CN109913914A - The control method of copper ion concentration in a kind of cyanide-free copper electroplating solution - Google Patents
The control method of copper ion concentration in a kind of cyanide-free copper electroplating solution Download PDFInfo
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- CN109913914A CN109913914A CN201910124588.4A CN201910124588A CN109913914A CN 109913914 A CN109913914 A CN 109913914A CN 201910124588 A CN201910124588 A CN 201910124588A CN 109913914 A CN109913914 A CN 109913914A
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- Prior art keywords
- copper
- cyanide
- resin
- electroplating solution
- ion concentration
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 84
- 239000010949 copper Substances 0.000 title claims abstract description 84
- 238000009713 electroplating Methods 0.000 title claims abstract description 64
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910001431 copper ion Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 61
- 229920005989 resin Polymers 0.000 claims abstract description 61
- 238000007747 plating Methods 0.000 claims abstract description 30
- 238000005342 ion exchange Methods 0.000 claims abstract description 26
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 230000008929 regeneration Effects 0.000 claims abstract description 12
- 238000011069 regeneration method Methods 0.000 claims abstract description 12
- 230000001172 regenerating effect Effects 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims description 7
- 229940116318 copper carbonate Drugs 0.000 claims description 6
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 claims description 6
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical group [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- 239000008235 industrial water Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 230000000630 rising effect Effects 0.000 abstract description 3
- 229910001297 Zn alloy Inorganic materials 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241000969106 Megalaima haemacephala Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052927 chalcanthite Inorganic materials 0.000 description 1
- ZFXTZKMYLJXJDY-UHFFFAOYSA-N copper;oxalonitrile Chemical compound [Cu].N#CC#N ZFXTZKMYLJXJDY-UHFFFAOYSA-N 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000004064 dysfunction Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention discloses a kind of control methods of copper ion concentration in cyanide-free copper electroplating solution, include the following steps: that cyanide-free copper electroplating solution, which 1) is pumped into resin container with certain flow rate, with pump carries out ion exchange, while the copper plating solution after exchange is returned to by coating bath by resin container outlet；2) it circulates 2-4 hours, after resin sufficiently exchanges saturation, stops copper plating solution being pumped into resin container, remaining copper plating solution is discharged in resin container to coating bath；3) then resin is regenerated, the resin regeneration time is 1-4 hours；4) resin after regenerating continues to carry out ion exchange to cyanide-free copper electroplating solution, is recycled.The present invention can effectively solve the problem that the copper ion concentration in cyanide-free copper electroplating solution continues the problem of slowly rising；The copper ion concentration in cyanide-free copper electroplating solution can accurately be controlled within the scope of optimality criterion, promote electroplating quality.
Description
Technical field
The present invention relates to a kind of control methods of copper ion concentration in cyanide-free copper electroplating solution.
Background technique
At present in the electroplating technology of kirsite, the overwhelming majority still uses backward cyanide strike copper plating technique at present, due to
Containing hypertoxic cyanide in plating solution, so that the backwardness technique will gradually be eliminated.Exploitation plates coppersmith using new environmental non-cyanide
Skill is an urgent demand of development.
The existing without phosphorus strike copper plating technique of zinc alloy cyanide-free, remaining copper ion concentration in the plating solution in process of production can delay
Slow the problem of rising, reason is: the solid copper anode in 1. coating baths is soaked among solution, under unpowered state due to
Slow chemolysis can also occur for the effect of air stirring, generate copper ion；Even if 2. in energized state, the electric current of anode and cathode
Efficiency is also not quite identical, and the copper dissolution speed of anode is slightly above the copper deposition speed of cathode.If copper ion concentration exceeds work
The critical field of skill, it will cause the risk of Zinc alloy electroplating dysfunction.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide copper ion concentrations in a kind of cyanide-free copper electroplating solution
Control method.
The present invention is achieved through the following technical solutions:
The control method of copper ion concentration, includes the following steps: in a kind of cyanide-free copper electroplating solution
1) cyanide-free copper electroplating solution is pumped into resin container with certain flow rate with pump and carries out ion exchange, while gone out by resin container
Copper plating solution after exchange is returned to coating bath by mouth；
2) it circulates 2-4 hours, after resin sufficiently exchanges saturation, stops copper plating solution being pumped into resin container, be discharged
Remaining copper plating solution is to coating bath in resin container；
3) then resin is regenerated, the resin regeneration time is 1-4 hours；
4) resin after regenerating continues to carry out ion exchange to cyanide-free copper electroplating solution, is recycled.
