CN102383152A - Low-foam carrier brightening agent and using method thereof - Google Patents
Low-foam carrier brightening agent and using method thereof Download PDFInfo
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- CN102383152A CN102383152A CN2011103663101A CN201110366310A CN102383152A CN 102383152 A CN102383152 A CN 102383152A CN 2011103663101 A CN2011103663101 A CN 2011103663101A CN 201110366310 A CN201110366310 A CN 201110366310A CN 102383152 A CN102383152 A CN 102383152A
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Abstract
The invention discloses a low-foam carrier brightening agent. The low-foam carrier brightening agent comprises 90 to 95 mass percent of nonionic surfactant and 5 to 10 mass percent of nonionic organic silicon surfactant. The invention also discloses a softening agent and a brightening agent prepared by compounding the low-foaming carrier brightening agent, and a potassium chloride galvanizing additive prepared by compounding the softening agent and the brightening agent. The invention also provides a process for galvanizing potassium chloride by using the additive. A plating solution of the potassium chloride galvanizing additive is low-foam, can be stirred by compressed air, and has large permissible current density and high sedimentation velocity. The additive has low consumption. Compared with the first generation and the second generation of potassium chloride galvanizing processes, the process for galvanizing the potassium chloride by using the additive has the advantages that: the additive consumption can be reduced by 30 to 50 percent; a few organic matters are attached to a zinc coating; and corrosion resistance is high.
Description
Technical field
The invention belongs to the electroplating technology field, relate to a kind of low alveolitoid carrier brightening agent and the application on electroplating technology thereof.
Background technology
The muriate acid zinc plating developed rapidly in the U.S. from 1967, and early stage tank liquor has developed the chloride galvanizing liquid of low ammonium mixed type and no ammonium later on for containing ammonium and sequestrant class.To the eighties,, developed first-generation Repone K zinc-plating additive along with the research success of new additive agent; This technology bath element is simple, the coating light, and current efficiency is high; Can be directly zinc-plated at ironcasting, high-carbon steel part, carburizing steel part, and wastewater treatment is simple.Existing problems: 1, the high foam of plating bath; 2, the brightening agent consumption is big, and degradation production is many; 3, coating is organic is mingled with morely, and coating fragility is big, and passivation is difficulty relatively, and passive film is easy to change, and corrosion resistance of coating is poor.
Developed s-generation Repone K zinc-plating additive at the beginning of 90 generations.Advantages such as s-generation potassium chloride zinc plating process also has the depletion of additive amount lower except having the galvanized characteristics of first-generation Repone K, and coating luminance brightness height and fragility are lower.Existing problems: though 1, foam is zinc-plated lower than first-generation Repone K, because it is the organic solvent froth breaking that leans in the brightening agent, can not adopt pneumatic blending; 2, main brightener o-chlorobenzaldehyde and verivate less stable thereof are if plating bath is with ydrogen peroxide 50 or potassium permanganate deironing (Fe
2+) time, the key light agent in the plating bath also can be destroyed; When 3, zinc coating was color blunt, membranous layer binding force was poor, and demoulding, so s-generation Repone K easily is zinc-plated relatively to be suitable for silvery white passivation or blue white passivation, and is not suitable for chromatic passivation; 4, the solidity to corrosion behind the zinc coating passivation (neutral salt spray test) is not as the zinc-plated and alkaline zinc plating of cyaniding.Therefore limited the application of its industry of having relatively high expectations in the zinc coating solidity to corrosion.
Summary of the invention
To above-mentioned technical problem, an object of the present invention is to provide a kind of low alveolitoid carrier brightening agent that contains the non-ionic type organic silicon surfactant;
Another object of the present invention provides a kind of softening agent by the composite gained of above-mentioned low alveolitoid carrier brightening agent;
Another object of the present invention provides a kind of brightening agent by the composite gained of above-mentioned low alveolitoid carrier brightening agent;
Another object of the present invention provides a kind of by above-mentioned softening agent and the composite Repone K zinc-plating additive that obtains of brightening agent;
Another object of the present invention provides a kind ofly utilizes above-mentioned Repone K zinc-plating additive to carry out the galvanized technology of Repone K.
