CN106835216A - Without cyanogen, it is without phosphorus, without aminoform gold plating bath and its preparation and electroplating technology - Google Patents
Without cyanogen, it is without phosphorus, without aminoform gold plating bath and its preparation and electroplating technology Download PDFInfo
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- CN106835216A CN106835216A CN201710156908.5A CN201710156908A CN106835216A CN 106835216 A CN106835216 A CN 106835216A CN 201710156908 A CN201710156908 A CN 201710156908A CN 106835216 A CN106835216 A CN 106835216A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/58—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of copper
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Abstract
The invention discloses one kind without cyanogen, it is without phosphorus, without aminoform gold plating bath and its preparation and electroplating technology, the electroplating surface processing technology field of category metal or on-metallic article.The present invention with copper sulphate, zinc sulfate and sodium stannate be main salt, be the complexing agent of metal cation in main salt with main complexant and auxiliary complexing agent, be the brightener and dispersant of imitation gold plating liquid with boric acid as the PH buffers of imitation gold plating liquid, with potassium hydroxide as the PH conditioning agents of imitation gold plating liquid, with bright property dispersant.The made imitation gold plating liquid of the present invention is without to the composition such as human body and the harmful potassium cyanide (sodium) of environment, phosphorus (phosphine), fluorine, free inorganic ammonia (amine) and nitrogen, and using the present invention prepare without cyanogen, process condition wide ranges without phosphorus, that imitation gold plating is carried out without aminoform gold plating bath, easy to operate, the imitative layer gold color stability of gained, and can be realized from the change between rose gold 16K, 18K to 24K with the change of operating condition.
Description
Technical field
The present invention relates to metal or the electroplating surface processing technology field of on-metallic article, it is more particularly to a kind of without cyanogen,
It is without phosphorus, without aminoform gold plating bath, the invention further relates to it is this without cyanogen, preparation without phosphorus, without aminoform gold plating bath and electroplating technology.
Background technology
In metal or nonmetallic technical field of surface, there is a kind of very important electroplating technology technology --- electricity
Plating imitation gold process.It can plate out one layer like 12-24K gold in metal and nonmetallic surface, and be actually non-gold dollar
The alloy layer of element.This alloy-layer is, using the principle of electrochemical deposition, the Cu-Zn alloys of binary to be electroplated out in product surface
Or the Cu-Zn-Sn alloy-layers of ternary, can be by changing the temperature of plating solution, or the cathode-current density implemented, or adjustment operation
Time, obtain the alloy layer of the different colours such as roseate 16K gold, 18K gold or even proof gold.
Imitation gold deposit is widely used for hardware, furniture, lamp decoration, case and bag, clock and watch, sound equipment, building materials, indoor and outdoor advertisement, trick
The aspects such as board, jewellery, there is performance and security performance that proof gold is irreplaceable, excellent, with low cost.
At present in ripe gold simulating electroplating process, plating solution is still mostly cyanide bath, and it has stabilization and basic unit's coating
The advantages of coating blond shades that adhesion is good, obtain are more true to nature, but cyanide bath toxicity is big, contaminated wastewater environment is serious,
Influence the health of operating personnel, the industry of this and China and Economic development direction grave fault.
Nineteen seventies begin, and China has started the research and development that cyanideless electro-plating imitates gold, and its technology is also more early than external, progress
Also than state extra income.The bath system that cyanideless electro-plating imitates gold mainly has pyrophosphate, tartaric acid (salt), 1-hydroxy ethylidene-1,1-diphosphonic acid
And ethylenediamine (HEDP).In addition to above-mentioned main complexant, in plating solution also containing inorganic hypophosphites, ammonium sulfate, ammonium chloride,
Fluorination (hydrogen) ammonium etc..But, the gold that above-mentioned bath system has the imitative layer gold of less stable, gained is less true to nature, discharge
The shortcomings of in water containing the big phosphorus of chemical oxygen consumption (COC) (phosphine), fluorine, ammonia (amine), and above-mentioned bath system technology is still immature, behaviour
Make condition, such as current density, temperature, time scope is too narrow, be difficult to grasp, therefore, many factories will be from the end of the year of twentieth century 80
Since again recovered cyanide the Imitating Gold Electroplating Technology one after another.
