CN109252194A - A kind of Zinc-nickel alloy electroplating liquid and its preparation process - Google Patents
A kind of Zinc-nickel alloy electroplating liquid and its preparation process Download PDFInfo
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- CN109252194A CN109252194A CN201811396932.7A CN201811396932A CN109252194A CN 109252194 A CN109252194 A CN 109252194A CN 201811396932 A CN201811396932 A CN 201811396932A CN 109252194 A CN109252194 A CN 109252194A
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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
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Abstract
The present invention discloses a kind of Zinc-nickel alloy electroplating liquid, includes zinc oxide, sodium hydroxide, nickel replenishers, nickel complexing agent, brightener M and brightener B, wherein brightener B is the solution being configured to by the ethylenediamine and epoxychloropropane synthetic product of 1~3:1 of mol ratio.Add this kind of brightener B make in electroplate liquid coating crystallization it is careful, coating is bright, simultaneously admiro be evenly distributed in coating so that cladding wearability is good, hardness is high and coating is also not easily to fall off during secondary withhold.Meanwhile invention additionally discloses a kind of preparation process of Zinc-nickel alloy electroplating liquid, preparation process is simple, easy to operate, at low cost, is suitable for large-scale production and uses.
Description
Technical field
The invention belongs to electroplate liquid technical fields, and in particular to a kind of Zinc-nickel alloy electroplating liquid and its preparation process.
Background technique
Zn-ni alloy deposits are a kind of novel excellent protective coatings, be mainly used in aerospace, auto industry and
In mechano-electronic product.In electric field component surface anti-corrosion and protection, admiro film layer is as final protecting film
Layer, it is desirable that it has excellent corrosion resistance, wearability and hardness etc..
With the fast development of modern industry and science and technology, material surface antiseptic property also proposed higher and higher
It is required that.Currently, brightener would generally be added in Zinc-nickel alloy electroplating liquid.Brightener is a kind of gloss agent, usually in various productions
Play the role of coating in product surface.The main function of brightener shows the oil for removing by active surface and resting on metal surface
Dirty, oxidation and unoxidized surface impurity keep cleaning outside object, glossiness, color fastness.Increase in electroplate liquid bright
The glossiness and color fastness of workpiece to be plated can be improved in agent.For example, in patent 200680028815.4, Zinc-nickel alloy electroplating system
Carrier brightener is used as using polyethylene glycol -3350 in system, achieves all bright cladding；For another example patent 200910094368.8 1
Kind Zinc-nickel alloy electroplating liquid is using nonylphenol polyoxyethylene ether as carrier brightener, the same coating for obtaining light.However it is existing
In some patents, the brightener in Zinc-nickel alloy electroplating liquid is only capable of playing the role of improving glossiness, the wearability of coating with
And hardness is lower, therefore coating surface is easy to be hung, and influences the quality of coating.Therefore, study a kind of cladding wearability and
The higher Zinc-nickel alloy electroplating liquid of hardness and its preparation process are particularly important.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of Zinc-nickel alloy electroplating liquid and its preparation processes, solve
The technical problem that cladding wearability is poor, hardness is low in the prior art.
In order to solve the above technical problems, the technical solution adopted by the present invention: a kind of Zinc-nickel alloy electroplating liquid, feature exist
In every liter of electroplate liquid includes following components:
The nickel replenishers are nickel salt solution, and nickel ion concentration is 60-100g/L in the nickel salt solution；The nickel complexing
The concentration of agent is 10-600g/L；The concentration 10-50g/L, the brightener B of the brightener M is by mol ratio 1~3: 1
The solution that ethylenediamine and epoxychloropropane synthetic product are configured to, and the solution concentration of brightener B is 100-500g/L.
