CN106835216B - 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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- CN106835216B CN106835216B CN201710156908.5A CN201710156908A CN106835216B CN 106835216 B CN106835216 B CN 106835216B CN 201710156908 A CN201710156908 A CN 201710156908A CN 106835216 B CN106835216 B CN 106835216B
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- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention discloses a kind of no cyanogen, it is without phosphorus, without aminoform gold plating bath and its preparation and electroplating technology, belong to the electroplating surface processing technology field of metal or on-metallic article.The present invention using copper sulphate, zinc sulfate and sodium stannate as main salt, using main complexant and auxiliary complexing agent as the complexing agent of metal cation in main salt, using boric acid as the PH buffer of imitation gold plating liquid, using potassium hydroxide as the PH regulator of imitation gold plating liquid, using bright property dispersing agent as the brightener of imitation gold plating liquid and dispersing agent.The made imitation gold plating liquid of the present invention is free of to the ingredients such as human body and the harmful potassium cyanide of environment (sodium), phosphorus (phosphine), fluorine, free inorganic ammonia (amine) and nitrogen, and it is wide, easy to operate using no cyanogen prepared by the present invention, without phosphorus, without aminoform gold plating bath progress imitation gold plating process condition range, resulting imitative layer gold color stability, and can realize with the change of operating condition from the variation between rose gold 16K, 18K to 24K.
Description
Technical field
The present invention relates to the electroplating surface processing technology field of metal or on-metallic article, more particularly to a kind of no cyanogen,
It is without phosphorus, without aminoform gold plating bath, the invention further relates to this no cyanogen, without phosphorus, without aminoform gold plating bath preparation and electroplating technologies.
Background technique
In metal or nonmetallic technical field of surface, there is a kind of very important electroplating technology technology --- electricity
Plate 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 the principle using electrochemical deposition, and the Cu-Zn alloy of binary is electroplated out in product surface
Or the Cu-Zn-Sn alloy-layer of ternary, the temperature of change plating solution, or the cathode-current density of implementation, or adjustment operation can be passed through
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, luggage, clock and watch, sound equipment, building materials, indoor and outdoor advertisement, recruits
Board, jewellery etc. have irreplaceable, excellent, the low-cost performance of proof gold and security performance.
At present in mature gold simulating electroplating process, plating solution is still cyanide bath mostly, has stable and base's coating
The advantages that coating blond shades that binding force is good, obtains are more true to nature, but cyanide bath toxicity is big, contaminated wastewater environment is serious,
The health of operator is influenced, the industrial and Economic development direction grave fault of this and China.
Nineteen seventies begin, and China has started the research and development that cyanideless electro-plating imitates gold, and 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
(HEDP) and ethylenediamine.Other than above-mentioned main complexant, in plating solution also containing inorganic hypophosphites, ammonium sulfate, ammonium chloride,
It is fluorinated (hydrogen) ammonium etc..But there is less stable in above-mentioned bath system, gained imitates the golden less true to nature, discharge of layer gold
The disadvantages 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 range are too narrow, are not easy to grasp, therefore, many factories will be from the end of the year 80 of twentieth century
Since restored cyanide the Imitating Gold Electroplating Technology one after another again.
Summary of the invention
It is an object of the invention to overcome the problems, such as that the above-mentioned prior art exists, provide it is a kind of completely new without cyanogen, it is without phosphorus, without ammonia
Imitation gold plating liquid and its preparation and electroplating technology, imitation gold plating liquid prepared by the present invention 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 range is wide, easy to operate, resulting imitative gold
Layer color stability, and can realize with the change of operating condition from the variation between rose gold 16K, 18K to 24K.
To achieve the above object, the present invention adopts 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 dispersing agent：16~20mL/L.
As the present invention without cyanogen, a kind of without phosphorus, without aminoform gold plating bath preferred embodiment, the main complexant is lemon
Acid, auxiliary complexing agent are succimide.
As the present invention without cyanogen, without phosphorus, without aminoform gold plating bath another preferred embodiment, every liter of bright property dispersion
Agent includes following components；
Ethyoxyl butynediols：160~170g/L,
Niacin：60~70g/L,
Potassium hydroxide：30~50g/L,
Saccharin：40~60g/L,
Sodium Allyl Sulfonate：40~50g/L.
