CN106637160A - Regeneration method of chemical plating NiWP solution - Google Patents
Regeneration method of chemical plating NiWP solution Download PDFInfo
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- CN106637160A CN106637160A CN201710003260.8A CN201710003260A CN106637160A CN 106637160 A CN106637160 A CN 106637160A CN 201710003260 A CN201710003260 A CN 201710003260A CN 106637160 A CN106637160 A CN 106637160A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1617—Purification and regeneration of coating baths
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Chemically Coating (AREA)
Abstract
The invention discloses a regeneration method of a chemical plating NiWP solution. The regeneration method comprises the following steps: (1) a preparation process; (2) an electrolysis process; (3) a cooling and crystallization process. According to the regeneration method, hypophosphite ions in the chemical plating NiWP plating solution are oxidized into phosphate ions through an electrolysis method, and the solubility of sodium phosphate is smaller than that of sodium hypophosphite and thus sodium phosphate is easier to remove; meanwhile, heavy metal ions, such as Pb<2+> (which is commonly used as a stabilizer in the chemical plating solution), in the plating solution are removed through electrolytic deposition, so that the aim of purifying the plating solution is realized; phosphate, sulfate and sodium ions are removed through freezing and wastes are changed into valuable things; the utilization period of the chemical plating NiWP solution is prolonged and the production cost is reduced.
Description
Technical field
The present invention relates to a kind of surface chemical plating field, specifically a kind of renovation process of Electroless Plating Ni WP solution.
Background technology
Electroless Plating Ni WP coating has more excellent corrosion resistance and wearability, and nearest 10 years, the country disclosed nearly 20
The Electroless Plating Ni WP patented technology of item, but usage cycles are not long, and chemical plating fluid can not regenerate, and limit its technology
Application.
The composition of Electroless Plating Ni WP plating solution has：1. nickel sulfate and sodium tungstate, provide respectively nickel and wolfram element；2. reducing agent is
Sodium hypophosphite, while providing P elements；3. complexing agent selects sodium citrate, some addition sodium gluconates, sodium lactate etc. to act on
Auxiliary complex-former；4. stabilizer, accelerator are from thiocarbamide, fluorine ion, Potassiumiodate etc.；5. ammoniacal liquor or NaOH adjust plating solution
pH。
Nickel sulfate, sodium tungstate, sodium hypophosphite and NaOH are continually added in plating process（Ammoniacal liquor）, deposit NiWP
Coating, so as to cause solution in sulfate ion, sodium ion, ammonium ion and hypophosphorous acid root oxidation product orthophosphite product
Tired, and the catabolite of organic matter, wherein orthophosphite ions accumulating rate is most fast.How effectively to remove in solution this
The product of accumulation, especially orthophosphite ions, are the keys of Electroless Plating Ni WP solution regeneration.
The regeneration of existing chemical nickel plating phosphor bath has：1. chemical precipitation method, such as a kind of acid chemical plating nickel solution are again
Generation method（Application number CN93104747.1）, by adding calcium acetate or calcium chloride, make orthophosphite ions and calcium binding
And there is precipitation reaction, remove the orthophosphite ions of accumulation；2. freezing, the such as regeneration treating method of chemical nickel-plating liquid（Shen
Please number CN200610034390.X）, directly used chemical nickel plating phosphorus solution is reduced to into 1-5 DEG C, separate out sodium sulphate and Asia
Phosphoric acid sodium crystal；3. electroosmose process, such as a kind of method and apparatus that body lotion is deposited by Ion-exchange chemical plating metal（Application
Number CN99806806.3, CN201010149324.3）, in the presence of electricity, make orthophosphite through pellicle to anode direction
Mobile, sodium ion to cathode direction is moved, and reaches the purpose of removal；4. solvent extraction, such as a kind of solvent extraction-ion
The method that exchange process processes the dense waste liquid of chemical nickel plating（Application number CN201510290426.X）.Industrially, conventional is the first
Method.
But, the solubility of artificial schellite is suitable with Arizona bacilli solubility, all in 0.002g/100g water or so, so by adding
Entering the compound of calcium ion also can make artificial schellite coprecipitation out, tungsten it is expensive, so necessarily causing cost significantly to rise
It is high；Other methods, price itself is all high, along with the interference of tungstate radicle, so bringing for the regeneration of Electroless Plating Ni WP plating solution
Just seem very improper.Therefore the patent information and paper information in terms of Electroless Plating Ni WP solution regeneration is had not seen.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the renovation process of Electroless Plating Ni WP solution, to solve background
Problem present in technology.