The technical scheme that the present invention adopted is following:
A kind of low alveolitoid carrier brightening agent is calculated by mass percentage, contains 90～95% non-ionics and 5～10% non-ionic type organic silicon surfactant.
Preferably, shown in the structural formula as I of said non-ionic type organic silicon surfactant:
Wherein, R=O (C
2H
4O)
a(C
3H
6O)
b(C
2H
4O)
cCH
3, a=16, b=10, c=15; N=7～9.
Preferably, said non-ionics can be at least a in polyoxyethylene octylphenol ether (EO 50～100), lauryl alcohol Soxylat A 25-7 (EO 50～100), the isomerous tridecanol polyoxyethylene ether (EO 50～100).
A kind of softening agent is measured by mass percentage, contains following component: low alveolitoid carrier brightening agent 10～15%, and Sodium Benzoate 6～15%, solubility promoter 5～10%, surplus is a water; Said solubility promoter is at least a in methyl alcohol, ethanol, ethylene glycol ethyl ether, the Virahol.
A kind of brightening agent is measured by mass percentage, contains following component: main brightener 3-6%, and low alveolitoid carrier brightening agent 5～10%, solubility promoter 5～10%, surplus is a water; Said solubility promoter is at least a in methyl alcohol, ethanol, ethylene glycol ethyl ether, the Virahol.
Preferably, said main brightener is at least a in the reactant of o-chlorobenzaldehyde, BENZALACETONE, o-chlorobenzaldehyde and BENZALACETONE, and wherein, the chemical formula of the reactant of said o-chlorobenzaldehyde and BENZALACETONE is shown in II:
A kind of Repone K zinc-plating additive comprises above-mentioned softening agent and brightening agent.
A kind of potassium chloride zinc plating process is characterized in that, contains above-mentioned Repone K zinc-plating additive in the used electroplate liquid.
Preferably, the galvanized electroplating technical conditions of said Repone K is: temperature is 10～50 ℃, pH4.8～5.6, and the rack plating current density is 0.5～4 ampere/square decimeter, barrel plating strength of current is 100～200 amperes/every barrel.
Preferably, in the electroplating process, electroplate liquid adopts pressurized air to stir and continuous filtration, per hour electroplate liquid is filtered 1～4 time.
Beneficial effect of the present invention is:
(1) use the plating bath of zinc-plated softening agent of Repone K of the present invention and brightening agent to hang down bubble; Can stir with pressurized air, allow current density big, Huo Shi groove test current can be brought up to 2A from 1A; The full sheet light of Huo Shi groove test piece, the permission current density can be from 0.5-2A/dm in the production
2Bring up to 0.5-4A/dm
2, sedimentation velocity is fast, at Dk=3A/dm
2The time, average deposition speed reaches 55 μ/h;
(2) through pneumatic blending, can be the main harmful impurity F e in the plating bath
2+Be oxidized to Fe
3+, and remove through the continuous filtration of tank liquor;
(3) the depletion of additive amount is low, compares with the first-generation, s-generation potassium chloride zinc plating process, and the depletion of additive amount can reduce 30-50%;
(4) zinc coating organism folder attaches few; Zinc coating cooperates the trivalent chromium bright blue passivation with protective material; Solidity to corrosion (neutral salt spray test) >=96 hour; Cooperate the trivalent chromium colorful passivation with protective material, solidity to corrosion (neutral salt spray test) >=160 hour surpasses the zinc-plated solidity to corrosion with the passivation of no cyanogen alkali zinc trivalent chromium of cyaniding.
Embodiment
Below in conjunction with embodiment the present invention is further described, but is not limited thereto.As do not have specified otherwise, used in following examples " % " all refers to mass percent.
Use the low bubble of plating bath of zinc-plated softening agent of Repone K of the present invention and brightening agent; Can stir with pressurized air, allow current density big, Huo Shi groove test current can be brought up to 2A from 1A; The full sheet light of Huo Shi groove test piece, the permission current density can be from 0.5-2A/dm in the production
2Bring up to 0.5-4A/dm
2, sedimentation velocity is fast, at Dk=3A/dm
2The time, average deposition speed reaches 55 μ/h.It is as shown in table 1 to use softening agent of the present invention and brightening agent to carry out the electroplate liquid formulation and the processing condition of potassium chloride zinc plating process.Certainly, in those skilled in the art's understanding scope, softening agent of the present invention and brightening agent also can be used for other potassium chloride zinc plating process.
