CN103480860A - Method for preparing high-purity nanometer copper by using printed circuit board alkaline etching waste liquid - Google Patents
Method for preparing high-purity nanometer copper by using printed circuit board alkaline etching waste liquid Download PDFInfo
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Abstract
The invention discloses a method for preparing high-purity nanometer copper by using printed circuit board alkaline etching waste liquid. The method is characterized by including the following steps: a. taking an appropriate amount of alkaline etching waste liquid and putting the liquid into a centrifuge tube to conduct high-speed centrifugation, adding upper-layer clarified liquor in the centrifuge tube into an ammonium hydroxide adjusting solution, and adding a surface active dispersing agent into the solution to obtain a reactant A; b. preparing a solution B containing hydrazine hydrate, sodium hydroxide and a nanometer copper dispersing accelerant, heating and stirring, and adding the reactant A into the solution B dropwise slowly to conduct reaction; c. cooling to the room temperature after the reaction is finished, transferring to the centrifuge tube to conduct high-speed centrifugal separation and collecting lower-layer solution after separation; d. washing the obtained solution containing high-purity nanometer copper by using absolute ethyl alcohol, and after the last washing, transferring an alcoholic solution containing the nanometer copper into a vacuum rotary evaporator to extract nanometer copper powder. The method is easy to operate and free of large energy consumption and can conduct large-scale production under the existing conditions.
Description
Technical field
The present invention relates to extract the technical field of nano-metallic copper powder method, particularly relate to the method that the alkaline etching waste liquid for producing emitted prepares the high-purity nano copper powder from printed circuit board factory.
Background technology
Copper nanoparticle due to its size in 100 nanometer range, compare and have than bigger serface with common copper powder, exactly because also so nano copper particle shows excellent characteristic at aspects such as optical property, catalytic performance, electric conductivities, in the industrial products of some characteristics of the ground of extensive use at present application, enhance product performance.For example, due to very little and soft of copper nanoparticle size, therefore be a kind of good lubricating additive, it is added in automobile lubricating oil used, can improve the wearability of engine cylinder and piston, the lubricating oil that adds copper nanoparticle also has the function of energy-conserving and environment-protective, because copper nanoparticle has higher electric conductivity, the copper nanoparticle of having take at present adds material as conduction and has prepared various conductor pastes, for the formation of printed circuit board circuit in addition.
At present, most printed circuit board circuits are all to utilize etching solution to carry out etching by the design of engineering to form, therefore produce a large amount of etching waste liquors.Contain a large amount of copper in alkaline etching waste liquid for producing, it is mainly with [Cu (NH
3)
4]
2+form exist, also contain a large amount of NH simultaneously
3h
2o, Cl
-deng.Optionally abandon not only serious environment pollution of etching waste liquor, and waste a large amount of copper.
In recent years, the researcher had proposed some effective recovery methods for the recovery of utility in the etching waste liquor produced in the PCB manufacture process, and these methods have: 1 ﹑ chemical precipitation method.Add NaOH, Na in alkaline etching waste liquid for producing
2cO
3deng alkaline matter, generate Cu (OH)
2precipitation obtains Cu (OH) through filtering
2solid then obtains CuO or adds H after high-temperature heating
2sO
4solution finally obtains CuSO
4; 2 ﹑ extraction electro-deposition.First to adding the contact break agent to make copper dissociate out in alkaline etching waste liquid for producing, become copper ion from the complex compound of copper, then add some extractants of copper to the inside, has obtained the solution of copper ion through stripping, then utilize the method for electro-deposition to obtain elemental copper; The direct electro-deposition of 3 ﹑.Representational is German Elochen alkaline etching liquid recovery system.The method requires the CuCl in etching solution
2become CuSO
4.After production process produces etching waste liquor.Owing to there is no Cl in waste liquid
-, can be out of use extraction and directly electro-deposition obtain Cu simple substance.The shortcoming such as yet these method ubiquity complex process, the rate of recovery are not high, it is higher to expend and the regenerant cost performance is not high, limited their extensive uses in this industry.
Summary of the invention
Purpose of the present invention is exactly the deficiency in order to solve prior art and a kind of easy operation that provides, environmental protection and energy saving, and the alkaline etching waste liquid for producing printed circuit board that utilizes that can under existence conditions, carry out large-scale production prepares the method for high-purity nano copper.
