CN109576742A - Novel alkaline non-cyanogen galvanization additive - Google Patents
Novel alkaline non-cyanogen galvanization additive Download PDFInfo
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- CN109576742A CN109576742A CN201910076435.7A CN201910076435A CN109576742A CN 109576742 A CN109576742 A CN 109576742A CN 201910076435 A CN201910076435 A CN 201910076435A CN 109576742 A CN109576742 A CN 109576742A
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- additive
- modified aromatic
- plating
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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
- C25D3/22—Electroplating: Baths therefor from solutions of zinc
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Abstract
The invention discloses a kind of novel alkaline non-cyanogen galvanization additives, are made of following component: urea amine cation quaternary ammonium salt 15%~25%;Imidazoles propoxyl group condensation product 10%~20%;Polyethyleneimine cation quaternary ammonium salt 4%~6%;Benzyl group niacin drone salt 0.8%~1.2%;Modified aromatic aldehyde compound 1%~1.4%;EDTA-2Na2.0%~2.5%;Modified aromatic aldehydes sulfonated bodies 7.5%~8.0%;Pure water surplus.The plating solution of gained additive configuration has good deep plating and covering power, and low brittle coatings brightness is high, and careful smooth, salt fog performance is high;Deposition velocity is especially fast, and current efficiency is high, and easy to operate, controlling is good, is suitable for rack plating and barrel plating.
Description
Technical field
The present invention relates to galvanizing surface processing technology fields, more specifically, it relates to a kind of novel alkaline non-cyanogen galvanization
Additive.
Background technique
Zinc plating electrolyte can be divided into alkalinity and acid two major classes, there are commonly non-cyanide alkalis both at home and abroad zinc-plated, cyanide
It is zinc-plated, ammonium salt is zinc-plated, chloride galvanizing, sulfate zinc plating etc..Acid zinc plating is since brightness is good, high-efficient, bright current is close
Degree haves a wide reach, plating massive plate part and barrel plating in terms of have advantage, cyanide zinc plating wastewater have relatively high comprehensive performance, but because
It is more toxic, environmental-protecting performance is poor, only still has application in special industry.Alkaline non-cyanogen galvanization, because the toxicity of plating solution is smaller, waste water
Be easier to handle, while more excellent and non-corrosive compared to the dispersibility of acid zinc plating, the operation of operation system and plating solution at
This be also it is lower, be especially considering that the later period expense of wastewater treatment, this makes alkaline non-cyanide plating solution in advocating environment protection and energy conservation
Society have attracted more and more attention from people.
But compare other systems, there is also the deficiencies of some aspect of performance for alkaline non-cyanogen galvanization: such as with acidic bath phase
Than evolving hydrogen reaction, efficiency is relatively low, and in addition brightness and planarization are poor;It is zinc-plated compared to cyanide, bright density range
Poor, coating is crisp and anode causes to be passivated, and pre-treatment is stringenter, and ductility is poor.Therefore, alkaline non-cyanogen galvanization additive
Selection it is just very crucial.
Although there are many trans-corporations at present brings its high performance alkaline non-cyanogen galvanization technology and product into China,
But the process materials condition limitation of expensive price and harshness is received, the practical application of the advanced technology at home is limited
System.At present at home, it is the biography of representative that alkaline non-cyanogen galvanization major part additive, which is still DPE- III, the DE etc. of the exploitation seventies,
Unite additive, these additives use when there are following problems: first is that low current density delusters, clear zone is narrow so that using by
Limitation, unsuitable barrel plating;Second is that dispersibility is poor, waste of resource is caused, is especially unsuitable for complex part;Third is that covering power
Difference is also to lead to the wasting of resources, is not suitable for barrel plating;Fourth is that coating brittleness is high, suitability for secondary processing is poor.