The content of the invention
There is problem it is an object of the invention to overcome above-mentioned prior art, there is provided it is a kind of it is brand-new without cyanogen, it is without phosphorus, without ammonia
Imitation gold plating liquid and its preparation and electroplating technology, the present invention prepare imitation gold plating liquid without potassium cyanide (sodium), not phosphorous (phosphine),
It is not fluorine-containing, without free inorganic ammonia (amine) and nitrogen, and present invention process operating condition wide ranges, easy to operate, the imitative gold of gained
Layer color stability, and can be realized from the change between rose gold 16K, 18K to 24K with the change of operating condition.
To achieve the above object, the present invention is adopted the following technical scheme that：
Without cyanogen, it is without phosphorus, without aminoform gold plating bath, every liter of solution contains following components：
Copper sulphate (CuSO45H2O)：20~25g/L,
Zinc sulfate (ZnSO47H2O)：30~40g/L,
Sodium stannate (42%Na2SnO3)：0~8g/L,
Boric acid (H3BO3)：20~30g/L,
Main complexant：80~100g/L.
Auxiliary complexing agent：8~10g/L,
Potassium hydroxide (KOH)：80~110g/L,
Bright property dispersant：16~20mL/L.
As the present invention without cyanogen, a kind of preferred scheme without phosphorus, without aminoform gold plating bath, the main complexant is lemon
Acid, auxiliary complexing agent are succimide.
As the present invention without cyanogen, another preferred scheme without phosphorus, without aminoform gold plating bath, every liter of bright property dispersion
Agent includes following components；
Ethyoxyl butynediols：160~170g/L,
Nicotinic acid：60~70g/L,
Potassium hydroxide：30~50g/L,
Saccharin：40~60g/L,
ALS：40~50g/L.
Prepare it is above-mentioned without cyanogen, technique without phosphorus, without aminoform gold plating bath, comprise the following steps：
1) boric acid is dissolved in the hot distilled water that temperature is 50~60 DEG C, is subsequently adding main complexant, stirring to dissolving
Completely；
2) to step 1) obtained in auxiliary complexing agent is added in solution, stirring is complete to dissolving；
3) to step 2) obtained in copper sulphate is added in solution, stirring is complete to dissolving；
4) to step 3) obtained in zinc sulfate is added in solution, stirring is complete to dissolving；
5) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is complete to dissolving, after cooling, under agitation, by institute's hydrogen manufacturing
Potassium oxide solution is added to step 4) in made solution, you can binary Cn-Zn it is initial without cyanogen, it is without phosphorus, without ammonia imitation gold plating
Liquid；
6) to step 5) made binary Cn-Zn it is initial without cyanogen, it is without phosphorus, without adding bright property dispersion in aminoform gold plating bath
Agent and normal-temperature distilled water, stir, stand 12~24h, you can binary Cn-Zn without cyanogen, it is without phosphorus, without aminoform gold plating bath.
Prepare it is above-mentioned without cyanogen, technique without phosphorus, without aminoform gold plating bath, comprise the following steps：
1) boric acid is dissolved in temperature in 50~60 DEG C of hot distilled waters, to be subsequently adding main complexant, stirring is to having dissolved
Entirely；
2) to step 1) obtained in auxiliary complexing agent is added in solution, stirring is complete to dissolving；
3) to step 2) obtained in copper sulphate is added in solution, stirring is complete to dissolving；
4) to step 3) obtained in zinc sulfate is added in solution, stirring is complete to dissolving；
5) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is complete to dissolving, after cooling, under agitation, by institute's hydrogen manufacturing
Potassium oxide solution is added to step 4) in made solution；
6) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is complete to dissolving, then, under agitation, to the hydrogen of dissolving
Sodium stannate is marginally repeatedly added in potassium oxide solution, completely and after removing impurity, under agitation, is added to after sodium stannate dissolving
Step 5) in made solution, you can ternary Cn-Zn-Sn it is initial without cyanogen, it is without phosphorus, without aminoform gold plating bath；
7) to step 6) made ternary Cn-Zn-Sn adds bright property dispersant in imitating the initial plating solution of gold, and supplement normal temperature
Distilled water, stirs, stand 12~24h, you can ternary Cn-Zn-Sn without cyanogen, it is without phosphorus, without aminoform gold plating bath.
Using it is above-mentioned without cyanogen, it is without phosphorus, plating piece imitation gold plating, wherein the technique bar of imitation gold plating are carried out without aminoform gold plating bath
Part is：
PH value：8.5~10.0,
Cathode-current density：0.25~1.0A/dm2,
Bath temperature：50~58 DEG C,
Electroplating time：30~180s,
Anode：Cu-Zn plates.