The present invention adopts following technical solution to realize above-mentioned purpose: a kind of method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare high-purity nano copper, it is characterized in that, and it comprises the steps:
A, get appropriate alkaline etching waste liquid for producing and pack in centrifuge tube and carry out high speed centrifugation, to remove suspended impurity trickle in alkaline etching waste liquid for producing, centrifugal after by centrifuge tube at the middle and upper levels clarified solution transfer in container, add the pH value of ammoniacal liquor regulator solution in the 8-12 scope, to solution, add by the active dispersant of the composite surface of softex kw and polyvinylpyrrolidone simultaneously, its addition be take the alkaline etching waste liquid for producing amount as benchmark, add 0.04 kilogram-0.15 kilogram in the alkaline etching waste liquid for producing of 1 liter, will now obtain solution as reaction A thing;
B, preparation reactant B solution, comprise hydrazine hydrate with reproducibility in B solution, there is alkaline NaOH and Nanometer Copper disperses the promoter polyethylene glycol, the amount concentration that the amount of substance concentration that wherein the amount concentration of hydrazine hydrate is 0.05～0.25 mol/L, NaOH is 0.2-2 mol/L, polyethylene glycol is the 0.5-2 mol/L, solution B is heated to 60 ℃-100 ℃, stirs with 100 rev/mins of-1000 rev/mins of speed simultaneously; Again reactant A is slowly dropped in solution B, drip with relief system reaction 60 minutes-120 minutes;
C, be cooled to room temperature after having reacted; Then transfer in centrifuge tube and carry out the high speed centrifugation separation, after separating, present the solution of the gel state that contains the high-purity nano copper powder and the upper solution of clarification, collect lower floor's solution, supernatant liquid can be utilized on technique after separating again;
D, the solution that will obtain containing high-purity nano copper is by absolute ethanol washing, and the alcoholic solution that washing will contain Nanometer Copper is for the last time transferred to vacuum rotary evaporator and extracted copper nanoparticle, and adjusting vacuum is 0.08Mpa-0.1Mpa.
Preferably, method step is more specifically: get 45-50 milliliter alkaline etching waste liquid for producing and pack in the centrifuge tube of 2 25 milliliters, carry out centrifugal; Centrifugally the centrifuge tube supernatant liquid is poured in the beaker of 200 milliliters after complete, added 4-6 gram polyvinylpyrrolidone and 4-6 gram softex kw as reactant A solution simultaneously; The NaOH that preparation contains 0.08-0.12 mol/L hydration hydrazine, 0.4-0.6 mol/L gram, the B solution 40-60 milliliter of 0.8-1.2 mol/L polyethylene glycol; B solution is poured in there-necked flask, and the regulating thermostatic bath temperature, at 70-90 ℃, is opened and is stirred, and mixing speed, 150-250 rev/min of left and right, drips A solution in there-necked flask, after having reacted, takes out and is cooled to room temperature; The reaction solution that is cooled to room temperature is poured in the centrifuge tube of 2 50 milliliters and again carried out centrifugation, collect the material of lower floor's gel state in centrifuge tube, upper strata liquid is reclaimed to treat standby to production line; To collect the material absolute ethanol washing that is gel state, washing is transferred to when last in rotation vacuum evaporation instrument and is extracted copper nanoparticle, and control vacuum is 0.08-0.09Mpa.
Preferably, method step is more specifically: get 45-50 milliliter alkaline etching waste liquid for producing and pack in the centrifuge tube of 2 25 milliliters, carry out centrifugal; Centrifugally the centrifuge tube supernatant liquid is poured in the beaker of 200 milliliters after complete, added 7-9 gram polyvinylpyrrolidone and 7-9 gram softex kw as reactant A solution simultaneously; The B solution 45-60 milliliter of the polyethylene glycol of the hydrazine hydrate that preparation contains the 0.3-0.6 mol/L, the NaOH of 0.3-0.6 mol/L, 0.8-1.2 mol/L; B solution is poured in there-necked flask, and the regulating thermostatic bath temperature, at 85-100 ℃, is opened and is stirred, and mixing speed, 180-300 rev/min of left and right, drips A solution in there-necked flask, after having reacted, takes out and is cooled to room temperature; The reaction solution that is cooled to room temperature is poured in the centrifuge tube of 2 50 milliliters and is carried out centrifugation, collects the material of lower floor's gel state in centrifuge tube, and upper strata liquid is reclaimed to treat standby to production line; To collect the material absolute ethanol washing that is gel state, washing is transferred to when last in rotation vacuum evaporation instrument and is extracted copper nanoparticle, and control vacuum is 0.08-0.09Mpa.
