CN102352521A - Environment-friendly barrel-plating type trivalent chromium plating solution and barrel-plating method thereof - Google Patents
Environment-friendly barrel-plating type trivalent chromium plating solution and barrel-plating method thereof Download PDFInfo
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- CN102352521A CN102352521A CN2011103526034A CN201110352603A CN102352521A CN 102352521 A CN102352521 A CN 102352521A CN 2011103526034 A CN2011103526034 A CN 2011103526034A CN 201110352603 A CN201110352603 A CN 201110352603A CN 102352521 A CN102352521 A CN 102352521A
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Abstract
The invention provides an environment-friendly barrel-plating type trivalent chromium plating solution and a barrel-plating method thereof, belonging to the field of a plating process. Aiming at the serious problems of large toxicity, heavy pollution, difficult wastewater treatment and the like due to the existence of hexavalent chromium in the existing barrel-plating process for plating chromium, the invention develops an environment-friendly trivalent chromium plating solution suitable for barrel-plating application and a barrel-plating method thereof. The plating solution is mainly prepared from a main salt, a complexing agent, a stabilizing agent, a wetting agent, a conducting salt, a buffering agent and water and also comprises a displacement agent. The invention has the advantages of cleanness and no pollution, and a plating layer has uniform and bright appearance and high corrosion resistance; and in the process provided by the invention, the acidity control is moderate, so that the phenomenon of dissolution of the plating layer can not appear even if the power is switched off. After the displacement agent is introduced into the environment-friendly trivalent chromium plating solution provided by the invention, the displacement and dispersion capabilities of the plating layer can be effectively improved, and the current efficiency and the rate of finished products can be effectively improved. The plating solution is suitable for barrel-plating operation of trivalent chromium on a workpiece.
Description
Invention field
The present invention relates to a kind of electroplating technology, in particular, relate to a kind of barrel plating type trivalent chromium plating technology.
Background technology
Chromium coating has good hardness, wear resistance, solidity to corrosion and ornamental, is that electroplating industry is used one of the widest plating.What but electrodeposited chromium mainly adopted at present is rack plating technology, extremely rare on barrel plating is used, and has so just limited the application of chrome-plated process on finding is electroplated.Study carefully its major cause and be because chrome-plated process walks, dispersive ability is poor, through regular meeting occur low district plating lid less than situation.Electroplate even if traditional barrel plating technology also can only be used for some simple parts that do not have low district, occur coating acid dissolving when particularly cutting off the power supply easily.Resulting corrosion resistance of coating is poor, coating is black partially, and overall cost is very high.
And barrel plating technology contains sexavalent chrome, exist toxicity big, pollute serious problems such as weight, wastewater treatment difficulty.The existence of the problems referred to above forces chromium barrel plating technology can't obtain excellent popularization and application always.
Therefore, develop the environmental protection trivalent chromium plating technology that a kind of suitable barrel plating uses and just just crucial meaning has been arranged.
Summary of the invention
To the problems referred to above, the present invention provides a kind of environmental protection barrel plating type trivalent chromium plating liquid and barrel plating method thereof.
First purpose of the present invention provides a kind of environmental protection barrel plating type trivalent chromium plating liquid, and this electroplate liquid cleanliness without any pollution in electroplating process has splendid dispersive ability.
In order to realize first purpose of the present invention, the invention provides a kind of environmental protection barrel plating type trivalent chromium plating liquid, this electroplate liquid mainly is made up of main salt, complexing agent, stablizer, wetting agent, conducting salt, buffer reagent and water, also includes the agent that walks; Said main salt is at least a in chromium sulphate or the potassium chromium sulfate; Said complexing agent is a formic acid; At least a in acetate and tribromoacetic acid and the salt thereof; Said stablizer is a Padil; Mercaptosuccinic acid sodium; At least a in sodium sorbate and the sodium hypophosphite; Said wetting agent is an alkylphenol polyoxyethylene; At least a in the hexadecyl diethanolamine Soxylat A 25-7; The said agent that walks is the acrylate homopolymer sodium salt; Sodium vinyl sulfonate; Thiourea derivative with contain in the C=S heterogeneous ring compound at least a; Said buffer reagent is a boric acid; Sodium Tetraborate; At least a in sodium phosphate and the Trisodium Citrate, said conducting salt is a vitriolate of tartar; Sodium sulfate; At least a in the ammonium sulfate.