It is especially domestic for the research of alkaline non-cyanogen galvanization additive based on above-mentioned status, it was not interrupted.Such as
200310112330.1 Alkaline Not Have Cyanogen Zincate Galvanization Brightening Agent and Composite Brightening Agent disclosed in number patent is by least
A kind of nitrogen-containing heterocycle compound 0.5-5.0mol, and at least one hydroxylamine 0.5-4.0mol, and it is at least one containing acyl group or sulphur
Two tertiary amine 0.5-5.0mol of acyl group are generated with 4.0-10.0mol epoxyhalopropane and/or the random copolyreaction of glycerol halohydrin
Copolymerized polymer;Preparation method are as follows: by the nitrogen-containing heterocycle compound of above-mentioned formula, hydroxylamine, containing acyl group or sulfonyl
Epoxyhalopropane and/or glycerol halohydrin is added in two tertiary amines and suitable water, heat temperature raising while stirring, and temperature control exists
Reflux temperature keeps the temperature 4-10 hours hereinafter, the time at 0.5-2 hours, then heats to reflux temperature.The technology is applied to alkalinity
In non-cyanogen galvanization technique, although improving using current density range, the problems such as brittleness, depth capability, still fails to be solved
Certainly.
It a kind of alkaline zinc plating additive disclosed in No. 200810120879.8 patent and its applies on ironcasting
Zincincation, the alkaline zinc plating additive includes auxiliary additive and brightener, in brightener I, II, III compound
Or mixtures thereof one kind, auxiliary additive is the complexing agent of zinc ion, the pK shakiness value of the unstable constant of the complexing agent
Between 16.8~22.36, the brightener concentration in used alkaline zinc plating additive is 50mg/L~5000mg/L, auxiliary
Additive concentration be 0.5g/L~10g/L. program mainly as the addition of auxiliary additive so that obtained by zinc-plating additive solution
Determined bright blue passivation when the problem of being easy jaundice, but be not directed to the raising of other performances such as deep plating, current efficiency.
In view of above-mentioned, existing domestic technique and disclosed relevant information, still there is very big research space, constantly
The novel alkaline zinc-plating additive for haveing excellent performance, meeting work processing performance demand is developed, it is imperative.
Summary of the invention
The purpose of the present invention is for domestic alkaline non-cyanogen galvanization technological lag, brittleness, depth capability are inadequate, ductility
Difference, not environmentally the problems such as, a kind of alkaline non-cyanogen galvanization additive of novel suitable domestic prior art material condition is provided.
To achieve the above object, it is realized by following technological means: a kind of novel alkaline non-cyanogen galvanization additive, by as follows
Component is constituted:
It advanced optimizes are as follows: novel alkaline non-cyanogen galvanization additive is made of following component:
It advanced optimizes are as follows: novel alkaline non-cyanogen galvanization additive is made of following component:
It advanced optimizes are as follows: the modified aromatic aldehydes sulfonated bodies is to utilize sulfamic acid, the concentrated sulfuric acid or chlorosulfonic acid pair
Modified aromatic aldehyde compound carries out obtained by sulfonation.
The method of the novel alkaline non-cyanogen galvanization additive includes the following steps: that calculating is added first in reaction kettle
The pure water of amount, then sequentially added when stirring urea amine cation quaternary ammonium salt, imidazoles propoxyl group condensation product, polyethyleneimine sun from
Sub- quaternary ammonium salt, benzyl group niacin drone salt, modified aromatic aldehyde compound, EDTA-2Na, modified aromatic aldehydes sulfonated bodies stir 10-
20 minutes to uniformly without precipitating.
The advantages of the present invention over the prior art are that:
1, additive of the invention can improve the deposition efficiency of plating solution, than commercially available additive raising efficiency 2 times or more, one
As alkaline non-cyanide plating solution rack plating need electric current be 3~4A/dm2, and this product only needs 1~2A/dm2, energy conservation and environmental protection;
2, additive deep hole of the invention plating is high-efficient, and performance is good, and general additive deep hole plating aperture ratio only has 1:4,
And this product, up to 1:8, the plating solution zinc concentration that general additive is configured is in 8g/L hereinafter, this product is up to 12g/L;
3, after using this product, obtained coating brittleness is small, and zinc layers flexibility is good, unlike existing non-cyanide bright agent is crisp
Property it is big, be particularly suitable for functional plating, as auto parts and components plating, it can be achieved that functional coating up to bending after 10~20 μm not
Crisp zinc;
4, the plating performance of this product is good, and the height area thickness of coating ratio through the commercially available additive of hull trough test is greater than 1:
1.5, and this product is up to 1:1.2;
5, this product is particularly suitable for barrel plating and rack plating.