Preferably, method step is more specifically: get 90-100 milliliter alkaline etching waste liquid for producing and pack in the centrifuge tube of 2 50 milliliters, carry out centrifugal; Centrifugally the centrifuge tube supernatant liquid is poured in the beaker of 200 milliliters after complete, added 7-10 gram polyvinylpyrrolidone and 7-10 gram softex kw as reactant A solution simultaneously; The NaOH that preparation contains 0.2-0.25 mol/L hydration hydrazine, 0.8-1.5 mol/L gram, the B solution 45-50 milliliter of 1.8-2 mol/L polyethylene glycol; B solution is poured in there-necked flask, and the regulating thermostatic bath temperature, at 80-100 ℃, is opened and is stirred, and mixing speed, 180-250 rev/min of left and right, drips A solution in there-necked flask, after having reacted, takes out and is cooled to room temperature; The reaction solution that is cooled to room temperature is poured in the centrifuge tube of 3 50 milliliters and is carried out centrifugation, collects the material of lower floor's gel state in centrifuge tube, and upper strata liquid is reclaimed to treat standby to production line; To collect the material absolute ethanol washing that is gel state, washing is transferred to when last in rotation vacuum evaporation instrument and is extracted copper nanoparticle, and control vacuum is 0.08-0.09Mpa.
The beneficial effect that the present invention adopts above-mentioned technical solution to reach is:
The process conditions that the present invention adopts are not harsh, and easily operation without large power consumption, can be carried out large-scale production under existence conditions; Through test, the copper nanoparticle purity prepared is high, good dispersion, antioxygenic property are good, and the granular size size is in the 30-100 nanometer; Meet the requirement of " Green Chemistry " in whole preparation process, realized waste water discharge-reducing, the purpose of resources circulation recycling.
The accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates that the present invention prepares copper nanoparticle.
Fig. 2 a and Fig. 2 b are the SEM collection of illustrative plates that the present invention prepares copper nanoparticle.
The specific embodiment
A kind of method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare high-purity nano copper of the present invention, it comprises the steps:
A, get appropriate alkaline etching waste liquid for producing and pack in centrifuge tube and carry out high speed centrifugation, to remove suspended impurity trickle in alkaline etching waste liquid for producing, centrifugal after by centrifuge tube at the middle and upper levels clarified solution transfer in container, add the pH value of ammoniacal liquor regulator solution in the 8-12 scope, to solution, add by the active dispersant of the composite surface of softex kw and polyvinylpyrrolidone simultaneously, its addition be take the alkaline etching waste liquid for producing amount as benchmark, add 0.04 kilogram-0.15 kilogram in the alkaline etching waste liquid for producing of 1 liter, will now obtain solution as reaction A thing;
B, preparation reactant B solution, comprise hydrazine hydrate with reproducibility in B solution, there is alkaline NaOH and Nanometer Copper disperses the promoter polyethylene glycol, the amount concentration that the amount of substance concentration that wherein the amount concentration of hydrazine hydrate is 0.05～0.25 mol/L, NaOH is 0.2-2 mol/L, polyethylene glycol is the 0.5-2 mol/L, solution B is heated to 60 ℃-100 ℃, stirs with 100 rev/mins of-1000 rev/mins of speed simultaneously; Again reactant A is slowly dropped in solution B, drip with relief system reaction 60 minutes-120 minutes;
C, be cooled to room temperature after having reacted; Then transfer in centrifuge tube and carry out the high speed centrifugation separation, after separating, present the solution of the gel state that contains the high-purity nano copper powder and the upper solution of clarification, collect lower floor's solution, supernatant liquid can be utilized on technique after separating again;
D, the solution that will obtain containing high-purity nano copper is by absolute ethanol washing, and the alcoholic solution that washing will contain Nanometer Copper is for the last time transferred to vacuum rotary evaporator and extracted copper nanoparticle, and adjusting vacuum is 0.08Mpa-0.1Mpa.