Preferably, the ion exchange in step 1) is with the copper ion in the hydrogen ion exchange plating solution on resin.
Preferably, the pH range of the cyanide-free copper electroplating solution in step 1) is 3.0-12.0.
Preferably, its volume-exchange capacity >=04mmol/mL for being directed to copper ion of the ion exchange in step 1).
Preferably, resin container is set up directly on plating trough rim in step 1), can carry out online processing to cyanide-free copper electroplating solution, no
Production line is influenced to operate normally.
Preferably, when carrying out regeneration treatment to resin in step 3), the actified solution of selection is that volume ratio is 1%-25%
Sulfuric acid solution or 1%-20% hydrochloric acid solution.
Preferably, the resin in step 4) after sulfuric acid solution regenerates continues directly to carry out ion friendship to cyanide-free copper electroplating solution
It changes.
Preferably, if the copper ion concentration in step 1) after ion-exchange treatment in cyanide-free copper electroplating solution is lower than a certain range
When, the mantoquita of required quality can be directly added in cyanide-free copper electroplating solution.
Preferably, the mantoquita is at least one of copper sulphate, copper chloride, copper nitrate, basic copper carbonate, copper carbonate.
Preferably, the copper ions solution that resin container is discharged after step 3) regeneration is by industrial water treatment plant together with copper system waste water
Handle or be individually recycled.
Copper ion concentration in cyanide-free copper electroplating solution can be efficiently solved the invention has the following beneficial effects: this method to hold
It is continuous slowly to rise, exceed the problem of critical field, it is in copper ion concentration in cyanide-free copper electroplating solution in optimum range always, it should
Method directly can carry out efficient online processing to the cyanide-free copper electroplating solution that pH range is 3.0-12.0, do not influence production line and normally give birth to
Produce operation；It can effectively solve the problem that the copper ion concentration in cyanide-free copper electroplating solution continues the problem of slowly rising；It can accurately control
Copper ion concentration in cyanide-free copper electroplating solution promotes electroplating quality within the scope of optimality criterion.
Detailed description of the invention
It, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical solution of the present invention
The attached drawing used is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, right
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings
Its attached drawing.
Fig. 1 is flow chart of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, carries out to the technical solution in inventive embodiments clear, complete
Ground description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, those of ordinary skill in the art's every other reality obtained without making creative work
Example is applied, shall fall within the protection scope of the present invention.
Reference book attached drawing 1, cyanide-free copper electroplating solution trough rim be equipped with a resin container, with pump by cyanide-free copper electroplating solution with
Certain flow rate is pumped into resin container and carries out ion exchange, while resin is exported by tank the copper plating solution after exchange returning to coating bath, is followed
Circulation is 2-4 hours dynamic, after resin sufficiently exchanges saturation, stops for copper plating solution being pumped into resin container, is discharged remaining in resin container
Plating solution is to the coating bath, and then carrying out regeneration 1-4 hours to resin, (the copper ions solution that resin container is discharged after regeneration can be by work
Industry water treatment plant is handled together with copper system waste water, can also be individually recycled), the resin after regeneration can continue to no cyanogen
Copper plating solution carries out ion exchange, is recycled.If the copper ion concentration after ion-exchange treatment in cyanide-free copper electroplating solution is lower than
A certain range can directly add the mantoquita of required quality in cyanide-free copper electroplating solution.
