CN102102200A - Phosphorization solution for cathode electrophoresis - Google Patents
Phosphorization solution for cathode electrophoresis Download PDFInfo
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- CN102102200A CN102102200A CN2010105761481A CN201010576148A CN102102200A CN 102102200 A CN102102200 A CN 102102200A CN 2010105761481 A CN2010105761481 A CN 2010105761481A CN 201010576148 A CN201010576148 A CN 201010576148A CN 102102200 A CN102102200 A CN 102102200A
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- phosphatization
- cathode electrophoresis
- phosphorization
- phosphatization liquid
- ability cathode
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Abstract
The invention relates to phosphorization solution for cathode electrophoresis. A phosphorization film with good alkali resistance can be obtained on the surface of steel by a dipping or spraying phosphorization process, and the phosphorization solution is suitable for phosphorization treatment before steel workpiece cathode electrophoresis. The phosphorization solution consists of the following substances: 20 to 50 g/L of zinc salt, 20 to 50 g/L of manganese salt, 150 to 250 g/L of phosphoric acid, 20 to 80 g/L of hydroxylamine sulfate, 15 to 30 g/L of sodium carbonate, 10 to 20 g/L of complexing agent, 1 to 20 g/L of additive, and the balance of water. The phosphorization solution does not contain toxic or harmful substances to the environment such as nickel ions, nitrite, nitrate, fluoride and the like; and the film forming speed is high, the weight of the film is 1.5 to 3mg/m<2>, little sediment is generated in phosphorization, slot distribution and regulation are simple, the phosphorization film is uniform and compact, the crystal is granular, the alkali resistance is good, the P ratio is more than 90 percent, and the phosphorization solution has good mating property with cathode electrophoresis.
Description
Technical field
The invention belongs to the metallic surface chemical treatment method, be specifically related to the phosphatization liquid that a kind of ability cathode electrophoresis is used, be applicable to bonderizing the demanding cathode electro-coating of coating protection.
Background technology
In automobile, household electrical appliances coating process, be important procedure, its objective is and improve erosion resistance and adhesive force of coatings the metal parts phosphatization.Carry out the product of negative electrode cathode electro-coating, for example car, heavy-duty car etc. require its outside plate non-corroding 6 years, no outside plate pitting corrosion 10 years, the corrosion of nothing damage structure 20 years.This has excellent erosion resistance with regard to requiring with the supporting phosphatize phosphate coat of negative electrode ability cathode electrophoresis.
Metal is coated with workpiece as negative electrode in the cathode electro-coating, because electrochemical result, the cathodic area pH value of electric field can reach about 12, and this just requires the phosphatize phosphate coat of metallic surface must possess good alkali resistance.Cathode electro-coating also requires phosphatize phosphate coat will have certain electric conductivity, therefore must strict control phosphatization thickness.The subject matter of the employed phosphatization liquid existence of cathode electro-coating at present has: " P ratio " is low, alkali resistance is poor, contain deleterious materials such as nitrite, nitrate radical, nickel ion, fluorion in the phosphatization liquid, the operating procedure complexity is wayward, and working temperature height, phosphatization sediment are many.
At present existing patent provides the phosphatization liquid of no nickel, no nitrite, but patent CN200810228602 " a kind of non-nickle ion phosphatization liquid that is used for the steel plate processing " contains nitrate, cobalt ion.CN94193230 " phosphatization process of no nickel " contains fluorochemical, nitrate, itrogenous organic substance m-nitrobenzene sulfonate.Nitric acid and sodium chlorate have been used among the CN200410021272 " Low-Temperature Phosphate Liquid of sulfur acid hydroxylamine sulfate accelerator and preparation method thereof ".CN200710034699.3 " is used for the calcic zinc-manganese triple cationic phosphorizing fluid that steel plate and galvanized sheet are handled " and has used nitrate, m-nitrobenzene sodium sulfonate, oxymuriate, and phosphatization temperature is higher.The speed of growth of algae and waterplant can be increased after the nitrate discharging, the water body degradation of streams and lake water can be made.M-nitrobenzene sodium sulfonate is a kind of nitrogenous benzene organism that contains, and causes water pollution.Fluorochemical is a kind of toxic pollutants.Cobalt ion is a kind of toxic heavy metal.Oxymuriate can produce chlorion in phosphatization liquid, influence the solidity to corrosion of phosphatize phosphate coat, and chlorion can become the potential source of corrosion after the application.