Specific embodiment
Invention is described in further detail below by specific embodiment, it is not to limit that following embodiment, which is descriptive,
Protection scope of the present invention of property.
Novel alkaline non-cyanogen galvanization additive of the invention, is made of following component:
Wherein, the modified aromatic aldehydes sulfonated bodies is using sulfamic acid, the concentrated sulfuric acid or chlorosulfonic acid to modified aromatic
Aldehyde compound carries out obtained by sulfonation.Such as when with sulfamic acid sulfonation, specific sulfonation process are as follows: be added 1 in beaker and rub
The powdered sulfamic acid of 2 moles of purifications is added in your modified aromatic aldehyde compound, and for 70g urea as catalyst, stirring is equal
It is even, it is placed in water-bath and is heated to 60~80 DEG C, terminate to sulfonating reaction within insulated and stirred 1 hour, product is transferred to three-neck flask
In, caustic soda ammonia excretion gas is added, and cooling with cold water, temperature is made to be no more than 60 DEG C, adjusts pH to 10~12, after neutralization,
The remaining ammonia of exclusion is vacuumized under the vacuum degree of 1.33~2kPa, pH is down to 8~9.
In said components, zinc ion is mainly complexed in urea amine cation quaternary ammonium salt, is allowed to low to electric current from the high area of electric current
Area's migration, imidazoles propoxyl group condensation product improve leveling, the light of zinc layers, polyethyleneimine amine cation season as auxiliary brightener
Ammonium salt improves zinc-plated dispersibility, improves the light in the low area of electric current, and benzyl group niacin drone salt and modified aromatic aldehyde compound improve
The bright levelling of zinc layers, EDTA-2Na play the role of that impurity is complexed and zinc ion, modified aromatic aldehydes are complexed as complexing agent
Sulfonated bodies mainly promotes low area's current density, overcomes Faraday effect, deposition of the enhancing zinc ion in the low area of electric current.
The applicable operating condition of above-mentioned additive are as follows: in plating solution the content of zinc and sodium hydroxide ratio exists in 1:10~14
Contain 10~12 grams of zinc oxide, 100~160 grams of sodium hydroxide, 10~80 grams of sodium carbonate, 16~20ml of additive in every liter of plating solution.
Applicable temperature is 15~35 DEG C, is applicable in that voltage is 3~8V, electric current is 2~4A/dm when rack plating2, it is 6 that voltage is applicable in when barrel plating
~12V, electric current are 0.5~1A/dm2。
Under the operating conditions described above, the consumption of the additive is 150~220 milliliters/kilo-ampere hour.Above-mentioned additive is also
It can be used cooperatively together with other brighteners, regulator.When the consumption of the additive is 150-220ml/ kilo-ampere, brightener
Additional amount be often plus 1L brightener is added in the 2-5L additive, i.e. the additive: brightener=2-5:1, if to coating
Brightness requirement is high, and the additive amount of brightener can be improved.The additional amount of regulator is that 0.5-1L is added in every addition 10-20L brightener
Regulator.Here brightener and regulator can be existing procucts in the market, as the scientific and technological share of Wuhan sail electrification is limited
The ZN-500B brightener and ZN-500C regulator of company's production;Or the 223B of Hong Zheng Chemical Co., Ltd., Xiamen City production is bright
Agent and 223C regulator.