Above-mentioned no cyanogen, without phosphorus, without aminoform gold plating bath technique are prepared, is included the following steps：
1) boric acid is dissolved in the hot distilled water that temperature is 50~60 DEG C, main complexant, stirring to dissolution is then added
Completely；
2) auxiliary complexing agent is added into solution made from step 1), stirring is complete to dissolving；
3) copper sulphate is added into solution made from step 2), stirring is complete to dissolving；
4) zinc sulfate is added into solution made from step 3), stirring is complete to dissolving；
5) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is to dissolving completely, after cooling, under stiring, by institute's hydrogen manufacturing
Potassium oxide solution is added in the made solution of step 4), can obtain binary Cn-Zn initially without cyanogen, it is without phosphorus, without ammonia imitation gold plating
Liquid；
6) to the made binary Cn-Zn of step 5) initially without cyanogen, it is without phosphorus, without in aminoform gold plating bath be added bright property dispersion
Agent and normal-temperature distilled water, stir evenly, stand 12~for 24 hours, can obtain binary Cn-Zn without cyanogen, it is without phosphorus, without aminoform gold plating bath.
Above-mentioned no cyanogen, without phosphorus, without aminoform gold plating bath technique are prepared, is included the following steps：
1) boric acid is dissolved in temperature is that main complexant is then added in 50~60 DEG C of hot distilled waters, and stirring is to having dissolved
Entirely；
2) auxiliary complexing agent is added into solution made from step 1), stirring is complete to dissolving；
3) copper sulphate is added into solution made from step 2), stirring is complete to dissolving；
4) zinc sulfate is added into solution made from step 3), stirring is complete to dissolving；
5) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is to dissolving completely, after cooling, under stiring, by institute's hydrogen manufacturing
Potassium oxide solution is added in the made solution of step 4)；
6) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is complete to dissolving, then, under stiring, to the hydrogen of dissolution
Sodium stannate is marginally repeatedly added in potassium oxide solution, completely and after removing impurity, under stiring, is added to after sodium stannate dissolution
In the made solution of step 5), can obtain ternary Cn-Zn-Sn initially without cyanogen, it is without phosphorus, without aminoform gold plating bath；
7) bright property dispersing agent is added into the initial plating solution of the imitative gold of the made ternary Cn-Zn-Sn of step 6), and supplements room temperature
Distilled water stirs evenly, stand 12~for 24 hours, can obtain ternary Cn-Zn-Sn without cyanogen, it is without phosphorus, without aminoform gold plating bath.
Using above-mentioned no cyanogen, it is without phosphorus, carry out plating piece imitation gold plating, wherein the technique item of imitation gold plating 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 plate.
As the present invention using no cyanogen, it is without phosphorus, without aminoform gold plating bath progress plating piece imitation gold plating a kind of preferred embodiment,
It is 20%~25% that Cu content, which is 75%~80%, Zn content, in the Cu-Zn plate.
The invention has the advantages that：
1, the present invention using copper sulphate, zinc sulfate and sodium stannate as main salt, using main complexant and auxiliary complexing agent as main salt in
The complexing agent of metal cation, using boric acid as the PH buffer of imitation gold plating liquid, using potassium hydroxide as the PH tune of imitation gold plating liquid
Agent is saved, using bright property dispersing agent as the brightener of imitation gold plating liquid and dispersing agent, so that made imitation gold plating liquid is free of to human body
The ingredients such as potassium cyanide (sodium) harmful with environment, phosphorus (phosphine), fluorine, free inorganic ammonia (amine) and nitrogen.
2, 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, without phosphorus, without aminoform gold plating bath preparation, preparation process is simple, easy to industrialized production.
3, using no cyanogen prepared by the present invention, process condition that is without phosphorus, carrying out imitation gold plating without aminoform gold plating bath
Range is wide, easy to operate, resulting imitative layer gold color stability, and can with the change of operating condition realize from rose gold 16K, 18K to
Variation between 24K.
Specific embodiment
In order to better understand the present invention, below by embodiment, invention is further explained, and embodiment is only used
In explaining the present invention, any restriction is not constituted to the present invention.