The present invention also can do following improvement:
The said agent content that walks is 1g/L～120g/L; The C=S heterogeneous ring compound is α-thiophene derivant in the said agent that walks.
Said conducting salt content is 100g/L～200g/L.
Said main salts contg is 10g/L～120g/L.
Said complexing agent content is 1g/L～120g/L.
Said stabiliser content is 1g/L～120g/L.
Said humectant content is 1g/L～8g/L.
Said buffer content is 1g/L～120g/L.
Another object of the present invention is to provide a kind of environmental protection sulfuric acid type trivalent chromium barrel plating method of using the described barrel plating environmental protection of claim 1 barrel plating type trivalent chromium plating liquid, uses this method in the barrel plating process, current efficiency to be improved significantly.
In order to realize second purpose of the present invention, a kind of environmental protection sulfuric acid type trivalent chromium barrel plating method provided by the invention may further comprise the steps:
(1) with workpiece with pickling and washing;
(2) carry out barrel plating with above-mentioned a kind of environmental protection barrel plating type trivalent chromium plating liquid; Condition is: temperature is that 40-60 ℃, cathode current density are that 0.1-15ASD, pH value are 3-6; 1-30 minute barrel plating time; The rotating speed of cylinder is 0.5-10 rev/min, and the anode that uses is DSA (Dimensionally Stable Anode) iridium titanium coated anode;
(3) with water plating piece is cleaned up, dry up then.
The present invention also can do following improvement:
In the step (2), the barrel plating condition is: temperature is that 45-55 ℃, barrel plating cathode current density are 2-5ASD (average current density), and rack plating barrel plating current density is that 6-15, pH value are 4-5, and 20-30 minute barrel plating time, the rotating speed of cylinder is 1-5 rev/min.
Compared with prior art, the beneficial effect that has of the present invention is:
1) adopt a kind of environmental protection barrel plating type trivalent chromium plating liquid of the present invention and barrel plating method thereof, cleanliness without any pollution, the coating outward appearance is light evenly, and solidity to corrosion doubles than conventional barrel plating chromium at least;
2) a kind of environmental protection sulfuric acid type trivalent chromium barrel plating method of the present invention, not fluorine-containing silicic acid, its technology acidity control is moderate, also the coating dissolution phenomena can not occur even have a power failure;
3) can know through embodiment, after a kind of environmental protection barrel plating type trivalent chromium plating liquid of the present invention is introduced the agent that walks, can improve effectively that coating walks and dispersive ability;
4) a kind of environmental protection sulfuric acid type trivalent chromium barrel plating method of the present invention can effectively improve current efficiency, reaches about 30%, improves yield rate 80-90% simultaneously, is applicable to barrel plating trivalent chromium on workpiece.
Embodiment
Below in conjunction with specific embodiment the present invention is done further detailed description, but do not constitute to any restriction of the present invention.
Adopt following condition to carry out barrel plating experiment (plating thickness and solidity to corrosion test): coating bath is the cylinder chrome-plating bath, 6 inches * 8 inches of cylinder sizes (can adorn product 1000 grams-2000 grams); Electroplating object is nickel plating irony hexagonal head bolt, and nickel layer thickness is 3 μ m; The pH value is 5; Drum rotational speed is 2rpm; Electroplating time is 30min; Electroplating temperature is 50 ℃; Current density is 3ASD; Anode is a DSA iridium titanium coated anode.