For achieving the above object, the present invention provides following technical scheme：
A kind of renovation process of Electroless Plating Ni WP solution, comprises the following steps：
（1）Preparatory technology：Weigh sodium tungstate 55-65 g, sodium citrate 75-85g, sodium hypophosphite 15-25g, boric acid 15-25g, two
Ammonium methyl borine 2-7g, adds 5-7L pure water, while stirring heated solution, and heating-up temperature is 50-55 DEG C, subsequently adds nickel sulfate
15-25g and stirring and dissolving, being subsequently added into NaOH carries out the regulation of pH, until pH is adjusted to 7.0 ± 0.2, adds 3-5L water to determine
Hold, subsequently carry out Electroless Plating Ni WP, when the quality of coating for plating out reaches 40 ± 2g, carry out next link；
（2）Electrolysis process：Using stainless steel as positive electrode, iron plate is negative electrode, and current density is controlled in 2- during electrolysis
5A/dm2, the electricity that electrolysis time control passes through in 8-12h, and every liter of electroplate liquid is 40-60Ah, until plating liquor face
Color becomes colorless and pH is changed into 0.9；
（3）Cooling and crystallizing process：Now -5-0 DEG C will be cooled to for electroplate liquid, start crystallization, until separating out crystal reaches 50-65g/
L, detection crystalline component is aqueous phosphoric acid sodium crystal；NaOH is subsequently added into until supernatant pH is in the range of 7-10, to incite somebody to action
Temperature is promoted to 10-15 DEG C, continues 5-10min, and low temperature is cooled to again, and cryogenic temperature is controlled at 0-8 DEG C, starts crystallization, directly
55-65g/L is reached to crystal is separated out, detection crystalline component is aqueous sodium sulfate crystal；Supplement after second crystallisation by cooling steady
Determine agent and brightener, that is, realize the regeneration technology of Electroless Plating Ni WP solution.
As further scheme of the invention：Step（1）In weigh sodium tungstate 57-63g, sodium citrate 78-82g, secondary phosphorus
Sour sodium 18-21g, boric acid 16-23g, Dimethyl Ammonium borine 3-6g adds 5L pure water, while stirring heated solution, and heating-up temperature is
51-54 DEG C, subsequently add nickel sulfate 18-22g and stirring and dissolving.
As further scheme of the invention：Step（1）Middle step（1）In weigh sodium tungstate 60g, sodium citrate 80g, it is secondary
Sodium phosphate 20g, boric acid 20g, Dimethyl Ammonium borine 5g adds 6L pure water, while stirring heated solution, and heating-up temperature is 53 DEG C,
Subsequently add nickel sulfate 20g and stirring and dissolving.
As further scheme of the invention：Step（1）Middle addition 4L water constant volumes.
As further scheme of the invention：Step（2）Current density is controlled in 3.5A/dm during middle electrolysis2, electrolysis time
The electricity that control passes through in 10h, and every liter of electroplate liquid is 50Ah.
As further scheme of the invention：Step（3）In now will cool to -2.5 DEG C for electroplate liquid, start crystallization, directly
55g/L is reached to crystal is separated out, detection crystalline component is aqueous phosphoric acid sodium crystal.
As further scheme of the invention：Step（3）In be subsequently added into NaOH until supernatant pH be 9 scopes
It is interior, temperature is promoted to into 13 DEG C, continue 8min.
As further scheme of the invention：Step（3）In be cooled to low temperature again, cryogenic temperature is controlled at 4 DEG C, is started
Crystallization, until separating out crystal reaches 60g/L, detection crystalline component is aqueous sodium sulfate crystal.