Preferably, the synthetic product of the ethylenediamine and epoxychloropropane the preparation method is as follows:
(21) ethylenediamine and epoxychloropropane are weighed according to the proportion；
(22) ethylenediamine is put into reaction vessel, stirs and ethylenediamine is heated, elevated the temperature to 50-70
℃；
(23) epoxychloropropane is added dropwise into ethylenediamine, maintaining reaction temperature is 80-90 DEG C；
(24) reaction solution in step (23) is kept the temperature, holding temperature is 100-120 DEG C, soaking time 10-
20min is finally cooled to room temperature, obtains the synthetic product of aminated compounds and epoxychloropropane.
Preferably, the nickel replenishers are the aqueous solution of nickel sulfate or nickel sulfamic acid.
Preferably, the nickel complexing agent includes polyamine compound.
Preferably, the solution concentration of the polyamine compound is 10-50g/L.
Preferably, the polyamine compound is one of polyethyleneimine, polypropylene amine or two kinds of combinations.
Preferably, the brightener M is one of polyethyleneimine, polypropylene amine or two kinds of combination
A kind of preparation method of Zinc-nickel alloy electroplating liquid, which comprises the following steps:
(81), nickel replenishers, nickel complexing agent, brightener M and brightener B solution are configured；
(82), part water is added in a reservoir, then zinc oxide and sodium hydroxide are dissolved in the water, are configured to solution；
(83), it is molten that nickel replenishers, nickel complexing agent, brightener M and brightener B are sequentially added in the solution of step (82)
Liquid；
(84), remaining water is finally added in step (83).
Beneficial effects of the present invention: the present invention discloses a kind of Zinc-nickel alloy electroplating liquid, includes zinc oxide, sodium hydroxide, nickel
Replenishers, nickel complexing agent, brightener M and brightener B, wherein brightener B is the ethylenediamine and epoxy by mol ratio 1~3: 1
The solution that chloropropane synthetic product is configured to.Add this kind of brightener B makes coating crystallize careful, coating light in electroplate liquid
Bright while admiro is evenly distributed in coating, so that cladding wearability is good, hardness is high and coating is withheld secondary
Also not easily to fall off in the process.Meanwhile invention additionally discloses a kind of preparation process of Zinc-nickel alloy electroplating liquid, preparation process letters
It is single, it is easy to operate, it is at low cost, it is suitable for large-scale production and uses.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1:
A kind of Zinc-nickel alloy electroplating liquid, every liter of electroplate liquid includes following components:
Wherein, nickel ion concentration is 62g/L in nickel sulfate solution, and the concentration of polypropylene amine solution is 30g/L, polyethyleneimine
The concentration of amine aqueous solution is 10g/L, and the solution concentration of ethylenediamine and epoxychloropropane synthetic product is 500g/L.
In the present embodiment, the synthetic method of ethylenediamine and epoxychloropropane synthetic is as follows:
(1), 60g ethylenediamine and 92g epoxychloropropane are weighed；
(2), ethylenediamine is poured into three-necked flask, three-necked flask is put into magnetic agitation electric jacket and is stirred, simultaneously will
Ethylenediamine is heated to 60 DEG C；
(3), epoxychloropropane is added in separatory funnel, is then slowly added dropwise into ethylenediamine, solution can be fast at this time
Speed heats up, and needs to cool down reaction solution in the present embodiment, and the type of cooling can use conventional method, maintaining reaction temperature
It is 85 DEG C:
(4), it needs to keep the temperature reaction solution after dripping epoxychloropropane, removes cooling device at this time, and to anti-
Solution is answered to heat, so that holding temperature is 110 DEG C, soaking time 15min is finally cooled to room temperature, obtains synthetic product.