Adopt following condition to carry out Hull groove experiment (dispersive ability test): coating bath is a 267ml Hull groove; Electroplating object is 10cm * 6cm nickel plating copper sheet, and nickel layer thickness is 5 μ m; The pH value is 5; Electroplating time is 5min; Electroplating temperature is 50 ℃; Current density is 10ASD; The sun level is a DSA iridium titanium coated anode; Pre-treatment is through chlorohydric acid pickling and washing.
Experiment obtains sample and tests according to following project and method:
1. outward appearance: range estimation.
2. plating thickness: with the same position (getting the compromise position in high district and low district) of thickness tester test plating back nut.
3. solidity to corrosion test: carry out the neutral salt spray test test according to national standard GB 10125-1997.
4. dispersive ability test:
δ
1For apart from 1cm place, Gao Qu edge thickness, δ
2For being the low district of distance 1cm place, edge thickness.
Comparative example 1
Electroplating bath components:
Chromic anhydride: 320-350g/L
Silicofluoric acid: 4.5-5g/L
Sulfuric acid: 0.5-0.6g/L
Surplus is a water
Comparative example 2
Electroplating bath components:
Vitriolate of tartar: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid: 8g/L
Xitix: 30g/L
Glycerin: 2g/L
Boric acid: 60g/L
Surplus is a water
Embodiment 1
Electroplating bath components:
Vitriolate of tartar: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetate/tribromoacetic acid (1: 1: 1): 8g/L
Padil: 30g/L
Alkylphenol polyoxyethylene: 2g/L
Acrylate homopolymer sodium salt: 8g/L
Boric acid: 60g/L
Surplus is a water
Embodiment 2
Electroplating bath components:
Vitriolate of tartar: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetate/tribromoacetic acid (1: 1: 1): 8g/L
Padil: 30g/L
Alkylphenol polyoxyethylene: 2g/L
Thiourea derivative: 8g/L
Boric acid: 60g/L
Surplus is a water
Embodiment 3
Electroplating bath components:
Vitriolate of tartar: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetate/tribromoacetic acid (1: 1: 1): 8g/L
Padil: 30g/L
Alkylphenol polyoxyethylene: 2g/L
α-thiophene derivant: 8g/L
Boric acid: 60g/L
Surplus is a water
Embodiment 4
Electroplating bath components:
Vitriolate of tartar: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetate/tribromoacetic acid (1: 1: 1): 8g/L
Mercaptosuccinic acid sodium: 30g/L
Hexadecyl diethanolamine Soxylat A 25-7: 2g/L
Acrylate homopolymer sodium salt: 8g/L
Boric acid: 60g/L
Surplus is a water
Embodiment 5
Electroplating bath components:
Vitriolate of tartar: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetate/tribromoacetic acid (1: 1: 1): 8g/L
Mercaptosuccinic acid sodium: 30g/L
Hexadecyl diethanolamine Soxylat A 25-7: 2g/L
Thiourea derivative: 8g/L
Boric acid: 60g/L
Surplus is a water
Embodiment 6
Electroplating bath components:
Vitriolate of tartar: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetate/tribromoacetic acid (1: 1: 1): 8g/L
Mercaptosuccinic acid sodium: 30g/L
Hexadecyl diethanolamine Soxylat A 25-7: 2g/L
α-thiophene derivant: 8g/L
Boric acid: 60g/L
Surplus is a water
Embodiment 7
Electroplating bath components:
Vitriolate of tartar: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetate/tribromoacetic acid (1: 1: 1): 8g/L
Padil: 30g/L
Hexadecyl diethanolamine Soxylat A 25-7: 2g/L
α-thiophene derivant: 8g/L
Boric acid: 60g/L
Surplus is a water
Embodiment 8
Electroplating bath components:
Vitriolate of tartar: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetate/tribromoacetic acid (1: 1: 1): 8g/L
Mercaptosuccinic acid sodium: 30g/L
Alkylphenol polyoxyethylene: 2g/L
α-thiophene derivant: 8g/L
Boric acid: 60g/L
Surplus is a water
Embodiment 9
Electroplating bath components:
Sodium sulfate: 250g/L
Chromium sulphate: 40g/L
Formic acid: 5g/L
Sodium sorbate: 10g/L
Alkylphenol polyoxyethylene: 1g/L
Sodium vinyl sulfonate: 5g/L
Sodium Tetraborate: 50g/L