The present invention utilizes oxammonium sulfate promotor to be easy to obtain Zn
2Fe (PO
4)
24H
2The characteristics of O (P phase) content height, phosphatize phosphate coat that alkali resistance is strong, and add alkali resistance and the solidity to corrosion that manganese salt, tungstate, molybdate further improve phosphatize phosphate coat, do not use harmful toxic matters such as nickel ion, nitrite, nitrate, fluorochemical, it is good to obtain alkali resistance, the phosphatization liquid good with the ability cathode electrophoresis matching capacity.Phosphatization liquid phosphatization temperature of the present invention is lower, and the phosphatization sediment is few; Open cylinder liquid and add liquid and be a kind of solution, easy to use.
The phosphatization liquid that ability cathode electrophoresis of the present invention is used is achieved through the following technical solutions, and the content of each composition in a premium on currency solution is:
Zinc salt is one or both sums in zinc oxide, the primary zinc phosphate, consumption 20～50g;
Manganese salt is one or both sums of phosphate dihydrogen manganese, manganous carbonate, consumption 20～50g;
Phosphoric acid consumption 150～250g;
Sodium carbonate amount 15～30g;
Additive is one or both sums of sodium wolframate, Sodium orthomolybdate, consumption 1～20g;
Complexing agent is one or both in citric acid, the tartrate, consumption 10～20g;
All the other are water.
A kind of ability cathode electrophoresis of the present invention compound method of phosphatization liquid:
Get zinc salt, the manganese salt of specified amount, add the phosphoric acid of entry and specified amount, be stirred well to dissolving; The complexing agent, yellow soda ash, oxammonium sulfate, the additive that add specified amount respectively fully add water to prescribed volume after the dissolving.
A kind of ability cathode electrophoresis of the present invention phosphatization liquid phosphatization liquid using method:
Add water by the concentration of phosphatization liquid hold-up 100ml/L and be mixed with the phosphatization working fluid, measure and adjust phosphatization working fluid free acidity, total acidity 20～30 points 0.8～1.5.25～45 ℃ of Heating temperatures, phosphating time 2～6 minutes.
Carry out bonderizing with a kind of ability cathode electrophoresis provided by the invention with phosphatization liquid phosphatization liquid, phosphorization filming speed is fast, and the phosphatize phosphate coat crystallization is careful, and alkali resistance is good.This phosphatize phosphate coat ℃ floods 5min in (30.0 ± 0.5) in 0.1mol/LNaOH solution, unit surface phosphatize phosphate coat weightlessness is less than 5%, and is suitable with nickelic phosphatize phosphate coat.Therefore the phosphatize phosphate coat that obtains of the present invention has good alkali resistance, has good matching capacity with cathode electro-coating.
Embodiment:
Embodiment 1:
Zinc oxide 20g/L, phosphate dihydrogen manganese 30g/L, phosphatase 11 50g/L,, citric acid 10g/L, oxammonium sulfate 20g/L, sodium wolframate 10g/L, Sodium orthomolybdate 1g/L, yellow soda ash 15g/L, all the other are water.
Phosphatization liquid free acidity is 8, and total acidity is 220.40 ℃ of phosphatizations 3 minutes, the phosphatize phosphate coat outward appearance that obtains was even, fine and close, and the phosphatization crystallization is a particulate state, the heavy 2.8mg/m of film
2, phosphatize phosphate coat alkali resistance 2.6%, the P ratio is 96%.
Embodiment 2:
Zinc oxide 30g/L, manganous carbonate 20g/L, phosphatase 11 70g/L, tartrate 10g/L, oxammonium sulfate 50g/L, sodium wolframate 20g/L, yellow soda ash 22g/L, all the other are water.
Phosphatization liquid free acidity is 12, and total acidity is 280.35 ℃ of phosphatizations 4 minutes, the phosphatize phosphate coat outward appearance that obtains was even, fine and close, and the phosphatization crystallization is a particulate state, the heavy 1.6mg/m of film
2, phosphatize phosphate coat alkali resistance 4.8%, the P ratio is 91%.
Embodiment 3:
Zinc oxide 10g/L, primary zinc phosphate 40g/L, phosphate dihydrogen manganese 50g/L, 85% phosphoric acid 250g/L, tartrate 10g/L, citric acid 10g/L,, oxammonium sulfate 80g/L, sodium wolframate 15g/L, Sodium orthomolybdate 5g/L, yellow soda ash 30g/L surplus be water.
Phosphatization liquid free acidity is 10, and total acidity is 250.25 ℃ of phosphatizations 6 minutes, the phosphatize phosphate coat outward appearance that obtains was even, fine and close, and the phosphatization crystallization is a particulate state, the heavy 2.1mg/m of film
2, phosphatize phosphate coat alkali resistance 3.8%, the P ratio is 92%.
Embodiment 4:
Zinc oxide 15g/L, primary zinc phosphate 20g/L, manganous carbonate 10g/L, phosphate dihydrogen manganese 10g/L, phosphoric acid 200g/L, citric acid 5g/L, tartrate 10g/L, oxammonium sulfate 20g/L, Sodium orthomolybdate 5g/L, yellow soda ash 27g/L, all the other are water.