Prepare the XRD collection of illustrative plates of copper nanoparticle and SEM collection of illustrative plates as shown in Figure 1, Figure 2 shown in a and Fig. 2 b, purity is high, good dispersion.As seen from Figure 1, the copper nanoparticle purity of preparation is high, does not contain other impurity; Fig. 2 illustrates its 10000 times of copper nanoparticles and 30000 times of Electronic Speculum results of preparation, good dispersion, and granular size is in the 30-100 nanometer range.
Below in conjunction with specific embodiment, technical scheme of the present invention is described in further detail.
Get 50 milliliters of alkaline etching waste liquid for producing and pack in the centrifuge tube of 2 25 milliliters, carry out centrifugal; Centrifugally the centrifuge tube supernatant liquid is poured in the beaker of 200 milliliters after complete, added 5 gram polyvinylpyrrolidones and 5 gram softex kws as reactant A solution simultaneously; 50 milliliters of the NaOH that preparation contains 0.1 mol/L hydration hydrazine, 0.5 mol/L gram, the B solution of 1 mol/L polyethylene glycol; B solution is poured in there-necked flask, and the regulating thermostatic bath temperature, at 80 ℃, is opened and is stirred, and mixing speed, 200 rev/mins of left and right, drips A solution in there-necked flask, after having reacted, takes out and is cooled to room temperature; The reaction solution that is cooled to room temperature is poured in the centrifuge tube of 2 50 milliliters and again carried out centrifugation, collect the material of lower floor's gel state in centrifuge tube, upper strata liquid is reclaimed to treat standby to production line; To collect the material absolute ethanol washing that is gel state, washing is transferred to when last in rotation vacuum evaporation instrument and is extracted copper nanoparticle, and control vacuum is 0.08Mpa.
Get 50 milliliters of alkaline etching waste liquid for producing and pack in the centrifuge tube of 2 25 milliliters, carry out centrifugal; Centrifugally the centrifuge tube supernatant liquid is poured in the beaker of 200 milliliters after complete, added 8 gram polyvinylpyrrolidones and 8 gram softex kws as reactant A solution simultaneously; 50 milliliters of the B solution of the polyethylene glycol of the hydrazine hydrate that preparation contains 0.5 mol/L, the NaOH of 0.5 mol/L, 1 mol/L; B solution is poured in there-necked flask, and the regulating thermostatic bath temperature, at 90 ℃, is opened and is stirred, and mixing speed, 200 rev/mins of left and right, drips A solution in there-necked flask, after having reacted, takes out and is cooled to room temperature; The reaction solution that is cooled to room temperature is poured in the centrifuge tube of 2 50 milliliters and is carried out centrifugation, collects the material of lower floor's gel state in centrifuge tube, and upper strata liquid is reclaimed to treat standby to production line; To collect the material absolute ethanol washing that is gel state, washing is transferred to when last in rotation vacuum evaporation instrument and is extracted copper nanoparticle, and control vacuum is 0.08Mpa.
Example 3
Get 100 milliliters of alkaline etching waste liquid for producing and pack in the centrifuge tube of 2 50 milliliters, carry out centrifugal; Centrifugally the centrifuge tube supernatant liquid is poured in the beaker of 200 milliliters after complete, added 8 gram polyvinylpyrrolidones and 8 gram softex kws as reactant A solution simultaneously; 50 milliliters of the NaOH that preparation contains 0.25 mol/L hydration hydrazine, 1.0 mol/L grams, the B solution of 2 mol/L polyethylene glycol; B solution is poured in there-necked flask, and the regulating thermostatic bath temperature, at 90 ℃, is opened and is stirred, and mixing speed, 200 rev/mins of left and right, drips A solution in there-necked flask, after having reacted, takes out and is cooled to room temperature; The reaction solution that is cooled to room temperature is poured in the centrifuge tube of 3 50 milliliters and is carried out centrifugation, collects the material of lower floor's gel state in centrifuge tube, and upper strata liquid is reclaimed to treat standby to production line; To collect the material absolute ethanol washing that is gel state, washing is transferred to when last in rotation vacuum evaporation instrument and is extracted copper nanoparticle, and control vacuum is 0.08Mpa.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, without departing from the concept of the premise of the invention, can also make some distortion and improvement, and these all belong to protection scope of the present invention.