Used without cyanogen, a kind of preferred scheme without phosphorus, that plating piece imitation gold plating is carried out without aminoform gold plating bath as the present invention,
Cu contents are that 75%~80%, Zn contents are 20%~25% in the Cu-Zn plates.
The invention has the advantages that：
1st, during the present invention is with copper sulphate, zinc sulfate and sodium stannate as main salt, with main complexant and auxiliary complexing agent as main salt
The complexing agent of metal cation, with boric acid as the PH buffers of imitation gold plating liquid, with potassium hydroxide be the PH of imitation gold plating liquid adjust
Save agent, be the brightener and dispersant of imitation gold plating liquid with bright property dispersant so that made imitation gold plating liquid is free of to human body
The compositions such as the potassium cyanide (sodium), phosphorus (phosphine), fluorine, free inorganic ammonia (amine) and the nitrogen that are harmful to environment.
2nd, the present invention can realize as needed binary Cn-Zn without cyanogen, it is without phosphorus, without aminoform gold plating bath and ternary Cn-Zn-Sn
Without cyanogen, preparation without phosphorus, without aminoform gold plating bath, preparation process is simple, it is easy to industrialized production.
3rd, using present invention preparation without cyanogen, process condition without phosphorus, that imitation gold plating is carried out without aminoform gold plating bath
Wide ranges, easy to operate, the imitative layer gold color stability of gained, and can with operating condition change realize from rose gold 16K, 18K to
Change between 24K.
Specific embodiment
In order to be better understood from the present invention, the present invention is further described below by embodiment, embodiment is only used
In the present invention is explained, any restriction is not constituted to the present invention.
Table 1 be the embodiment of the present invention 1~3 using without the nontoxic imitation gold plating complexant of cyanogen prepare without cyanogen, it is without phosphorus, without aminoform gold
Each composition proportion of electroplate liquid.
Table 1
Table 2 is matched somebody with somebody for above-described embodiment 1~3 without cyanogen, each composition without phosphorus, without bright property dispersant in aminoform gold plating bath
Than.
Table 2
| Embodiment | Ethyoxyl butynediols/(g/L) | Nicotinic acid/(g/L) | Potassium hydroxide/(g/L) | Saccharin/(g/L) | ALS/(g/L) |
| Embodiment 1 | 160 | 60 | 30 | 40 | 40 |
| Embodiment 2 | 165 | 65 | 40 | 50 | 45 |
| Embodiment 3 | 170 | 70 | 50 | 60 | 50 |
Embodiment 1
Prepare without cyanogen, it is without phosphorus, without aminoform gold plating bath, comprise the following steps：
1) container of 1000mL is taken, 20g boric acid is dissolved in the 500mL hot distilled waters that temperature is 50~60 DEG C,
80g citric acids are subsequently adding, stirring is complete to dissolving；
2) to step 1) obtained in 8g succimides are added in solution, stirring is complete to dissolving；
3) to step 2) obtained in 20g copper sulphate is added in solution, stirring is complete to dissolving；
4) to step 3) obtained in 30g zinc sulfate is added in solution, stirring is complete to dissolving；
5) a container separately is taken, 80g potassium hydroxide is dissolved in the normal-temperature distilled water of 300mL, stirring is complete to dissolving, cold
But after, under agitation, made potassium hydroxide solution is added to step 4) in made solution, you can binary Cn-Zn is initial
Without cyanogen, it is without phosphorus, without aminoform gold plating bath；
6) to step 5) made binary Cn-Zn it is initial without cyanogen, it is without phosphorus, without adding 16mL bright properties in aminoform gold plating bath
Dispersant, and normal-temperature distilled water is supplemented to 1000mL, stir, stand 12~24h, you can obtain binary Cn-Zn without cyanogen, nothing
Phosphorus, without aminoform gold plating bath；
Using above-mentioned binary Cn-Zn without cyanogen, it is without phosphorus, imitation gold plating, the technique of imitation gold plating are carried out without aminoform gold plating bath
Condition is：PH value：8.5, cathode-current density：0.25A/dm2, bath temperature：50 DEG C, electroplating time：30s, anode：(75%)
Cu- (25%) Zn plates.