The electroplate liquid formulation of table 1 potassium chloride zinc plating process and processing condition
Softening agent is formed: low alveolitoid carrier brightening agent 10～15%, Sodium Benzoate 6～15%, solubility promoter 5～10%, and surplus is a water;
Brightening agent is formed: main brightener 3～6%, low alveolitoid carrier brightening agent 5～10%, solubility promoter 5～10%, surplus are water;
Wherein, Above-mentioned low alveolitoid carrier brightening agent is made up of non-ionics and non-ionic type organic silicon surfactant; Said non-ionics is polyoxyethylene octylphenol ether (EO 50～100); Lauryl alcohol Soxylat A 25-7 (EO 50～100), at least a in the isomerous tridecanol polyoxyethylene ether (EO 50～100); Shown in the structural formula as I of said non-ionic type organic silicon surfactant:
Wherein, R=O (C
2H
4O)
a(C
3H
6O)
b(C
2H
4O)
cCH
3, a=16, b=10, c=15; N=7～9.
Said main brightener is at least a in the reactant of o-chlorobenzaldehyde, BENZALACETONE, o-chlorobenzaldehyde and BENZALACETONE, and wherein, the chemical formula of the reactant of said o-chlorobenzaldehyde and BENZALACETONE is shown in II:
Said solubility promoter is at least a in methyl alcohol, ethanol, ethylene glycol ethyl ether, the Virahol.
The concrete operations step that the electroplate liquid of use table 1 carries out potassium chloride zinc plating process is:
Galvanizing process flow:
Zinc-plated part reaches the standard grade → and electrochemical deoiling → UW oil removing → catholyte oil removing, scale removal → washing * 2 → acid deoiling → washing * 2 → anode electrolysis oil removing → washing * 2 → acid activation → washing * 2 → Repone K be zinc-plated → and washing * 2 → UW washing → rare nitric acid bright dipping → washing * 2 → SF-571 trivalent chromium coloured silk blunt (or the SF-572 trivalent chromium bright blue is blunt) → washing * 2 → pure water washes → hot water wash (50 ℃) → blowing → oven dry → time extension.
Embodiment 1
The electroplate liquid formulation and the processing condition of potassium chloride zinc plating process are as shown in table 2:
Table 2
Softening agent is formed: and 10% low alveolitoid carrier brightening agent (comprise 0.5% non-ionic type organic silicon surfactant, 9.5% isomerous tridecanol polyoxyethylene ether, EO=100), 6% Sodium Benzoate, 5% methyl alcohol, surplus is a water;
Brightening agent is formed: 3% o-chlorobenzaldehyde, 5.3% low alveolitoid carrier brightening agent (comprise 0.3% non-ionic type organic silicon surfactant, 5% isomerous tridecanol polyoxyethylene ether, EO=50), 5% methyl alcohol, surplus is a water;
Wherein, the structural formula of above-mentioned non-ionic type organic silicon surfactant is:
R＝O(C
2H
4O)
a(C
3H
6O)
b(C
2H
4O)
cCH
3，a＝16，b＝10，c＝15；n＝7。
Adopt Repone K galvanization liquid prescription and the processing condition of embodiment 1 to carry out the test of Huo Shi groove, plating bath does not carry out pressurized air and stirs, and the full sheet crow of Huo Shi groove test piece light is gloomy, and plating bath adopts pressurized air to stir, the full sheet light of Huo Shi groove test piece.