Table 1 is the embodiment of the present invention 1~3 using the preparation of no cyanogen nontoxic imitation gold plating complexant without cyanogen, without phosphorus, golden without aminoform
Each composition proportion of electroplate liquid.
Table 1
Table 2 is that above-described embodiment 1~3 is matched without cyanogen, without phosphorus, without bright property dispersing agent in aminoform gold plating bath each ingredient
Than.
Table 2
| Embodiment | Ethyoxyl butynediols/(g/L) | Niacin/(g/L) | Potassium hydroxide/(g/L) | Saccharin/(g/L) | Sodium Allyl Sulfonate/(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
Preparation without cyanogen, it is without phosphorus, without aminoform gold plating bath, include the following steps：
1) 20g boric acid is dissolved in the 500mL hot distilled water that temperature is 50~60 DEG C by the container for taking a 1000mL,
Then 80g citric acid is added, stirring is complete to dissolving；
2) 8g succimide is added into solution made from step 1), stirring is complete to dissolving；
3) 20g copper sulphate is added into solution made from step 2), stirring is complete to dissolving；
4) 30g zinc sulfate is added into solution made from step 3), 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 stiring, made potassium hydroxide solution is added in the made solution of step 4), it is initial that binary Cn-Zn can be obtained
Without cyanogen, it is without phosphorus, without aminoform gold plating bath；
6) to the made binary Cn-Zn of step 5) initially without cyanogen, it is without phosphorus, without in aminoform gold plating bath be added 16mL bright property
Dispersing agent, and supplement normal-temperature distilled water to 1000mL, stirs evenly, stand 12~for 24 hours, binary Cn-Zn can be obtained without cyanogen, nothing
Phosphorus, without aminoform gold plating bath；
Using above-mentioned binary Cn-Zn without cyanogen, it is without phosphorus, without aminoform gold plating bath carry out imitation gold plating, the technique of imitation gold plating
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 plate.
Embodiment 2
Prepare above-mentioned no cyanogen, it is without phosphorus, without aminoform gold plating bath, include the following steps：
1) 25g boric acid is dissolved in the 500mL hot distilled water that temperature is 50~60 DEG C by the container for taking a 1000mL,
Then 90g citric acid is added, stirring is complete to dissolving；
2) 9g succimide is added into solution made from step 1), stirring is complete to dissolving；
3) 22.5g copper sulphate is added into solution made from step 2), stirring is complete to dissolving；
4) 35g zinc sulfate is added into solution made from step 3), 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 stiring, made potassium hydroxide solution is added in the made solution of step 4)；
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 stiring, 6g sodium stannate is repeatedly marginally added into the potassium hydroxide solution of dissolution, dissolves completely and goes to sodium stannate
It after falling impurity, under stiring, is added in the made solution of step 5), ternary Cn-Zn-Sn can be obtained initially without cyanogen, without phosphorus, nothing
Aminoform gold plating bath；
7) to the made ternary Cn-Zn-Sn of step 6) initially without cyanogen, it is without phosphorus, without in aminoform gold plating bath be added 18mL light
Bright property dispersing agent, and supplement normal-temperature distilled water to 1000mL, stirs evenly, and stands 12~for 24 hours, can obtain 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, without aminoform gold plating bath carry out imitation gold plating, the work of imitation gold plating
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 plate.
Embodiment 3
Prepare above-mentioned no cyanogen, it is without phosphorus, without aminoform gold plating bath, include the following steps：
1) 30g boric acid is dissolved in the 500mL hot distilled water that temperature is 50~60 DEG C by the container for taking a 1000mL,
Then 100g citric acid is added, stirring is complete to dissolving；
2) 10g succimide is added into solution made from step 1), stirring is complete to dissolving；
3) 25g copper sulphate is added into solution made from step 2), stirring is complete to dissolving；
4) 40g zinc sulfate is added into solution made from step 3), 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 stiring, made potassium hydroxide solution is added in the made solution of step 4)；
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 stiring, 8g sodium stannate is repeatedly marginally added into the potassium hydroxide solution of dissolution, dissolves completely and goes to sodium stannate
It after falling impurity, under stiring, is added in the made solution of step 5), ternary Cn-Zn-Sn can be obtained initially without cyanogen, without phosphorus, nothing
Aminoform gold plating bath；
7) 20mL bright property dispersing agent is added into the initial plating solution of the imitative gold of the made ternary Cn-Zn-Sn of step 6), and supplements
Normal-temperature distilled water is stirred evenly to 1000mL, stands 12~for 24 hours, can obtain 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, without aminoform gold plating bath carry out imitation gold plating, the work of imitation gold plating
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 plate.