Embodiment 2
Prepare it is above-mentioned without cyanogen, it is without phosphorus, without aminoform gold plating bath, comprise the following steps：
1) container of 1000mL is taken, 25g boric acid is dissolved in the 500mL hot distilled waters that temperature is 50~60 DEG C,
90g citric acids are subsequently adding, stirring is complete to dissolving；
2) to step 1) obtained in 9g succimides are added in solution, stirring is complete to dissolving；
3) to step 2) obtained in 22.5g copper sulphate is added in solution, stirring is complete to dissolving；
4) to step 3) obtained in 35g zinc sulfate is added in solution, stirring is complete to dissolving；
5) a container separately is taken, 90g potassium hydroxide is dissolved in the normal-temperature distilled water of 300mL, stirring is complete to dissolving, cold
But after, under agitation, made potassium hydroxide solution is added to step 4) in made solution；
6) a container separately is taken, 20g potassium hydroxide is dissolved in the normal-temperature distilled water of 180mL, stirring is complete to dissolving, so
Afterwards, under agitation, to 6g sodium stannates are repeatedly marginally added in the potassium hydroxide solution of dissolving, treat sodium stannate dissolving completely and go
After falling impurity, under agitation, be added to step 5) in made solution, you can ternary Cn-Zn-Sn is initial without cyanogen, without phosphorus, nothing
Aminoform gold plating bath；
7) to step 6) made ternary Cn-Zn-Sn it is initial without cyanogen, it is without phosphorus, without adding 18mL light in aminoform gold plating bath
Bright property dispersant, and supplement normal-temperature distilled water to 1000mL, stirs, and stands 12~24h, you can ternary Cn-Zn-Sn without
Cyanogen, it is without phosphorus, without aminoform gold plating bath.
Using above-mentioned ternary Cn-Zn-Sn without cyanogen, it is without phosphorus, imitation gold plating, the work of imitation gold plating are carried out without aminoform gold plating bath
Skill condition is：PH value：9, cathode-current density：0.5A/dm2, 55 DEG C of bath temperature, electroplating time：90s, anode：(78%)
Cu- (22%) Zn plates.
Embodiment 3
Prepare it is above-mentioned without cyanogen, it is without phosphorus, without aminoform gold plating bath, comprise the following steps：
1) container of 1000mL is taken, 30g boric acid is dissolved in the 500mL hot distilled waters that temperature is 50~60 DEG C,
100g citric acids are subsequently adding, stirring is complete to dissolving；
2) to step 1) obtained in 10g succimides are added in solution, stirring is complete to dissolving；
3) to step 2) obtained in 25g copper sulphate is added in solution, stirring is complete to dissolving；
4) to step 3) obtained in 40g zinc sulfate is added in solution, stirring is complete to dissolving；
5) a container separately is taken, 85g potassium hydroxide is dissolved in the normal-temperature distilled water of 300mL, stirring is complete to dissolving, cold
But after, under agitation, made potassium hydroxide solution is added to step 4) in made solution；
6) a container separately is taken, 25g potassium hydroxide is dissolved in the normal-temperature distilled water of 180mL, stirring is complete to dissolving, so
Afterwards, under agitation, to 8g sodium stannates are repeatedly marginally added in the potassium hydroxide solution of dissolving, treat sodium stannate dissolving completely and go
After falling impurity, under agitation, be added to step 5) in made solution, you can ternary Cn-Zn-Sn is initial without cyanogen, without phosphorus, nothing
Aminoform gold plating bath；
7) to step 6) made ternary Cn-Zn-Sn adds 20mL bright property dispersants in imitating the initial plating solution of gold, and supplement
Normal-temperature distilled water stirs to 1000mL, stand 12~24h, you can ternary Cn-Zn-Sn without cyanogen, it is without phosphorus, without aminoform gold
Electroplate liquid.
Using above-mentioned ternary Cn-Zn-Sn without cyanogen, it is without phosphorus, imitation gold plating, the work of imitation gold plating are carried out without aminoform gold plating bath
Skill condition is：PH value：10, cathode-current density：1.0A/dm2, 58 DEG C of bath temperature, electroplating time：180s, anode：(80%)
Cu- (20%) Zn plates.
Claims (7)
1. without cyanogen, it is without phosphorus, without aminoform gold plating bath, it is characterised in that：Every liter of solution contains following components：
Copper sulphate：20~25g/L,
Zinc sulfate：30~40g/L,
Sodium stannate：0~8g/L,
Boric acid：20~30g/L,
Main complexant：80~100g/L,
Auxiliary complexing agent：8~10g/L,
Potassium hydroxide：80~110g/L,
Bright property dispersant：16~20mL/L.