Embodiment 2
The electroplate liquid formulation and the processing condition of potassium chloride zinc plating process are as shown in table 3:
Table 3
Softening agent is formed: 10.8% low alveolitoid carrier brightening agent (comprising 0.8% non-ionic type organic silicon surfactant, 10% isomerous tridecanol polyoxyethylene ether EO=100), and 7% Sodium Benzoate, 6% ethanol, surplus is a water;
Brightening agent is formed: 4% BENZALACETONE, 6.4% low alveolitoid carrier brightening agent (comprising 0.4% non-ionic type organic silicon surfactant, 6% isomerous tridecanol polyoxyethylene ether EO=50), and 6% ethanol, surplus is a water;
Wherein, the structural formula of above-mentioned non-ionic type organic silicon surfactant is:
R＝O(C
2H
4O)
a(C
3H
6O)
b(C
2H
4O)
cCH
3，a＝16，b＝10，c＝15；n＝8。
Adopt Repone K galvanization liquid prescription and the processing condition of embodiment 2 to carry out the test of Huo Shi groove, plating bath does not carry out pressurized air and stirs, and the full sheet crow of Huo Shi groove test piece light is gloomy, and plating bath adopts pressurized air to stir, the full sheet light of Huo Shi groove test piece.
Embodiment 3
The electroplate liquid formulation and the processing condition of potassium chloride zinc plating process are as shown in table 4:
Table 4
Softening agent is formed: 10% low alveolitoid carrier brightening agent (comprising 0.7% non-ionic type organic silicon surfactant, 9.3% polyoxyethylene octylphenol ether EO=100), and 8% Sodium Benzoate, 8% ethylene glycol ethyl ether, surplus is a water;
Brightening agent is formed: 5% o-chlorobenzaldehyde and BENZALACETONE reactant, 10% low alveolitoid carrier brightening agent (comprising 0.5% non-ionic type organic silicon surfactant, 9.5% lauryl alcohol Soxylat A 25-7 EO=50), and 7% ethylene glycol ethyl ether, surplus is a water;
Wherein, the structural formula of o-chlorobenzaldehyde and BENZALACETONE reactant is:
The structural formula of non-ionic type organic silicon surfactant is:
R＝O(C
2H
4O)
a(C
3H
6O)
b(C
2H
4O)
cCH
3，a＝16，b＝10，c＝15；n＝9。
Adopt Repone K galvanization liquid prescription and the processing condition of embodiment 3 to carry out the test of Huo Shi groove, plating bath does not carry out pressurized air and stirs, and the full sheet crow of Huo Shi groove test piece light is gloomy, and plating bath adopts pressurized air to stir, the full sheet light of Huo Shi groove test piece.
Embodiment 4
The electroplate liquid formulation and the processing condition of potassium chloride zinc plating process are as shown in table 5:
Table 5
Softening agent is formed: 12.6% low alveolitoid carrier brightening agent (comprising 1% non-ionic type organic silicon surfactant, 11.6% polyoxyethylene octylphenol ether EO=100), and 10% Sodium Benzoate, 8% Virahol, surplus is a water;
Brightening agent is formed: 4% o-chlorobenzaldehyde, 2% BENZALACETONE, 10% low alveolitoid carrier brightening agent (comprising 0.3% non-ionic type organic silicon surfactant, 9.7% polyoxyethylene octylphenol ether EO=50), and 8% Virahol, surplus is a water;
Wherein, the structural formula of non-ionic type organic silicon surfactant is:
R＝O(C
2H
4O)
a(C
3H
6O)
b(C
2H
4O)
cCH
3，n＝9，a＝16，b＝10，c＝15。
Adopt Repone K galvanization liquid prescription and the processing condition of embodiment 4 to carry out the test of Huo Shi groove, plating bath does not carry out pressurized air and stirs, and the full sheet crow of Huo Shi groove test piece light is gloomy, and plating bath adopts pressurized air to stir, the full sheet light of Huo Shi groove test piece.