Compared with prior art, the invention has the beneficial effects as follows：
The present invention is oxidized to phosphate anion, phosphoric acid by the method being electrolysed the orthophosphite ions in Electroless Plating Ni WP plating solution
The solubility of sodium is less than sodium phosphite, so easily remove, while the heavy metal ion in plating solution, such as Pb2+ is (conventional
Make the stabilizer in chemical plating fluid), electro-deposition is removed, and reaches the purpose of purification plating solution, then removes phosphate radical, sulfuric acid by freezing
Root and sodium ion, turn waste into wealth, and improve Electroless Plating Ni WP solution usage cycles, reduce production cost.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of renovation process of Electroless Plating Ni WP solution, comprises the following steps：
（1）Preparatory technology：Weigh the g of sodium tungstate 55, sodium citrate 75g, sodium hypophosphite 15g, boric acid 15g, Dimethyl Ammonium borine
2g, adds 5L pure water, while stirring heated solution, and heating-up temperature is 50 DEG C, and subsequently addition nickel sulfate 15g and stirring and dissolving, connect
The regulation for adding NaOH to carry out pH, until pH is adjusted to 7.0 ± 0.2,3L water constant volumes is added, chemical plating is subsequently carried out
NiWP, when the quality of coating for plating out reaches 40 ± 2g, carries out next link；
（2）Electrolysis process：Using stainless steel as positive electrode, iron plate is negative electrode, and current density is controlled in 2A/ during electrolysis
dm2, the electricity that electrolysis time control passes through in 8h, and every liter of electroplate liquid is 40Ah, until electroplate liquid solution colour is changed into nothing
Color and pH is changed into 0.9；
（3）Cooling and crystallizing process：Now -5 DEG C will be cooled to for electroplate liquid, start crystallization, until separating out crystal reaches 50g/L, be examined
It is aqueous phosphoric acid sodium crystal to survey crystalline component；It is in the range of 7, temperature to be lifted that NaOH is subsequently added into up to supernatant pH
To 10 DEG C, continue 5min, low temperature is cooled to again, cryogenic temperature is controlled at 0 DEG C, starts crystallization, until separate out crystal reaching
55g/L, detection crystalline component is aqueous sodium sulfate crystal；Stabilizer and brightener are supplemented after second crystallisation by cooling, i.e., in fact
The regeneration technology of existing Electroless Plating Ni WP solution.
Embodiment 2
A kind of renovation process of Electroless Plating Ni WP solution, comprises the following steps：
（1）Preparatory technology：Weigh sodium tungstate 55-65 g, sodium citrate 75-85g, sodium hypophosphite 15-25g, boric acid 15-25g, two
Ammonium methyl borine 2-7g, adds 5-7L pure water, while stirring heated solution, and heating-up temperature is 50-55 DEG C, subsequently adds nickel sulfate
15-25g and stirring and dissolving, being subsequently added into NaOH carries out the regulation of pH, until pH is adjusted to 7.0 ± 0.2, adds 3-5L water to determine
Hold, subsequently carry out Electroless Plating Ni WP, when the quality of coating for plating out reaches 40 ± 2g, carry out next link；
（2）Electrolysis process：Using stainless steel as positive electrode, iron plate is negative electrode, and current density is controlled in 2- during electrolysis
5A/dm2, the electricity that electrolysis time control passes through in 8-12h, and every liter of electroplate liquid is 40-60Ah, until plating liquor face
Color becomes colorless and pH is changed into 0.9；
（3）Cooling and crystallizing process：Now -5-0 DEG C will be cooled to for electroplate liquid, start crystallization, until separating out crystal reaches 50-65g/
L, detection crystalline component is aqueous phosphoric acid sodium crystal；NaOH is subsequently added into until supernatant pH is in the range of 7-10, to incite somebody to action
Temperature is promoted to 10-15 DEG C, continues 5-10min, and low temperature is cooled to again, and cryogenic temperature is controlled at 0-8 DEG C, starts crystallization, directly
55-65g/L is reached to crystal is separated out, detection crystalline component is aqueous sodium sulfate crystal；Supplement after second crystallisation by cooling steady
Determine agent and brightener, that is, realize the regeneration technology of Electroless Plating Ni WP solution.
As further scheme of the invention：Step（1）In weigh sodium tungstate 57g, sodium citrate 78g, sodium hypophosphite
18g, boric acid 16g, Dimethyl Ammonium borine 3g adds 5L pure water, while stirring heated solution, and heating-up temperature is 51 DEG C, is subsequently added
Plus nickel sulfate 18 and stirring and dissolving.
As further scheme of the invention：Step（1）Middle addition 4L water constant volumes.
As further scheme of the invention：Step（2）Current density is controlled in 3.5A/dm during middle electrolysis2, electrolysis time
The electricity that control passes through in 10h, and every liter of electroplate liquid is 50Ah.