The reaction equation of the synthetic product is as follows:
The preparation step of Zinc-nickel alloy electroplating liquid is as follows in the present embodiment:
(1), zinc oxide, sodium hydroxide, nickel sulfate, polypropylene amine, the polyethyleneimine, second two of formula ratio are weighed first
Amine and epoxychloropropane；Nickel sulfate solution is first configured, nickel sulfate is added to the water, heats up 80 DEG C, dissolution is sufficiently stirred；Match again
Polypropylene amine solution is set, polypropylene amine is added to the water, is dissolved after being sufficiently stirred；It is reconfigured polyethylenimine solution, will be gathered
Aziridine is added to the water, and dissolves after being sufficiently stirred；It is reconfigured the solution of ethylenediamine and epoxychloropropane synthetic product, by second
Diamines is added to the water with epoxychloropropane synthetic product, dissolves after being sufficiently stirred；
(2), part water is added in a reservoir, then the zinc oxide of formula ratio and sodium hydroxide are dissolved in the water, stirs
Solution is configured to after uniformly；
(3), it is sequentially added in the solution of step (2) by the nickel sulfate solution of the formula ratio of configuration, poly- third in step (1)
Enamine solution, polyethylenimine solution, ethylenediamine and epoxychloropropane synthetic product solution；
(4), remaining water is finally added in step (3).
Embodiment 2:
A kind of Zinc-nickel alloy electroplating liquid, every liter of electroplate liquid includes following components:
Wherein, nickel ion concentration is 62g/L in nickel sulfate solution, and the concentration of polypropylene amine solution is 30g/L, polyethyleneimine
The concentration of amine aqueous solution is 10g/L, and the solution concentration of ethylenediamine and epoxychloropropane synthetic product is 500g/L.
In the present embodiment, the synthetic method of ethylenediamine and epoxychloropropane synthetic is as follows:
(1), 60g ethylenediamine and 92g epoxychloropropane are weighed；
(2), ethylenediamine is poured into three-necked flask, three-necked flask is put into magnetic agitation electric jacket and is stirred, simultaneously will
Ethylenediamine is heated to 65 DEG C；
(3), epoxychloropropane is added in separatory funnel, is then slowly added dropwise into ethylenediamine, solution can be fast at this time
Speed heats up, and needs to cool down reaction solution in the present embodiment, and the type of cooling can use conventional method, maintaining reaction temperature
It is 80 DEG C；
(4), it needs to keep the temperature reaction solution after dripping epoxychloropropane, removes cooling device at this time, and to anti-
Solution is answered to heat, so that holding temperature is 120 DEG C, soaking time 10min is finally cooled to room temperature, obtains synthetic product.
The reaction equation of the synthetic product is as follows:
The preparation step of Zinc-nickel alloy electroplating liquid is the same as embodiment 1 in the present embodiment.
Embodiment 3:
A kind of Zinc-nickel alloy electroplating liquid, every liter of electroplate liquid includes following components:
Wherein, nickel ion concentration is 62g/L in nickel sulfate solution, and the concentration of polypropylene amine solution is 30g/L, polyethyleneimine
The concentration of amine aqueous solution is 10g/L, and the solution concentration of ethylenediamine and epoxychloropropane synthetic product is 500g/L.
In the present embodiment, the synthetic method of ethylenediamine and epoxychloropropane synthetic is as follows:
(1), 60g ethylenediamine and 92g epoxychloropropane are weighed；
(2), ethylenediamine is poured into three-necked flask, three-necked flask is put into magnetic agitation electric jacket and is stirred, simultaneously will
Ethylenediamine is heated to 65 DEG C；
(3), epoxychloropropane is added in separatory funnel, is then slowly added dropwise into ethylenediamine, solution can be fast at this time
Speed heats up, and needs to cool down reaction solution in the present embodiment, and the type of cooling can use conventional method, maintaining reaction temperature
It is 88 DEG C；
(4), it needs to keep the temperature reaction solution after dripping epoxychloropropane, removes cooling device at this time, and to anti-
Solution is answered to heat, so that holding temperature is 115 DEG C, soaking time 13min is finally cooled to room temperature, obtains synthetic product.
The reaction equation of the synthetic product is as follows:
The preparation step of Zinc-nickel alloy electroplating liquid is the same as embodiment 1 in the present embodiment.