Claims (4)
1. a method of utilizing alkaline etching waste liquid for producing printed circuit board to prepare high-purity nano copper, is characterized in that, it comprises the steps:
A, get appropriate alkaline etching waste liquid for producing and pack in centrifuge tube and carry out high speed centrifugation, centrifugal after by centrifuge tube at the middle and upper levels clarified solution transfer in container, add the pH value of ammoniacal liquor regulator solution in the 8-12 scope, to solution, add by the active dispersant of the composite surface of softex kw and polyvinylpyrrolidone simultaneously, its addition be take the alkaline etching waste liquid for producing amount as benchmark, add 0.04 kilogram-0.15 kilogram in the alkaline etching waste liquid for producing of 1 liter, will now obtain solution as reaction A thing;
B, preparation reactant B solution, comprise hydrazine hydrate with reproducibility in B solution, there is alkaline NaOH and Nanometer Copper disperses the promoter polyethylene glycol, the amount concentration that the amount of substance concentration that wherein the amount concentration of hydrazine hydrate is 0.05～0.25 mol/L, NaOH is 0.2-2 mol/L, polyethylene glycol is the 0.5-2 mol/L, solution B is heated to 60 ℃-100 ℃, stirs with 100 rev/mins of-1000 rev/mins of speed simultaneously; Again reactant A is slowly dropped in solution B, drip with relief system reaction 60 minutes-120 minutes;
C, be cooled to room temperature after having reacted; Then transfer in centrifuge tube and carry out the high speed centrifugation separation, after separating, present the solution of the gel state that contains the high-purity nano copper powder and the upper solution of clarification, collect lower floor's solution;
D, the solution that will obtain containing high-purity nano copper is by absolute ethanol washing, and the alcoholic solution that washing will contain Nanometer Copper is for the last time transferred to vacuum rotary evaporator and extracted copper nanoparticle, and adjusting vacuum is 0.08Mpa-0.1Mpa.
2. the method for utilizing alkaline etching waste liquid for producing printed circuit board to prepare high-purity nano copper according to claim 1, is characterized in that, described method step is specially: get 45-50 milliliter alkaline etching waste liquid for producing and pack in the centrifuge tube of 2 25 milliliters, carry out centrifugal; Centrifugally the centrifuge tube supernatant liquid is poured in the beaker of 200 milliliters after complete, added 4-6 gram polyvinylpyrrolidone and 4-6 gram softex kw as reactant A solution simultaneously; The NaOH that preparation contains 0.08-0.12 mol/L hydration hydrazine, 0.4-0.6 mol/L gram, the B solution 40-60 milliliter of 0.8-1.2 mol/L polyethylene glycol; B solution is poured in there-necked flask, and the regulating thermostatic bath temperature, at 70-90 ℃, is opened and is stirred, and mixing speed, 150-250 rev/min of left and right, drips A solution in there-necked flask, after having reacted, takes out and is cooled to room temperature; The reaction solution that is cooled to room temperature is poured in the centrifuge tube of 2 50 milliliters and again carried out centrifugation, collect the material of lower floor's gel state in centrifuge tube, upper strata liquid is reclaimed to treat standby to production line; To collect the material absolute ethanol washing that is gel state, washing is transferred to when last in rotation vacuum evaporation instrument and is extracted copper nanoparticle, and control vacuum is 0.08-0.09Mpa.
3. the method for utilizing alkaline etching waste liquid for producing printed circuit board to prepare high-purity nano copper according to claim 1, is characterized in that, described method step is specially: get 45-50 milliliter alkaline etching waste liquid for producing and pack in the centrifuge tube of 2 25 milliliters, carry out centrifugal; Centrifugally the centrifuge tube supernatant liquid is poured in the beaker of 200 milliliters after complete, added 7-9 gram polyvinylpyrrolidone and 7-9 gram softex kw as reactant A solution simultaneously; The B solution 45-60 milliliter of the polyethylene glycol of the hydrazine hydrate that preparation contains the 0.3-0.6 mol/L, the NaOH of 0.3-0.6 mol/L, 0.8-1.2 mol/L; B solution is poured in there-necked flask, and the regulating thermostatic bath temperature, at 85-100 ℃, is opened and is stirred, and mixing speed, 180-300 rev/min of left and right, drips A solution in there-necked flask, after having reacted, takes out and is cooled to room temperature; The reaction solution that is cooled to room temperature is poured in the centrifuge tube of 2 50 milliliters and is carried out centrifugation, collects the material of lower floor's gel state in centrifuge tube, and upper strata liquid is reclaimed to treat standby to production line; To collect the material absolute ethanol washing that is gel state, washing is transferred to when last in rotation vacuum evaporation instrument and is extracted copper nanoparticle, and control vacuum is 0.08-0.09Mpa.