As further scheme of the invention：Step（3）In now will cool to -2.5 DEG C for electroplate liquid, start crystallization, directly
55g/L is reached to crystal is separated out, detection crystalline component is aqueous phosphoric acid sodium crystal.
As further scheme of the invention：Step（3）In be subsequently added into NaOH until supernatant pH be 9 scopes
It is interior, temperature is promoted to into 13 DEG C, continue 8min.
As further scheme of the invention：Step（3）In be cooled to low temperature again, cryogenic temperature is controlled at 4 DEG C, is started
Crystallization, until separating out crystal reaches 60g/L, detection crystalline component is aqueous sodium sulfate crystal.
Embodiment 3
A kind of renovation process of Electroless Plating Ni WP solution, comprises the following steps：
（1）Preparatory technology：Weigh sodium tungstate 55-65 g, sodium citrate 75-85g, sodium hypophosphite 15-25g, boric acid 15-25g, two
Ammonium methyl borine 2-7g, adds 5-7L pure water, while stirring heated solution, and heating-up temperature is 50-55 DEG C, subsequently adds nickel sulfate
15-25g and stirring and dissolving, being subsequently added into NaOH carries out the regulation of pH, until pH is adjusted to 7.0 ± 0.2, adds 3-5L water to determine
Hold, subsequently carry out Electroless Plating Ni WP, when the quality of coating for plating out reaches 40 ± 2g, carry out next link；
（2）Electrolysis process：Using stainless steel as positive electrode, iron plate is negative electrode, and current density is controlled in 2- during electrolysis
5A/dm2, the electricity that electrolysis time control passes through in 8-12h, and every liter of electroplate liquid is 40-60Ah, until plating liquor face
Color becomes colorless and pH is changed into 0.9；
（3）Cooling and crystallizing process：Now -5-0 DEG C will be cooled to for electroplate liquid, start crystallization, until separating out crystal reaches 50-65g/
L, detection crystalline component is aqueous phosphoric acid sodium crystal；NaOH is subsequently added into until supernatant pH is in the range of 7-10, to incite somebody to action
Temperature is promoted to 10-15 DEG C, continues 5-10min, and low temperature is cooled to again, and cryogenic temperature is controlled at 0-8 DEG C, starts crystallization, directly
55-65g/L is reached to crystal is separated out, detection crystalline component is aqueous sodium sulfate crystal；Supplement after second crystallisation by cooling steady
Determine agent and brightener, that is, realize the regeneration technology of Electroless Plating Ni WP solution.
As further scheme of the invention：Step（1）Middle step（1）In weigh sodium tungstate 60g, sodium citrate 80g, it is secondary
Sodium phosphate 20g, boric acid 20g, Dimethyl Ammonium borine 5g adds 6L pure water, while stirring heated solution, and heating-up temperature is 53 DEG C,
Subsequently add nickel sulfate 20g and stirring and dissolving.
As further scheme of the invention：Step（1）Middle addition 4L water constant volumes.
As further scheme of the invention：Step（2）Current density is controlled in 3.5A/dm during middle electrolysis2, electrolysis time
The electricity that control passes through in 10h, and every liter of electroplate liquid is 50Ah.
As further scheme of the invention：Step（3）In now will cool to -2.5 DEG C for electroplate liquid, start crystallization, directly
55g/L is reached to crystal is separated out, detection crystalline component is aqueous phosphoric acid sodium crystal.
As further scheme of the invention：Step（3）In be subsequently added into NaOH until supernatant pH be 9 scopes
It is interior, temperature is promoted to into 13 DEG C, continue 8min.
As further scheme of the invention：Step（3）In be cooled to low temperature again, cryogenic temperature is controlled at 4 DEG C, is started
Crystallization, until separating out crystal reaches 60g/L, detection crystalline component is aqueous sodium sulfate crystal.