Embodiment 1
The additive of 1L is configured first, and wherein the weight ratio of each component is the quaternary ammonium salt of amine cation containing urea 15%;Imidazoles
Propoxyl group condensation product 10%;Polyethyleneimine cation quaternary ammonium salt 4%;Benzyl group niacin drone salt 0.8%;Modified aromatic aldehydes chemical combination
Object 1%;EDTA-2Na2.0%;Modified aromatic aldehydes sulfonated bodies 7.5%;Surplus is pure water.It is added and calculates first in reaction kettle
The pure water of amount, then sequentially added when stirring urea amine cation quaternary ammonium salt, imidazoles propoxyl group condensation product, polyethyleneimine sun from
Sub- quaternary ammonium salt, benzyl group niacin drone salt, modified aromatic aldehyde compound, EDTA-2Na, modified aromatic aldehydes sulfonated bodies stir 20 points
Clock is to uniformly without precipitating.
Plating solution 1L is configured, so that 10g containing zinc oxide, sodium hydroxide 100g, sodium carbonate 10g, above-mentioned additive in plating solution
16ml, temperature are 25 DEG C, current density 2A/dm2When, the consumption of the additive is 150 milliliters/kilo-ampere hour.
Embodiment 2
The additive of 1L is configured first, and wherein the weight ratio of each component is the quaternary ammonium salt of amine cation containing urea 25%;Imidazoles
Propoxyl group condensation product 20%;Polyethyleneimine cation quaternary ammonium salt 6%;Benzyl group niacin drone salt 1.2%;Modified aromatic aldehydes chemical combination
Object 1.4%;EDTA-2Na2.5%;Modified aromatic aldehydes sulfonated bodies 8%;Surplus is pure water.It is added and calculates first in reaction kettle
The pure water of amount, then sequentially added when stirring urea amine cation quaternary ammonium salt, imidazoles propoxyl group condensation product, polyethyleneimine sun from
Sub- quaternary ammonium salt, benzyl group niacin drone salt, modified aromatic aldehyde compound, EDTA-2Na, modified aromatic aldehydes sulfonated bodies stir 20 points
Clock is to uniformly without precipitating.
Plating solution 1L is configured, so that 11g containing zinc oxide, sodium hydroxide 130g, sodium carbonate 10g, above-mentioned additive in plating solution
18ml, temperature are 25 DEG C, current density 2A/dm2When, the consumption of the additive is 155 milliliters/kilo-ampere hour.
Embodiment 3
The additive of 1L is configured first, and wherein the weight ratio of each component is the quaternary ammonium salt of amine cation containing urea 17%;Imidazoles
Propoxyl group condensation product 12%;Polyethyleneimine cation quaternary ammonium salt 4%;Benzyl group niacin drone salt 0.9%;Modified aromatic aldehydes chemical combination
Object 1.1%;EDTA-2Na2.1%;Modified aromatic aldehydes sulfonated bodies 7.6%;Surplus is pure water.Meter is added first in reaction kettle
Then the pure water of calculation amount sequentially adds urea amine cation quaternary ammonium salt, imidazoles propoxyl group condensation product, polyethyleneimine sun when stirring
Quaternary ammonium salts, benzyl group niacin drone salt, modified aromatic aldehyde compound, EDTA-2Na, modified aromatic aldehydes sulfonated bodies, stirring 18
Minute is to uniformly without precipitating.
Plating solution 1L is configured, so that 12g containing zinc oxide, sodium hydroxide 140g, sodium carbonate 50g, above-mentioned additive in plating solution
20ml, temperature are 25 DEG C, current density 2A/dm2When, the consumption of the additive is 180 milliliters/kilo-ampere hour.