Phosphatization liquid free acidity is 12, and total acidity is 230.30 ℃ of phosphatizations 5 minutes, the phosphatize phosphate coat outward appearance that obtains was even, fine and close, and the phosphatization crystallization is a particulate state, the heavy 2.3mg/m of film
2, phosphatize phosphate coat alkali resistance 2.4%, the P ratio is 94%.
Embodiment 5:
Primary zinc phosphate 50g/L, manganous carbonate 10g/L, phosphate dihydrogen manganese 20g/L, phosphatase 11 50g/L, citric acid 20g/L, oxammonium sulfate 80g/L, sodium wolframate 10g/L, yellow soda ash 15～30g/L, all the other are water.
Phosphatization liquid free acidity is 15, and total acidity is 270.40 ℃ of phosphatizations 2 minutes, the phosphatize phosphate coat outward appearance that obtains was even, fine and close, and the phosphatization crystallization is a particulate state, the heavy 3.0mg/m of film
2, phosphatize phosphate coat alkali resistance 2.2%, the P ratio is 96%.
Embodiment 6:
Primary zinc phosphate 50g/L, manganous carbonate 30g/L, phosphoric acid 200g/L, tartrate 20g/L, oxammonium sulfate 80g/L, sodium wolframate 15g/L, Sodium orthomolybdate 3g/L, yellow soda ash 25g/L, all the other are water.
Phosphatization liquid free acidity is 13, and total acidity is 250.45 ℃ of phosphatizations 3 minutes, the phosphatize phosphate coat outward appearance that obtains was even, fine and close, and the phosphatization crystallization is a particulate state, the heavy 1.6mg/m of film
2, phosphatize phosphate coat alkali resistance 3%, the P ratio is 95%.
Embodiment 7:
Zinc nitrate 40g/L, phosphate dihydrogen manganese 30g/L, phosphoric acid 200g/L, citric acid 5g/L, tartrate 5g/L, oxammonium sulfate 50g/L, oxammonium sulfate 30g/L, sodium wolframate 15g/L, Sodium orthomolybdate 1g/L, yellow soda ash 30g/L, all the other are water.
Phosphatization liquid free acidity is 9, and total acidity is 255.30 ℃ of phosphatizations 4 minutes, the phosphatize phosphate coat outward appearance that obtains was even, fine and close, and the phosphatization crystallization is a particulate state, the heavy 1.5mg/m of film
2, phosphatize phosphate coat alkali resistance 4.5%, the P ratio is 92%.
Embodiment 8:
Zinc oxide 10g/L, primary zinc phosphate 10g/L, manganous carbonate 10g/L, phosphate dihydrogen manganese 40g/L, phosphatase 11 50g/L, citric acid 15g/L, tartrate 5g/L, oxammonium sulfate 60g/L, sodium wolframate 18g/L, Sodium orthomolybdate 1g/L, yellow soda ash 28g/L, all the other are water.
Phosphatization liquid free acidity is 12, and total acidity is 240.40 ℃ of phosphatizations 3 minutes, the phosphatize phosphate coat outward appearance that obtains was even, fine and close, and the phosphatization crystallization is a particulate state, the heavy 2.6mg/m of film
2, phosphatize phosphate coat alkali resistance 3.3%, the P ratio is 95%.
Embodiment 9:
Zinc oxide 10g/L, primary zinc phosphate 10g/L, manganous carbonate 20g/L, phosphate dihydrogen manganese 10g/L, phosphatase 11 80g/L, citric acid 5g/L, tartrate 15g/L, oxammonium sulfate 50g/L, Sodium orthomolybdate 2g/L, yellow soda ash 29g/L, all the other are water.
Phosphatization liquid free acidity is 12, and total acidity is 250.35 ℃ of phosphatizations 5 minutes, the phosphatize phosphate coat outward appearance that obtains was even, fine and close, and the phosphatization crystallization is a particulate state, the heavy 1.6mg/m of film
2, phosphatize phosphate coat alkali resistance 4.7%, the P ratio is 91%.
Embodiment 10:
Primary zinc phosphate 20g/L, manganous carbonate 10g/L, phosphate dihydrogen manganese 40g/L, phosphatase 11 50g/L, tartrate 20g/L, oxammonium sulfate 60g/L, sodium wolframate 18g/L, Sodium orthomolybdate 2g/L, yellow soda ash 26g/L, all the other are water.
Phosphatization liquid free acidity is 8, and total acidity is 260.45 ℃ of phosphatizations 5 minutes, the phosphatize phosphate coat outward appearance that obtains was even, fine and close, and the phosphatization crystallization is a particulate state, the heavy 2.8mg/m of film
2, phosphatize phosphate coat alkali resistance 2%, the P ratio is 97%.