Claims (6)
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 dispersing agent：16~20mL/L,
Every liter of bright property dispersing agent includes following components：
Ethyoxyl butynediols：160~170g/L,
Niacin：60~70g/L,
Potassium hydroxide：30~50g/L,
Saccharin：40~60g/L,
Sodium Allyl Sulfonate：40~50g/L.
2. no cyanogen according to claim 1, 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. preparing no cyanogen of any of claims 1 or 2, without phosphorus, without aminoform gold plating bath technique, it is characterised in that：Including with
Lower step：
1) boric acid is dissolved in the hot distilled water that temperature is 50~60 DEG C, main complexant is then added, stirring is complete to dissolving；
2) auxiliary complexing agent is added into solution made from step 1), stirring is complete to dissolving；
3) copper sulphate is added into solution made from step 2), stirring is complete to dissolving；
4) zinc sulfate is added into solution made from step 3), stirring is complete to dissolving；
5) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is to dissolving completely, after cooling, under stiring, by made hydroxide
Potassium solution is added in the made solution of step 4), can obtain binary Cn-Zn initially without cyanogen, it is without phosphorus, without aminoform gold plating bath；
6) to the made binary Cn-Zn of step 5) initially without cyanogen, it is without phosphorus, without in aminoform gold plating bath be added bright property dispersing agent,
And supplement normal-temperature distilled water, stir evenly, stand 12~for 24 hours, can obtain binary Cn-Zn without cyanogen, it is without phosphorus, without ammonia imitation gold plating
Liquid.
4. preparing no cyanogen of any of claims 1 or 2, without phosphorus, without aminoform gold plating bath technique, it is characterised in that：Including with
Lower step：
1) boric acid is dissolved in temperature is that main complexant is then added in 50~60 DEG C of hot distilled waters, and stirring is complete to dissolving；
2) auxiliary complexing agent is added into solution made from step 1), stirring is complete to dissolving；
3) copper sulphate is added into solution made from step 2), stirring is complete to dissolving；
4) zinc sulfate is added into solution made from step 3), stirring is complete to dissolving；
5) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is to dissolving completely, after cooling, under stiring, by made hydroxide
Potassium solution is added in the made solution of step 4)；
6) potassium hydroxide is dissolved in normal-temperature distilled water, stirring is complete to dissolving, then, under stiring, to the hydroxide of dissolution
Sodium stannate is marginally repeatedly added in potassium solution, completely and after removing impurity, under stiring, is added to step after sodium stannate dissolution
5) in made solution, can obtain ternary Cn-Zn-Sn initially without cyanogen, it is without phosphorus, without aminoform gold plating bath；
7) to the made ternary Cn-Zn-Sn of step 6) initially without cyanogen, it is without phosphorus, without in aminoform gold plating bath be added bright property dispersion
Agent and normal-temperature distilled water, stir evenly, stand 12~for 24 hours, can obtain ternary Cn-Zn-Sn without cyanogen, it is without phosphorus, without ammonia imitation gold plating
Liquid.
5. using no cyanogen described in claim 1, it is without phosphorus, without aminoform gold plating bath carry out plating piece imitation gold plating, 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 plate.
6. it is according to claim 5 using no cyanogen, it is without phosphorus, without aminoform gold plating bath carry out plating piece imitation gold plating technique,
It is characterized in that：It is 20%~25% that Cu content, which is 75%~80%, Zn content, in the positive C u-Zn plate.
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|---|---|---|---|
| CN201710156908.5A CN106835216B (en) | 2017-03-16 | 2017-03-16 | Without cyanogen, it is without phosphorus, without aminoform gold plating bath and its preparation and electroplating technology |
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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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