Embodiment 4
A kind of renovation process of Electroless Plating Ni WP solution, comprises the following steps：
（1）Preparatory technology：Weigh sodium tungstate 55-65 g, sodium citrate 75-85g, sodium hypophosphite 15-25g, boric acid 15-25g, two
Ammonium methyl borine 2-7g, adds 5-7L pure water, while stirring heated solution, and heating-up temperature is 50-55 DEG C, subsequently adds nickel sulfate
15-25g and stirring and dissolving, being subsequently added into NaOH carries out the regulation of pH, until pH is adjusted to 7.0 ± 0.2, adds 3-5L water to determine
Hold, subsequently carry out Electroless Plating Ni WP, when the quality of coating for plating out reaches 40 ± 2g, carry out next link；
（2）Electrolysis process：Using stainless steel as positive electrode, iron plate is negative electrode, and current density is controlled in 2- during electrolysis
5A/dm2, the electricity that electrolysis time control passes through in 8-12h, and every liter of electroplate liquid is 40-60Ah, until plating liquor face
Color becomes colorless and pH is changed into 0.9；
（3）Cooling and crystallizing process：Now -5-0 DEG C will be cooled to for electroplate liquid, start crystallization, until separating out crystal reaches 50-65g/
L, detection crystalline component is aqueous phosphoric acid sodium crystal；NaOH is subsequently added into until supernatant pH is in the range of 7-10, to incite somebody to action
Temperature is promoted to 10-15 DEG C, continues 5-10min, and low temperature is cooled to again, and cryogenic temperature is controlled at 0-8 DEG C, starts crystallization, directly
55-65g/L is reached to crystal is separated out, detection crystalline component is aqueous sodium sulfate crystal；Supplement after second crystallisation by cooling steady
Determine agent and brightener, that is, realize the regeneration technology of Electroless Plating Ni WP solution.
As further scheme of the invention：Step（1）In weigh sodium tungstate 63g, sodium citrate 82g, sodium hypophosphite
21g, boric acid 23g, Dimethyl Ammonium borine 6g adds 5L pure water, while stirring heated solution, and heating-up temperature is 54 DEG C, is subsequently added
Plus nickel sulfate 22g and stirring and dissolving.
As further scheme of the invention：Step（1）Middle addition 4L water constant volumes.
As further scheme of the invention：Step（2）Current density is controlled in 3.5A/dm during middle electrolysis2, electrolysis time
The electricity that control passes through in 10h, and every liter of electroplate liquid is 50Ah.
As further scheme of the invention：Step（3）In now will cool to -2.5 DEG C for electroplate liquid, start crystallization, directly
55g/L is reached to crystal is separated out, detection crystalline component is aqueous phosphoric acid sodium crystal.
As further scheme of the invention：Step（3）In be subsequently added into NaOH until supernatant pH be 9 scopes
It is interior, temperature is promoted to into 13 DEG C, continue 8min.
As further scheme of the invention：Step（3）In be cooled to low temperature again, cryogenic temperature is controlled at 4 DEG C, is started
Crystallization, until separating out crystal reaches 60g/L, detection crystalline component is aqueous sodium sulfate crystal.
Embodiment 5
A kind of renovation process of Electroless Plating Ni WP solution, comprises the following steps：
（1）Preparatory technology：Weigh the g of sodium tungstate 65, sodium citrate 85g, sodium hypophosphite 25g, boric acid 25g, Dimethyl Ammonium borine
7g, adds 7L pure water, while stirring heated solution, and heating-up temperature is 55 DEG C, and subsequently addition nickel sulfate 25g and stirring and dissolving, connect
The regulation for adding NaOH to carry out pH, until pH is adjusted to 7.0 ± 0.2,5L water constant volumes is added, chemical plating is subsequently carried out
NiWP, when the quality of coating for plating out reaches 40 ± 2g, carries out next link；
（2）Electrolysis process：Using stainless steel as positive electrode, iron plate is negative electrode, and current density is controlled in 5A/ during electrolysis
dm2, the electricity that electrolysis time control passes through in 12h, and every liter of electroplate liquid is 60Ah, until electroplate liquid solution colour is changed into nothing
Color and pH is changed into 0.9；
（3）Cooling and crystallizing process：Now 0 DEG C will be cooled to for electroplate liquid, start crystallization, until separating out crystal reaches 65g/L, be detected
Crystalline component is aqueous phosphoric acid sodium crystal；It is in the range of 10, temperature to be lifted that NaOH is subsequently added into up to supernatant pH
To 15 DEG C, continue 10min, low temperature is cooled to again, cryogenic temperature is controlled at 8 DEG C, starts crystallization, until separate out crystal reaching
65g/L, detection crystalline component is aqueous sodium sulfate crystal；Stabilizer and brightener are supplemented after second crystallisation by cooling, i.e., in fact
The regeneration technology of existing Electroless Plating Ni WP solution.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be in other specific forms realized.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity those skilled in the art should
Using specification as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form those skilled in the art
Understandable other embodiment.