Surplus is a water
Embodiment 10
Electroplating bath components:
Ammonium sulfate: 350g/L
Potassium chromium sulfate: 70g/L
Acetate: 20g/L
Sodium hypophosphite: 50g/L
Hexadecyl diethanolamine Soxylat A 25-7: 5g/L
Acrylate homopolymer sodium salt: 12g/L
Sodium phosphate: 80g/L
Surplus is a water
Embodiment 11
Electroplating bath components:
Sodium sulfate: 100g/L
Chromium sulphate: 10g/L
Formic acid: 1g/L
Sodium sorbate: 10g/L
Alkylphenol polyoxyethylene: 1g/L
Sodium vinyl sulfonate: 1g/L
Sodium Tetraborate: 1g/L
Surplus is a water
Embodiment 12
Electroplating bath components:
Ammonium sulfate: 200g/L
Potassium chromium sulfate: 120g/L
Acetate: 120g/L
Sodium hypophosphite: 10g/L
Hexadecyl diethanolamine Soxylat A 25-7: 8g/L
Acrylate homopolymer sodium salt: 120g/L
Sodium phosphate: 120g/L
Surplus is a water
Embodiment 13
Adopt and carry out barrel plating with embodiment 3 identical electroplate liquids; Pre-treatment is used after chlorohydric acid pickling and washing, and the barrel plating condition: temperature is 40, cathode current density is that 0.1ASD, pH value are 3,1 minute barrel plating time; The rotating speed of cylinder is 10 rev/mins, the DSA iridium titanium coated anode of use;
Embodiment 14
Adopt and carry out barrel plating with embodiment 3 identical electroplate liquids; Pre-treatment is used after chlorohydric acid pickling and washing, and the barrel plating condition: temperature is 60, cathode current density is that 15ASD, pH value are 6,30 minutes barrel plating time; The rotating speed of cylinder is 0.5 rev/min, uses DSA iridium titanium coated anode;
Table 1. table with test results
Comparative example 1 is a barrel plating sexavalent chrome electroplate liquid, and comparative example 2 is conventional sulfuric acid type trivalent chromium plating liquid.Electroplate liquid of the present invention is compared with barrel plating sexavalent chrome technology and conventional sulfuric acid type trivalent chromium plating respectively.
Visible by above-mentioned test result, embodiment 1-12 is because the additive that adopts is different, and its bright appearance, even can reach the chromic effect of barrel plating, and comparative example 2 outward appearances are secretly bright, low district does not cover.Embodiment 1-12 plating bath contains the agent that walks, and comparative example 1 and 2 plating bath do not contain the agent that walks, the negative electrode light district of embodiment 1-12 and dispersive ability (slotted vane) reach 90% or more than, be up to 95%; Much larger than comparative example 1 70% with comparative example 2 80%; The dispersive ability of embodiment 1-12 (slotted vane) reach 35% or more than, be up to 40%, much larger than 20% of comparative example 1 and comparative example 2.This explanation the present invention can significantly improve the ability that walks and the dispersive ability of plating bath through in plating bath, adding the agent that walks.Since the complexing agent that adopts and wetting agent different; The current efficiency of embodiment 1-12 reaches 30%-40%; Greater than comparative example 1 16% with comparative example 2 18%; Because the raising of current efficiency, the thickness and the solidity to corrosion of corresponding coating also are greatly improved, for example; The screw solidity to corrosion (NSST) of embodiment 1-12 reaches as high as 18 hours; Greater than 8 hours and the 6h of comparative example 2 of comparative example 1, the present invention is through adopting different solution compositions in this explanation, obviously improves chromium layer resistance to corrosion.The raising of ability and current efficiency simultaneously because coating walks, the yield rate scope of product is 80%-90%, comparative example 1 and 2 yield rate are 30% and 40% only, make the barrel plating trivalent chromium become possibility.