Implement 5
The electroplate liquid formulation and the processing condition of potassium chloride zinc plating process are as shown in table 6
Table 6
Softening agent is formed: 15% low alveolitoid carrier brightening agent (comprising 1% non-ionic type organic silicon surfactant, 14% lauryl alcohol Soxylat A 25-7 EO=100), and 15% Sodium Benzoate, 10% ethylene glycol ethyl ether, surplus is a water;
Brightening agent is formed: 6% BENZALACETONE, and 8% low alveolitoid carrier brightening agent (comprising 0.4% non-ionic type organic silicon surfactant, 7.6% lauryl alcohol Soxylat A 25-7 EO=50), 10% ethylene glycol ethyl ether, surplus is a water;
Wherein, the structural formula of non-ionic type organic silicon surfactant is:
R＝O(C
2H
4O)
a(C
3H
6O)
b(C
2H
4O)
cCH
3，a＝16，b＝10，c＝15；n＝8。
Adopt Repone K galvanization liquid prescription and the processing condition of embodiment 5 to carry out the test of Huo Shi groove, plating bath does not carry out pressurized air and stirs, and the full sheet crow of Huo Shi groove test piece light is gloomy, and plating bath adopts pressurized air to stir, the full sheet light of Huo Shi groove test piece.
The performance test of the embodiment of the invention 1～5 used electroplate liquid:
1. current efficiency: adopt weighting method, current density 1A/dm
2, current efficiency is greater than 97.86%.
2. sedimentation velocity: at Dk=3A/dm
2, average deposition speed is 55 μ m/h.
3. solution dispersibility: the test of Huo Shi groove, electric current 1A is with 8 method test results: 39.09%.
4. covering power: testing method is the endoporus method, and its inwall all has coating.
The test of the embodiment of the invention 1～5 gained coating performance:
1, binding force of cladding material test
(1) pliability test:
(100 * 50mm) through pre-treatment, adopts the zinc-plated 8-10 μ of the zincincation m of embodiment 1～5, with the extremely fracture of test piece alternating bending of coating, splits and locates no dezincify layer, and coating does not separate with matrix to test two light A3 steel plates that employing thickness is 1mm.
(2) thermal shock test:
It is workpiece that the stamping forming loudspeaker of soft steel are adopted in experiment, and zinc-plated 8-10 μ m after pre-treatment was placed on the workpiece of coating in 200 ℃ the baking oven insulation 1 hour, dropped into immediately after the taking-up in the cold water, and coating does not bubble and peels.
2, the solidity to corrosion of zinc coating
(1) the stamping forming loudspeaker of experiment employing soft steel are workpiece, after pre-treatment, and zinc-plated 8-10 μ m; Through rare nitric acid bright dipping, the SF-571 trivalent chromium colour passivator passivation that employing three inspires confidence in company adds sealing; Timeliness is carried out neutral salt spray test after 48 hours; Through 160 hours, its surface white rust＜5% is qualified.
(2) experiment workpiece and zincincation are with (1), and zinc-plated the SF-572 trivalent chromium bright blue passivator passivation that employing three inspires confidence in company adds sealing after rare nitric acid is shared the same light, and timeliness is carried out neutral salt spray test after 48 hours, through 96 hours, its surface white rust＜5% is qualified.
Claims (10)
1. one kind low alveolitoid carrier brightening agent is calculated by mass percentage, contains 90 ~ 95% non-ionics and 5 ~ 10% non-ionic type organic silicon surfactant.
2. according to the said a kind of low alveolitoid carrier brightening agent of claim 1, it is characterized in that the structural formula of said non-ionic type organic silicon surfactant is shown in I:
Wherein, R=O (C
2H
4O)
a(C
3H
6O)
b(C
2H
4O)
cCH
3, a=16, b=10, c=15; N=7 ~ 9.
3. according to the said a kind of low alveolitoid carrier brightening agent of claim 1; It is characterized in that said non-ionics can be at least a in polyoxyethylene octylphenol ether (EO50～100), lauryl alcohol Soxylat A 25-7 (EO50～100), the isomerous tridecanol polyoxyethylene ether (EO50～100).
4. a softening agent is measured by mass percentage, contains following component: low alveolitoid carrier brightening agent 10 ~ 15%, and Sodium Benzoate 6 ~ 15%, solubility promoter 5 ~ 10%, surplus is a water; Wherein, said low alveolitoid carrier brightening agent is each described low alveolitoid carrier brightening agent of claim 1 ~ 3, and said solubility promoter is at least a in methyl alcohol, ethanol, ethylene glycol ethyl ether, the Virahol.