Embodiment 4:
A kind of Zinc-nickel alloy electroplating liquid, every liter of electroplate liquid includes following components:
Wherein, nickel ion concentration is 62g/L in nickel sulfate solution, and the concentration of polypropylene amine solution is 30g/L, polyethyleneimine
The concentration of amine aqueous solution is 10g/L, and the solution concentration of ethylenediamine and epoxychloropropane synthetic product is 500g/L.
In the present embodiment, the synthetic method of ethylenediamine and epoxychloropropane synthetic is as follows:
(1), 60g ethylenediamine and 92g epoxychloropropane are weighed；
(2), ethylenediamine is poured into three-necked flask, three-necked flask is put into magnetic agitation electric jacket and is stirred, simultaneously will
Ethylenediamine is heated to 68 DEG C；
(3), epoxychloropropane is added in separatory funnel, is then slowly added dropwise into ethylenediamine, solution can be fast at this time
Speed heats up, and needs to cool down reaction solution in the present embodiment, and the type of cooling can use conventional method, maintaining reaction temperature
It is 83 DEG C；
(4), it needs to keep the temperature reaction solution after dripping epoxychloropropane, removes cooling device at this time, and to anti-
Solution is answered to heat, so that holding temperature is 105 DEG C, soaking time 18min is finally cooled to room temperature, obtains synthetic product.
The reaction equation of the synthetic product is as follows:
The preparation step of Zinc-nickel alloy electroplating liquid is the same as embodiment 1 in the present embodiment.
Embodiment 5:
A kind of Zinc-nickel alloy electroplating liquid, every liter of electroplate liquid includes following components:
Wherein, nickel ion concentration is 62g/L in nickel sulfate solution, and the concentration of polypropylene amine solution is 30g/L, polyethyleneimine
The concentration of amine aqueous solution is 10g/L, and the solution concentration of ethylenediamine and epoxychloropropane synthetic product is 500g/L.
In the present embodiment, the synthetic method of ethylenediamine and epoxychloropropane synthetic is as follows:
(1), 60g ethylenediamine and 92g epoxychloropropane are weighed；
(2), ethylenediamine is poured into three-necked flask, three-necked flask is put into magnetic agitation electric jacket and is stirred, simultaneously will
Ethylenediamine is heated to 68 DEG C；
(3), epoxychloropropane is added in separatory funnel, is then slowly added dropwise into ethylenediamine, solution can be fast at this time
Speed heats up, and needs to cool down reaction solution in the present embodiment, and the type of cooling can use conventional method, maintaining reaction temperature
It is 90 DEG C；
(4), it needs to keep the temperature reaction solution after dripping epoxychloropropane, removes cooling device at this time, and to anti-
Solution is answered to heat, so that holding temperature is 120 DEG C, soaking time 10min is finally cooled to room temperature, obtains synthetic product.
The reaction equation of the synthetic product is as follows:
The preparation step of Zinc-nickel alloy electroplating liquid is the same as embodiment 1 in the present embodiment.
The leveling degree of coating embodiment 1-5 and ZN80 is measured by finish instrument, wherein ZN80 is one in the market
Kind electroplated product, determination data are shown in Table 1:
| Leveling value before plating | Leveling value after plating | Leveling degree (%) | |
| ZN80 | 0.41 | 0.20 | 51.2 |
| Embodiment 1 | 0.32 | 0.10 | 68.7 |
| Embodiment 2 | 0.43 | 0.13 | 69.8 |
| Embodiment 3 | 0.44 | 0.13 | 70.5 |
| Embodiment 4 | 0.39 | 0.12 | 69.2 |
| Embodiment 5 | 0.35 | 0.11 | 68.5 |
It should be noted that leveling degree is higher, the crystallization fineness of coating is better, i.e., brightness is better.As shown in Table 1, real
The leveling degree for applying a 1-5 is higher than existing product ZN80, illustrates that the coating crystallization fineness of embodiment 1-5 product is good compared with ZN80, i.e.,
Brightness is good compared with ZN80.