Ion exchange wherein is carried out to cyanide-free copper electroplating solution using resin, with the copper in the hydrogen ion exchange plating solution on resin
Ion can effectively reduce the copper ion concentration in plating solution, while not introduce other impurities ion；Using resin to non-cyanide plating
Ion exchange is carried out in copper solution, without being adjusted, the pH of cyanide-free copper electroplating solution may range from the pH of cyanide-free copper electroplating solution
3.0-12.0；Resin model used be D401, D402, D403, D463, TP207, TP208, TP260, CH-90, CR-11,
One kind or two kinds of HCD-101, HCD-105, LSC-100, LSC-500, IRC-747, IRC-748 combination of the above；Use resin
Ion exchange is carried out to cyanide-free copper electroplating solution, is directed to volume-exchange capacity >=0.4mmol/mL of copper ion, i.e., with 200L's
The cyanide-free copper electroplating solution of resin treatment 10000L, circulation primary effectively can at least reduce the copper ion concentration in cyanide-free copper electroplating solution
0.508g/L converts as CuSO4·5H2O is at least 2.0g/L；Ion exchange is carried out to cyanide-free copper electroplating solution using resin, it can be with
Resin container device is installed additional in plating trough rim and realizes online circulation, other are carried out to cyanide-free copper electroplating solution without stopping electroplating assembly line
Processing, does not influence the normal production run of plating line；When carrying out regeneration treatment to resin, the actified solution of selection is that volume ratio is
The sulfuric acid solution or 1%-20% hydrochloric acid solution of 1%-25%；Resin after sulfuric acid solution regenerates can be continued directly to non-cyanide plating
Copper solution carries out ion exchange, does not need made the transition again (such as sodium form, potassium type), shortens the reproduction time, while avoiding other
Accumulation (such as sodium ion, potassium ion) of the ion in cyanide-free copper electroplating solution；Ion friendship is carried out to cyanide-free copper electroplating solution using resin
It changes, it, can be directly in non-cyanide plating if the copper ion concentration after ion-exchange treatment in cyanide-free copper electroplating solution is lower than control critical field
Add the mantoquita of required quality in copper solution, mantoquita be copper sulphate, copper chloride, copper nitrate, basic copper carbonate, in copper carbonate extremely
Few one kind.
One embodiment of the present of invention is described below:
1. configuring the resin container that a volume is 250L in the zinc alloy cyanide-free copper facing trough rim of 10000L, it is provided with 200L's
TP208 resin, pH=8.50, the copper ion concentration 10.0g/L of cyanide-free copper electroplating solution in coating bath；
2. cyanide-free copper electroplating solution, which is evacuated to resin container, with 50L/min flow velocity with pump carries out ion exchange, while resin container
Outlet is connected to groove body, recycles 4 hours；
3. stopping circulation, the cyanide-free copper electroplating solution in resin container is flow back into groove body, is analyzed in coating bath in cyanide-free copper electroplating solution
Copper ion concentration, be reduced to 9.45g/L；
4. the sulfuric acid solution for being 20% with volumetric concentration carries out regeneration 2 hours to the resin in resin container, thereafter let out again
Raw solution；
5. repeating step 2, the copper ion concentration in coating bath in cyanide-free copper electroplating solution is analyzed, 8.9g/L is reduced to.
The accurate control of copper ion concentration in zinc alloy cyanide-free copper plating solution can be achieved in the present invention, avoids because cyanide-free copper electroplating is molten
Copper ion concentration persistently rises and influences the electroplating quality of zinc alloy workpiece in liquid, effectively promotion process rate.
The preferred embodiment of the present invention has shown and described in above description, as previously described, it should be understood that the present invention is not office
Be limited to form disclosed herein, should not be regarded as an exclusion of other examples, and can be used for various other combinations, modification and
Environment, and can be changed within that scope of the inventive concept describe herein by the above teachings or related fields of technology or knowledge
It is dynamic.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be appended by the present invention
In scope of protection of the claims.
Claims (10)
1. the control method of copper ion concentration in a kind of cyanide-free copper electroplating solution, which comprises the steps of:
1) cyanide-free copper electroplating solution is pumped into resin container with certain flow rate with pump and carries out ion exchange, while being exported by resin container will
Copper plating solution after exchange returns to coating bath；
2) it circulates 2-4 hours, after resin sufficiently exchanges saturation, stops for copper plating solution being pumped into resin container, resin is discharged
Remaining copper plating solution is to coating bath in tank；
3) then resin is regenerated, the resin regeneration time is 1-4 hours；
4) resin after regenerating continues to carry out ion exchange to cyanide-free copper electroplating solution, is recycled.
2. the control method of copper ion concentration in cyanide-free copper electroplating solution according to claim 1, which is characterized in that step 1)
In ion exchange be on resin hydrogen ion exchange plating solution in copper ion.
3. the control method of copper ion concentration in cyanide-free copper electroplating solution according to claim 1, which is characterized in that step 1)
In cyanide-free copper electroplating solution pH range be 3.0-12.0.
