) | 2016-06-20 | 2019-04-02 | Shenzhen China Star Optoelectronics Technology Co., Ltd | Copper etchant solution additives and method for producing copper etchant solution |
| CN107626207A (en) * | 2017-09-28 | 2018-01-26 | 昆明理工大学 | The method and apparatus for synchronously reclaiming metal using conductivity ceramics film enrichment spent acid |
| CN107626207B (en) * | 2017-09-28 | 2020-10-27 | 昆明理工大学 | Method and device for enriching waste acid and synchronously recovering metal by using conductive ceramic membrane |
| CN110468279A (en) * | 2019-09-09 | 2019-11-19 | 赵坤 | A method of recycling lead from the lead plaster material of waste lead storage battery |
| CN110468279B (en) * | 2019-09-09 | 2021-04-06 | 赵坤 | Method for recovering lead from lead plaster material of waste lead storage battery |
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