The comparative experimental data of ray velocity such as table 2 out:
Gather whether cold test method measurement coating blisters using heating.Embodiment 1-5 and ZN80 are proceeded as follows:
Sample coupon keeps the temperature 1 hour in 300 ± 1 DEG C of baking ovens after being electroplated, and then puts it into cooling in 15-351 DEG C of cold water, observation
Whether coating has foaming phenomena, and experimental result is shown in Table 3.
| Whether coating blisters | |
| ZN80 | There is blistering |
| Embodiment 1 | Without blistering |
| Embodiment 2 | Without blistering |
| Embodiment 3 | Without blistering |
| Embodiment 4 | Without blistering |
| Embodiment 5 | Without blistering |
Above-mentioned experimental data shows under identical plating conditions, and using different electroplate liquids, the bubblement of coating is different
It causes.After being electroplated using electroplate liquid disclosed by the invention, coating is not blistering, illustrates that the binding force of coating and workpiece is good, simultaneously
Illustrate that the wearability of coating is preferable.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (8)
1. a kind of Zinc-nickel alloy electroplating liquid, which is characterized in that every liter of electroplate liquid includes following components:
The nickel replenishers are nickel salt solution, and nickel ion concentration is 60-100g/L in the nickel salt solution；The nickel complexing agent
Concentration is 10-600g/L；The concentration 10-50g/L, the brightener B of the brightener M is the second two by 1~3:1 of mol ratio
The solution that amine and epoxychloropropane synthetic product are configured to, and the solution concentration of brightener B is 100-500g/L.
2. a kind of Zinc-nickel alloy electroplating liquid according to claim 1, it is characterised in that: the ethylenediamine and epoxychloropropane
Synthetic product the preparation method is as follows:
(21) ethylenediamine and epoxychloropropane are weighed according to the proportion；
(22) ethylenediamine is put into reaction vessel, stirs and ethylenediamine is heated, elevated the temperature to 50-70 DEG C；
(23) epoxychloropropane is added dropwise into ethylenediamine, maintaining reaction temperature is 80-90 DEG C；
(24) reaction solution in step (23) is kept the temperature, holding temperature is 100-120 DEG C, soaking time 10-
20min is finally cooled to room temperature, obtains the synthetic product of aminated compounds and epoxychloropropane.
3. a kind of Zinc-nickel alloy electroplating liquid according to claim 1, it is characterised in that: the nickel replenishers are nickel sulfate or ammonia
The aqueous solution of base nickel sulphonic acid.
4. a kind of Zinc-nickel alloy electroplating liquid according to claim 1, it is characterised in that: the nickel complexing agent includes polyamines
Close object.
5. a kind of Zinc-nickel alloy electroplating liquid according to claim 4, it is characterised in that: the solution of the polyamine compound is dense
Degree is 10-50g/L.
6. a kind of Zinc-nickel alloy electroplating liquid according to claim 5, it is characterised in that: the polyamine compound is polyethylene
One of imines, polypropylene amine or two kinds of combinations.
7. a kind of Zinc-nickel alloy electroplating liquid according to claim 1, it is characterised in that: the brightener M be polyethyleneimine,
One of polypropylene amine or two kinds of combinations.
8. a kind of preparation method of Zinc-nickel alloy electroplating liquid described in a kind of -7 any one according to claim 1, which is characterized in that
The following steps are included:
(81), nickel replenishers, nickel complexing agent, brightener M and brightener B solution are configured；
(82), part water is added in a reservoir, then zinc oxide and sodium hydroxide are dissolved in the water, are configured to solution；
(83), nickel replenishers, nickel complexing agent, brightener M and brightener B solution are sequentially added in the solution of step (82)；
(84), remaining water is finally added in step (83).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114592221A (en) * | 2022-01-17 | 2022-06-07 | 德锡化学(山东)有限公司 | Novel carrier brightener for zinc and zinc alloy |
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