4. the control method of copper ion concentration in a kind of cyanide-free copper electroplating solution according to claim 1, which is characterized in that step
It is rapid 1) in ion exchange its be directed to copper ion volume-exchange capacity >=0.4mmol/mL.
5. the control method of copper ion concentration in cyanide-free copper electroplating solution according to claim 1, which is characterized in that step 1)
Middle resin container is set up directly on plating trough rim.
6. the control method of copper ion concentration in cyanide-free copper electroplating solution according to claim 1, which is characterized in that step 3)
In to resin carry out regeneration treatment when, the actified solution of selection is the sulfuric acid solution that volume ratio is 1%-25% or 1%-20% salt
Acid solution.
7. the control method of copper ion concentration in a kind of cyanide-free copper electroplating solution according to claim 6, which is characterized in that step
It is rapid 4) in resin after sulfuric acid solution regenerates continue directly to carry out ion exchange to cyanide-free copper electroplating solution.
8. the control method of copper ion concentration in a kind of cyanide-free copper electroplating solution according to claim 1, which is characterized in that step
If it is rapid 1) in copper ion concentration after ion-exchange treatment in cyanide-free copper electroplating solution when being lower than a certain range, can be directly in non-cyanide plating
The mantoquita of required quality is added in copper solution.
9. the control method of copper ion concentration in a kind of cyanide-free copper electroplating solution according to claim 8, which is characterized in that institute
Stating mantoquita is at least one of copper sulphate, copper chloride, copper nitrate, basic copper carbonate, copper carbonate.
10. the control method of copper ion concentration in a kind of cyanide-free copper electroplating solution according to claim 1, which is characterized in that
The copper ions solution that resin container is discharged after step 3) regeneration is carried out processing or single by industrial water treatment plant together with copper system waste water
Solely it is recycled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910124588.4A CN109913914A (en) | 2019-02-19 | 2019-02-19 | The control method of copper ion concentration in a kind of cyanide-free copper electroplating solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910124588.4A CN109913914A (en) | 2019-02-19 | 2019-02-19 | The control method of copper ion concentration in a kind of cyanide-free copper electroplating solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109913914A true CN109913914A (en) | 2019-06-21 |
Family
ID=66961697
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910124588.4A Pending CN109913914A (en) | 2019-02-19 | 2019-02-19 | The control method of copper ion concentration in a kind of cyanide-free copper electroplating solution |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186876A (en) * | 1996-12-30 | 1998-07-08 | 中国环境科学研究院 | One-step process of resin regeneration and chromium reduction for reclaiming chromium from electroplating waste water |
| CN103241803A (en) * | 2013-05-14 | 2013-08-14 | 广东新大禹环境工程有限公司 | Electroplating wastewater separating process |
| CN103917691A (en) * | 2011-11-30 | 2014-07-09 | 不二商事株式会社 | Method for regenerating plating liquid, plating method, and plating apparatus |
| CN103938260A (en) * | 2014-05-13 | 2014-07-23 | 洛阳伟信电子科技有限公司 | Method for regenerating copper-containing plating solution |
| CN104418408A (en) * | 2013-08-30 | 2015-03-18 | 上海轻工业研究所有限公司 | Copper-electroplating wastewater treatment method and copper-electroplating wastewater treatment equipment |
-
2019
- 2019-02-19 CN CN201910124588.4A patent/CN109913914A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186876A (en) * | 1996-12-30 | 1998-07-08 | 中国环境科学研究院 | One-step process of resin regeneration and chromium reduction for reclaiming chromium from electroplating waste water |
| CN103917691A (en) * | 2011-11-30 | 2014-07-09 | 不二商事株式会社 | Method for regenerating plating liquid, plating method, and plating apparatus |
| CN103241803A (en) * | 2013-05-14 | 2013-08-14 | 广东新大禹环境工程有限公司 | Electroplating wastewater separating process |
| CN104418408A (en) * | 2013-08-30 | 2015-03-18 | 上海轻工业研究所有限公司 | Copper-electroplating wastewater treatment method and copper-electroplating wastewater treatment equipment |
| CN103938260A (en) * | 2014-05-13 | 2014-07-23 | 洛阳伟信电子科技有限公司 | Method for regenerating copper-containing plating solution |
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Application publication date: 20190621 |
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