While is visible by above-mentioned test result, adopts the different parameters condition of barrel plating method of the present invention, and like embodiment 13 and 14, its bright appearance, even can also reach the chromic effect of barrel plating.Negative electrode light district and dispersive ability (slotted vane) reach 90%; Much larger than comparative example 1 70% with comparative example 2 80%; Dispersive ability (slotted vane) reach 35% or more than, much larger than 20% of comparative example 1 and comparative example 2.Its current efficiency reaches more than the 30%-; Greater than comparative example 1 16% with comparative example 2 18%; Because the raising of current efficiency; The thickness and the solidity to corrosion of corresponding coating also are greatly improved; Its screw solidity to corrosion (NSST) reaches as high as 18 hours, greater than 8 hours and the 6h of comparative example 2 of comparative example 1.The raising of ability and current efficiency simultaneously because coating walks, the yield rate scope of product is 85%-90%, comparative example 1 and 2 yield rate are 30% and 40% only, make the barrel plating trivalent chromium become possibility.This explanation adopts this barrel plating method to meet the demands in the parameter condition and range.
In sum, a kind of sulfuric acid type barrel plating trivalent chromium plating liquid provided by the invention and electro-plating method thereof have outward appearance brilliant white, covering power is strong, erosion resistance is good, yield rate is high advantage.
The above embodiments only are the preferred embodiments of the present invention, can not limit interest field of the present invention with this, and therefore, the equivalent variations according to claim of the present invention is done still belongs to the scope that the present invention is contained.
Claims (10)
1. an environmental protection barrel plating type trivalent chromium plating liquid mainly is made up of main salt, complexing agent, stablizer, wetting agent, conducting salt, buffer reagent and water, it is characterized in that: also include the agent that walks; Said main salt is at least a in chromium sulphate or the potassium chromium sulfate; Said complexing agent is a formic acid; At least a in acetate and tribromoacetic acid and the salt thereof; Said stablizer is a Padil; Mercaptosuccinic acid sodium; At least a in sodium sorbate and the sodium hypophosphite; Said wetting agent is an alkylphenol polyoxyethylene; At least a in the hexadecyl diethanolamine Soxylat A 25-7; The said agent that walks is the acrylate homopolymer sodium salt; Sodium vinyl sulfonate; Thiourea derivative with contain in the C=S heterogeneous ring compound at least a; Said buffer reagent is a boric acid; Sodium Tetraborate; At least a in sodium phosphate and the Trisodium Citrate, said conducting salt is a vitriolate of tartar; Sodium sulfate; At least a in the ammonium sulfate.
2. a kind of environmental protection barrel plating type trivalent chromium plating liquid according to claim 1, it is characterized in that: the said agent content that walks is 1g/L～120g/L; The C=S heterogeneous ring compound is α-thiophene derivant in the said agent that walks.
3. a kind of environmental protection barrel plating type trivalent chromium plating liquid according to claim 1, it is characterized in that: said conducting salt content is 100g/L～200g/L.
4. a kind of environmental protection barrel plating type trivalent chromium plating liquid according to claim 1, it is characterized in that: said main salts contg is 10g/L～120g/L.
5. a kind of environmental protection barrel plating type trivalent chromium plating liquid according to claim 1, it is characterized in that: said complexing agent content is 1g/L～120g/L.
6. a kind of environmental protection barrel plating type trivalent chromium plating liquid according to claim 1, it is characterized in that: said stabiliser content is 1g/L～120g/L.
7. a kind of environmental protection barrel plating type trivalent chromium plating liquid according to claim 1, it is characterized in that: said humectant content is 1g/L～8g/L.
8. a kind of environmental protection barrel plating type trivalent chromium plating liquid according to claim 1, it is characterized in that: said buffer content is 1g/L～120g/L.