2. it is according to claim 1 without cyanogen, it is without phosphorus, without aminoform gold plating bath, it is characterised in that：The main complexant is lemon
Lemon acid, auxiliary complexing agent are succimide.
3. it is according to claim 1 without cyanogen, it is without phosphorus, without aminoform gold plating bath, it is characterised in that：Every liter of bright property point
Powder includes following components；
Ethyoxyl butynediols：160~170g/L,
Nicotinic acid：60~70g/L,
Potassium hydroxide：30~50g/L,
Saccharin：40~60g/L,
ALS：40~50g/L.
4. prepare claim 1 or 2 or 3 described in without cyanogen, technique without phosphorus, without aminoform gold plating bath, it is characterised in that：Including
Following steps：
1) boric acid is dissolved in the hot distilled water that temperature is 50~60 DEG C, is subsequently adding main complexant, stirring is complete to dissolving；
2) to step 1) obtained in auxiliary complexing agent is added in solution, stirring is complete to dissolving；
3) to step 2) obtained in copper sulphate is added in solution, stirring is complete to dissolving；
4) to step 3) obtained in zinc sulfate is added in solution, stirring is complete to dissolving；
5) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is complete to dissolving, after cooling, under agitation, by made hydroxide
Potassium solution is added to step 4) in made solution, you can binary Cn-Zn it is initial without cyanogen, it is without phosphorus, without aminoform gold plating bath；
6) to step 5) made binary Cn-Zn it is initial without cyanogen, it is without phosphorus, without adding bright property dispersant in aminoform gold plating bath,
And supplement normal-temperature distilled water, stir, stand 12~24h, you can binary Cn-Zn without cyanogen, it is without phosphorus, without ammonia imitation gold plating
Liquid.
5. prepare claim 1 or 2 or 3 described in without cyanogen, technique without phosphorus, without aminoform gold plating bath, it is characterised in that：Including
Following steps：
1) boric acid is dissolved in the hot distilled water that temperature is 50~60 DEG C, is subsequently adding main complexant, stirring is complete to dissolving；
2) to step 1) obtained in auxiliary complexing agent is added in solution, stirring is complete to dissolving；
3) to step 2) obtained in copper sulphate is added in solution, stirring is complete to dissolving；
4) to step 3) obtained in zinc sulfate is added in solution, stirring is complete to dissolving；
5) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is complete to dissolving, after cooling, under agitation, by made hydroxide
Potassium solution is added to step 4) in made solution；
6) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is complete to dissolving, then, under agitation, to the hydroxide of dissolving
Sodium stannate is marginally repeatedly added in potassium solution, completely and after removing impurity, under agitation, step is added to after sodium stannate dissolving
5) in made solution, you can ternary Cn-Zn-Sn it is initial without cyanogen, it is without phosphorus, without aminoform gold plating bath；
7) to step 6) made ternary Cn-Zn-Sn it is initial without cyanogen, it is without phosphorus, without adding bright property dispersion in aminoform gold plating bath
Agent and normal-temperature distilled water, stir, stand 12~24h, you can ternary Cn-Zn-Sn without cyanogen, it is without phosphorus, without ammonia imitation gold plating
Liquid.
6. using described in claim 1 without cyanogen, it is without phosphorus, carry out plating piece imitation gold plating without aminoform gold plating bath, it is characterised in that：
The process conditions of imitation gold plating are：
PH value：8.5~10.0,
Cathode-current density：0.25~1.0A/dm2,
Bath temperature：50~58 DEG C,
Electroplating time：30~180s,
Anode：Cu-Zn plates.
It is 7. according to claim 6 to use without cyanogen, technique without phosphorus, that plating piece imitation gold plating is carried out without aminoform gold plating bath,
It is characterized in that：Cu contents are that 75%~80%, Zn contents are 20%~25% in the positive C u-Zn plates.
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|---|---|---|---|
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Cited By (1)
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| CN106894063A (en) * | 2017-03-17 | 2017-06-27 | 湖北吉和昌化工科技有限公司 | Without cyanogen, nontoxic imitation gold plating complexant and without cyanogen, it is without phosphorus, without aminoform gold plating bath |
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| CN106835216B (en) | 2018-11-30 |
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