5. a brightening agent is measured by mass percentage, contains following component: main brightener 3 ~ 6%, and low alveolitoid carrier brightening agent 5 ~ 10%, solubility promoter 5 ~ 10%, surplus is a water; Wherein, said low alveolitoid carrier brightening agent is each described low alveolitoid carrier brightening agent of claim 1 ~ 3, and said solubility promoter is at least a in methyl alcohol, ethanol, ethylene glycol ethyl ether, the Virahol.
6. according to the said a kind of brightening agent of claim 5; It is characterized in that; Said main brightener is at least a in the reactant of o-chlorobenzaldehyde, BENZALACETONE, o-chlorobenzaldehyde and BENZALACETONE; Wherein, the chemical formula of the reactant of said o-chlorobenzaldehyde and BENZALACETONE is shown in II:
7. a Repone K zinc-plating additive is characterized in that, comprises the softening agent of claim 4 and the brightening agent of claim 5.
8. a potassium chloride zinc plating process is characterized in that, contains the described Repone K zinc-plating additive of claim 7 in the used electroplate liquid.
9. a kind of potassium chloride zinc plating process according to claim 8 is characterized in that, the electroplating technique condition is: temperature is 10 ~ 50 ℃, pH4.8 ~ 5.6, and the rack plating current density is 0.5 ~ 4 ampere/square decimeter, barrel plating strength of current is 100 ~ 200 amperes/every barrel.
10. according to Claim 8 or 9 described a kind of potassium chloride zinc plating process, it is characterized in that in the electroplating process, electroplate liquid adopts pressurized air to stir and continuous filtration, per hour electroplate liquid is filtered 1 ~ 4 time.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104060303A (en) * | 2014-06-25 | 2014-09-24 | 滨中元川金属制品（昆山）有限公司 | Salt-spray-resistant galvanizing technique |
| CN107299364A (en) * | 2017-06-07 | 2017-10-27 | 常州富思通管道有限公司 | A kind of zinc-plating brightener and preparation method thereof |
| CN108149283A (en) * | 2017-11-29 | 2018-06-12 | 武汉风帆电化科技股份有限公司 | A kind of zinc-plated low soaked dissolubility electroplate liquid and preparation method thereof |
| CN108914169A (en) * | 2018-09-03 | 2018-11-30 | 太康县明硕化工有限公司 | A kind of sylvite galvanized carrier walks agent and preparation method thereof |
| CN110318076A (en) * | 2019-07-17 | 2019-10-11 | 安徽启明表面技术有限公司 | The preparation method of zinc-plating brightener |
| CN110684997A (en) * | 2019-10-10 | 2020-01-14 | 广州三孚新材料科技股份有限公司 | Zinc-plating electroplating liquid and preparation method thereof |
| CN112176368A (en) * | 2020-09-08 | 2021-01-05 | 武汉奥邦表面技术有限公司 | Potassium chloride acidic zinc plating electroplating solution and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104060303A (en) * | 2014-06-25 | 2014-09-24 | 滨中元川金属制品（昆山）有限公司 | Salt-spray-resistant galvanizing technique |
| CN107299364A (en) * | 2017-06-07 | 2017-10-27 | 常州富思通管道有限公司 | A kind of zinc-plating brightener and preparation method thereof |
| CN108149283A (en) * | 2017-11-29 | 2018-06-12 | 武汉风帆电化科技股份有限公司 | A kind of zinc-plated low soaked dissolubility electroplate liquid and preparation method thereof |
| CN108914169A (en) * | 2018-09-03 | 2018-11-30 | 太康县明硕化工有限公司 | A kind of sylvite galvanized carrier walks agent and preparation method thereof |
| CN110318076A (en) * | 2019-07-17 | 2019-10-11 | 安徽启明表面技术有限公司 | The preparation method of zinc-plating brightener |
| CN110684997A (en) * | 2019-10-10 | 2020-01-14 | 广州三孚新材料科技股份有限公司 | Zinc-plating electroplating liquid and preparation method thereof |
| CN112176368A (en) * | 2020-09-08 | 2021-01-05 | 武汉奥邦表面技术有限公司 | Potassium chloride acidic zinc plating electroplating solution and application thereof |
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