9. environmental protection barrel plating type trivalent chromium barrel plating method is characterized in that may further comprise the steps:
(1) with workpiece with pickling and washing;
(2) carry out barrel plating with above-mentioned a kind of environmental protection barrel plating type trivalent chromium plating liquid; Condition is: temperature is that 40-60 ℃, cathode current density are that 0.1-15ASD, pH value are 3-6; 1-30 minute barrel plating time; The rotating speed of cylinder is 0.5-10 rev/min, and the anode that uses is DSA (Dimensionally Stable Anode) iridium titanium coated anode;
(3) with water plating piece is cleaned up, dry up then.
10. a kind of environmental protection barrel plating type trivalent chromium barrel plating method according to claim 9; It is characterized in that: in the step (2); The barrel plating condition is: temperature is that 45-55 ℃, barrel plating cathode current density are 2-5ASD; Rack plating barrel plating current density is that 6-15, pH value are 4-5; 20-30 minute barrel plating time, the rotating speed of cylinder is 1-5 rev/min.
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Cited By (8)
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| CN102677111A (en) * | 2012-04-20 | 2012-09-19 | 立兆股份有限公司 | Preparation method of workpiece with bright surface coating layer |
| CN103334149A (en) * | 2013-06-13 | 2013-10-02 | 中国科学院过程工程研究所 | Periodic intermittent-type hard chrome barrel-plating device and use method thereof |
| CN103510096A (en) * | 2012-06-20 | 2014-01-15 | 江苏华宇印涂设备集团有限公司 | Oil transmission roller |
| CN103526245A (en) * | 2013-09-30 | 2014-01-22 | 朱卓敏 | New environment-friendly process for chromium barrel plating after chloride zinc plating |
| CN104789996A (en) * | 2015-04-15 | 2015-07-22 | 吉林莱德化学科技有限公司 | Trivalent chrominm plating electroplating liquid |
| CN105018973A (en) * | 2014-11-27 | 2015-11-04 | 太仓市金鹿电镀有限公司 | Environment-friendly electroplating liquid and electroplating process |
| CN105696028A (en) * | 2014-11-28 | 2016-06-22 | 中国科学院金属研究所 | Trivalent chromium electroplating solution and electroplating method |
| CN107313078A (en) * | 2016-04-27 | 2017-11-03 | 中国科学院金属研究所 | A kind of trivalent chromium plating solution and preparation method thereof |
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| CN102677111A (en) * | 2012-04-20 | 2012-09-19 | 立兆股份有限公司 | Preparation method of workpiece with bright surface coating layer |
| CN102677111B (en) * | 2012-04-20 | 2015-03-11 | 立兆股份有限公司 | Preparation method of workpiece with bright surface coating layer |
| CN103510096A (en) * | 2012-06-20 | 2014-01-15 | 江苏华宇印涂设备集团有限公司 | Oil transmission roller |
| CN103334149A (en) * | 2013-06-13 | 2013-10-02 | 中国科学院过程工程研究所 | Periodic intermittent-type hard chrome barrel-plating device and use method thereof |
| CN103334149B (en) * | 2013-06-13 | 2016-04-27 | 中国科学院过程工程研究所 | A kind of cycle intermittent type rolls hard chromium plating device and using method |
| CN103526245A (en) * | 2013-09-30 | 2014-01-22 | 朱卓敏 | New environment-friendly process for chromium barrel plating after chloride zinc plating |
| CN105018973A (en) * | 2014-11-27 | 2015-11-04 | 太仓市金鹿电镀有限公司 | Environment-friendly electroplating liquid and electroplating process |
| CN105696028A (en) * | 2014-11-28 | 2016-06-22 | 中国科学院金属研究所 | Trivalent chromium electroplating solution and electroplating method |
| CN104789996A (en) * | 2015-04-15 | 2015-07-22 | 吉林莱德化学科技有限公司 | Trivalent chrominm plating electroplating liquid |
| CN107313078A (en) * | 2016-04-27 | 2017-11-03 | 中国科学院金属研究所 | A kind of trivalent chromium plating solution and preparation method thereof |
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