Embodiment 4
The additive of 1L is configured first, and wherein the weight ratio of each component is the quaternary ammonium salt of amine cation containing urea 23%;Imidazoles
Propoxyl group condensation product 18%;Polyethyleneimine cation quaternary ammonium salt 6%;Benzyl group niacin drone salt 1.1%;Modified aromatic aldehydes chemical combination
Object 1.2%;EDTA-2Na2.4%;Modified aromatic aldehydes sulfonated bodies 7.9%;Surplus is pure water.Meter is added first in reaction kettle
Then the pure water of calculation amount sequentially adds urea amine cation quaternary ammonium salt, imidazoles propoxyl group condensation product, polyethyleneimine sun when stirring
Quaternary ammonium salts, benzyl group niacin drone salt, modified aromatic aldehyde compound, EDTA-2Na, modified aromatic aldehydes sulfonated bodies, stirring 18
Minute is to uniformly without precipitating.
Plating solution 1L is configured, so that 12g containing zinc oxide, sodium hydroxide 120g, sodium carbonate 80g, above-mentioned additive in plating solution
19ml, temperature are 25 DEG C, current density 1A/dm2When, the consumption of the additive is 200 milliliters/kilo-ampere hour.
Embodiment 5
The additive of 1L is configured first, and wherein the weight ratio of each component is the quaternary ammonium salt of amine cation containing urea 20%;Imidazoles
Propoxyl group condensation product 15%;Polyethyleneimine cation quaternary ammonium salt 5%;Benzyl group niacin drone salt 1%;Modified aromatic aldehyde compound
1.2%;EDTA-2Na2.3%;Modified aromatic aldehydes sulfonated bodies 7.8%;Surplus is pure water.It is added and calculates first in reaction kettle
The pure water of amount, then sequentially added when stirring urea amine cation quaternary ammonium salt, imidazoles propoxyl group condensation product, polyethyleneimine sun from
Sub- quaternary ammonium salt, benzyl group niacin drone salt, modified aromatic aldehyde compound, EDTA-2Na, modified aromatic aldehydes sulfonated bodies stir 20 points
Clock is to uniformly without precipitating.
Plating solution 1L is configured, so that 11g containing zinc oxide, sodium hydroxide 160g, sodium carbonate 30g, above-mentioned additive in plating solution
20ml, temperature are 25 DEG C, current density 1A/dm2When, the consumption of the additive is 220 milliliters/kilo-ampere hour.
Comparative example 1
This comparative example is that modified aromatic aldehydes sulfonated bodies is added without in the additive configuration process of embodiment 1, other
The configuration of part and plating solution is all in the same manner as in Example 1.
The additive that above-described embodiment, comparative example and present state's internal clamp company use is subjected to hull trough test respectively
Comparison, the results are shown in Table 1.
The comparison of 1 various additives coating performance of table
As can be seen from Table 1, the height area dispersibility of the existing additive of fastener company is 1:1.68, the height of comparative example
Low area's dispersibility is 1:1.66, and the dispersibility of additive of the present invention is 1:1.2, coating bright property, appearance, brittleness etc. compared with
Good, the existing Additive Properties of fastener company are relatively poor.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of novel alkaline non-cyanogen galvanization additive, which is characterized in that be made of following component:
2. novel alkaline non-cyanogen galvanization additive according to claim 1, which is characterized in that be made of following component:
3. novel alkaline non-cyanogen galvanization additive according to claim 1, which is characterized in that be made of following component:
4. novel alkaline non-cyanogen galvanization additive according to any one of claim 1 to 3, which is characterized in that described
Modified aromatic aldehydes sulfonated bodies is to carry out sulfonation institute to modified aromatic aldehyde compound using sulfamic acid, the concentrated sulfuric acid or chlorosulfonic acid
?.
5. a kind of method for preparing novel alkaline non-cyanogen galvanization additive as claimed in claim 4, which is characterized in that including as follows
Step: the pure water of calculation amount is added first in reaction kettle, urea amine cation quaternary ammonium salt, imidazoles are then sequentially added when stirring
Propoxyl group condensation product, polyethyleneimine cation quaternary ammonium salt, benzyl group niacin drone salt, modified aromatic aldehyde compound, EDTA-2Na,
Modified aromatic aldehydes sulfonated bodies stirs 10-20 minutes to uniformly without precipitating.
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