Claims (8)
1. a kind of renovation process of Electroless Plating Ni WP solution, it is characterised in that comprise the following steps：
（1）Preparatory technology：Weigh sodium tungstate 55-65 g, sodium citrate 75-85g, sodium hypophosphite 15-25g, boric acid 15-25g, two
Ammonium methyl borine 2-7g, adds 5-7L pure water, while stirring heated solution, and heating-up temperature is 50-55 DEG C, subsequently adds nickel sulfate
15-25g and stirring and dissolving, being subsequently added into NaOH carries out the regulation of pH, until pH is adjusted to 7.0 ± 0.2, adds 3-5L water to determine
Hold, subsequently carry out Electroless Plating Ni WP, when the quality of coating for plating out reaches 40 ± 2g, carry out next link；
（2）Electrolysis process：Using stainless steel as positive electrode, iron plate is negative electrode, and current density is controlled in 2- during electrolysis
5A/dm2, the electricity that electrolysis time control passes through in 8-12h, and every liter of electroplate liquid is 40-60Ah, until plating liquor face
Color becomes colorless and pH is changed into 0.9；
（3）Cooling and crystallizing process：Now -5-0 DEG C will be cooled to for electroplate liquid, start crystallization, until separating out crystal reaches 50-65g/
L, detection crystalline component is aqueous phosphoric acid sodium crystal；NaOH is subsequently added into until supernatant pH is in the range of 7-10, to incite somebody to action
Temperature is promoted to 10-15 DEG C, continues 5-10min, and low temperature is cooled to again, and cryogenic temperature is controlled at 0-8 DEG C, starts crystallization, directly
55-65g/L is reached to crystal is separated out, detection crystalline component is aqueous sodium sulfate crystal；Supplement after second crystallisation by cooling steady
Determine agent and brightener, that is, realize the regeneration technology of Electroless Plating Ni WP solution.
2. the renovation process of Electroless Plating Ni WP solution according to claim 1, it is characterised in that step（1）In weigh tungsten
Sour sodium 57-63g, sodium citrate 78-82g, sodium hypophosphite 18-21g, boric acid 16-23g, Dimethyl Ammonium borine 3-6g adds 5L pure
Water, heated solution while stirring, heating-up temperature is 51-54 DEG C, subsequently addition nickel sulfate 18-22g and stirring and dissolving.
3. the renovation process of Electroless Plating Ni WP solution according to claim 1, it is characterised in that step（1）Middle step（1）
In weigh sodium tungstate 60g, sodium citrate 80g, sodium hypophosphite 20g, boric acid 20g, Dimethyl Ammonium borine 5g adds 6L pure water, side
Stirring side heated solution, heating-up temperature is 53 DEG C, subsequently addition nickel sulfate 20g and stirring and dissolving.
4. the renovation process of Electroless Plating Ni WP solution according to claim 3, it is characterised in that step（1）Middle addition 4L
Water constant volume.
5. the renovation process of Electroless Plating Ni WP solution according to claim 1, it is characterised in that step（2）During middle electrolysis
Current density is controlled in 3.5A/dm2, the electricity that electrolysis time control passes through in 10h, and every liter of electroplate liquid is 50Ah.
6. the renovation process of Electroless Plating Ni WP solution according to claim 1, it is characterised in that step（3）In will now
Electroplate liquid cools to -2.5 DEG C, starts crystallization, until separating out crystal reaches 55g/L, detection crystalline component is aqueous sodium phosphate
Crystal.
7. the renovation process of Electroless Plating Ni WP solution according to claim 1, it is characterised in that step（3）In then plus
It is in the range of 9, temperature to be promoted to into 13 DEG C to enter NaOH up to supernatant pH, continues 8min.
8. the renovation process of Electroless Plating Ni WP solution according to claim 1, it is characterised in that step（3）In it is cold again
But to low temperature, cryogenic temperature is controlled at 4 DEG C, starts crystallization, until separating out crystal reaches 60g/L, detection crystalline component is aqueous
Sodium sulfate crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710003260.8A CN106637160A (en) | 2017-01-04 | 2017-01-04 | Regeneration method of chemical plating NiWP solution |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710003260.8A CN106637160A (en) | 2017-01-04 | 2017-01-04 | Regeneration method of chemical plating NiWP solution |
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| CN (1) | CN106637160A (en) |
Cited By (1)
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