4. the method for utilizing alkaline etching waste liquid for producing printed circuit board to prepare high-purity nano copper according to claim 1, it is characterized in that, described method step is specially: method step is more specifically: get 90-100 milliliter alkaline etching waste liquid for producing and pack in the centrifuge tube of 2 50 milliliters, carry out centrifugal; Centrifugally the centrifuge tube supernatant liquid is poured in the beaker of 200 milliliters after complete, added 7-10 gram polyvinylpyrrolidone and 7-10 gram softex kw as reactant A solution simultaneously; The NaOH that preparation contains 0.2-0.25 mol/L hydration hydrazine, 0.8-1.5 mol/L gram, the B solution 45-50 milliliter of 1.8-2 mol/L polyethylene glycol; B solution is poured in there-necked flask, and the regulating thermostatic bath temperature, at 80-100 ℃, is opened and is stirred, and mixing speed, 180-250 rev/min of left and right, drips A solution in there-necked flask, after having reacted, takes out and is cooled to room temperature; The reaction solution that is cooled to room temperature is poured in the centrifuge tube of 3 50 milliliters and is carried out centrifugation, collects the material of lower floor's gel state in centrifuge tube, and upper strata liquid is reclaimed to treat standby to production line; To collect the material absolute ethanol washing that is gel state, washing is transferred to when last in rotation vacuum evaporation instrument and is extracted copper nanoparticle, and control vacuum is 0.08-0.09Mpa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106041122A (en) * | 2016-07-13 | 2016-10-26 | 许勤峰 | Method for preparing nanometre copper-catalyzed slurry by virtue of PCB acidic waste liquid |
| CN106077700A (en) * | 2016-07-13 | 2016-11-09 | 许勤峰 | A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102019430A (en) * | 2009-09-18 | 2011-04-20 | 福建师范大学福清分校 | Method for recovering copper from alkaline etching waste liquid and recycling alkaline etching liquid |
| CN102354571A (en) * | 2011-05-19 | 2012-02-15 | 广东成德电路股份有限公司 | Nano-copper conductive slurry preparation method by utilizing printed circuit board alkaline etching waste liquid |
| CN102557297A (en) * | 2011-12-31 | 2012-07-11 | 重庆重冶铜业有限公司 | Treatment method of waste liquid after cleaning copper plated layer of printed circuit board |
| CN102560500A (en) * | 2012-02-03 | 2012-07-11 | 昆山市洁驰环保科技发展有限公司 | Method for producing nanometer copper powder by use of waste alkaline etching solution which can be regenerated and apparatus thereof |
-
2013
- 2013-09-25 CN CN201310441610.0A patent/CN103480860B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102019430A (en) * | 2009-09-18 | 2011-04-20 | 福建师范大学福清分校 | Method for recovering copper from alkaline etching waste liquid and recycling alkaline etching liquid |
| CN102354571A (en) * | 2011-05-19 | 2012-02-15 | 广东成德电路股份有限公司 | Nano-copper conductive slurry preparation method by utilizing printed circuit board alkaline etching waste liquid |
| CN102557297A (en) * | 2011-12-31 | 2012-07-11 | 重庆重冶铜业有限公司 | Treatment method of waste liquid after cleaning copper plated layer of printed circuit board |
| CN102560500A (en) * | 2012-02-03 | 2012-07-11 | 昆山市洁驰环保科技发展有限公司 | Method for producing nanometer copper powder by use of waste alkaline etching solution which can be regenerated and apparatus thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106041122A (en) * | 2016-07-13 | 2016-10-26 | 许勤峰 | Method for preparing nanometre copper-catalyzed slurry by virtue of PCB acidic waste liquid |
| CN106077700A (en) * | 2016-07-13 | 2016-11-09 | 许勤峰 | A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry |
| 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 |
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| CN103480860B (en) | 2016-01-06 |
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