Autobody sheet carries out bonderizing and carries out cathode electro-coating, ability cathode electrophoresis coat-thickness 20 μ m through phosphatization liquid of the present invention.Detected result is as follows:
1. detect the phosphatize phosphate coat pattern with scanning electronic microscope (SEM)
The phosphatize phosphate coat crystallization is a particulate state as can be seen from Figure of description 1, the about 2 μ m of particle diameter, and uniform particles is fine and closely woven.
2. analyze the phosphatize phosphate coat composition, calculate the P ratio with X-ray diffractometer (XRD)
From Figure of description 2, in the phosphatize phosphate coat Zn is arranged as can be seen
2Fe (PO
4)
24H
2O (P phase) and iron phase, iron phase occurring is that the iron-based body has participated in diffraction because phosphatize phosphate coat is thinner.Zn in the phosphatize phosphate coat
3(PO
4)
24H
2O (H phase) denier almost can't check.P than for P phase diffracted intensity and P mutually with H phase diffracted intensity and ratio.
3. phosphatize phosphate coat alkaline resistance test
Accurate weighing (the W of test plate (panel) after the phosphatization
1) back immerses in the 0.1mol/LNaOH solution, at (30.0 ± 0.5) ℃ following dipping 5min, use washed with de-ionized water, oven dry, the accurate weighing (W in cooling back
2), calculate weightless ratio: (W
1-W
2)/S * 100% is less than 5%.
4. carry out the paint film adhesion check according to GB/T9286-1998 with cross-hatching, reach 1 grade.
5. carry out salt-fog test according to GB/T10125-1997 salt-fog test method
Paint film is not seen paint film bubbling phenomenon through 400 hours salt-fog tests.Paint film is drawn diagonal lines, draw thoroughly to metal base surface, through 48 hours salt-fog tests, corrosion penetration was less than 0.5mm.
6. the quantum of output of phosphatization slag:
Preparation 2L tank liquor is handled steel plate area 1m
2, then phosphatization liquid being filtered, filter residue is above to constant weight at (120 ± 5) ℃ oven dry 2h, puts into moisture eliminator calculating phosphatization slag quantum of output less than 2g/m
2
Claims (8)
1. phosphatization liquid that ability cathode electrophoresis is used, it is made up of following material: zinc salt 20～50g/L, manganese salt 20～50g/L, phosphatase 11 50～250g/L, oxammonium sulfate 20～80g/L, yellow soda ash 15～30g/L, complexing agent 10～20g/L, additive 1～20g/L, all the other are water.
2. the phosphatization liquid that a kind of ability cathode electrophoresis according to claim 1 is used is characterized in that zinc salt is one or both sums in zinc oxide, the primary zinc phosphate.
3. the phosphatization liquid that a kind of ability cathode electrophoresis according to claim 1 is used is characterized in that manganese salt is one or both sums in manganous carbonate, the phosphate dihydrogen manganese.
4. the phosphatization liquid that a kind of ability cathode electrophoresis according to claim 1 is used is characterized in that complexing agent is one or both sums in citric acid, the tartrate.
5. the phosphatization liquid that a kind of ability cathode electrophoresis according to claim 1 is used is characterized in that additive is one or both sums in sodium wolframate, the Sodium orthomolybdate.
6. a kind of ability cathode electrophoresis according to claim 1 is characterized in that: get zinc salt, the manganese salt of specified amount, add the phosphoric acid of entry and specified amount, be stirred well to dissolving with the compound method of phosphatization liquid; The complexing agent, yellow soda ash, oxammonium sulfate, the additive that add specified amount respectively fully add water to prescribed volume after the dissolving.
7. a kind of ability cathode electrophoresis according to claim 1 phosphatization liquid using method, it is characterized in that: add water by the concentration of phosphatization liquid hold-up 100ml/L and be mixed with the phosphatization working fluid, measure and adjust phosphatization working fluid free acidity 0.8～1.5, total acidity 20～30 points.Be heated to specified temperature and can carry out bonderizing.
8. a kind of ability cathode electrophoresis according to claim 1 is characterized in that: 25～45 ℃ of phosphatization temperatures, phosphating time 2～6 minutes with phosphatization liquid phosphating process parameter.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103114282A (en) * | 2013-02-27 | 2013-05-22 | 湖南中骏科技有限公司 | Washing-free normal-temperature phosphating solution after steel workpiece phosphating and preparation method thereof |
| CN103668145A (en) * | 2012-09-03 | 2014-03-26 | 洛阳艾笛曼机械设备有限公司 | Phosphorization and phosphorization deslagging integrated device and process |
| CN104451635A (en) * | 2014-11-05 | 2015-03-25 | 泰伦特生物工程股份有限公司 | Special surface treating agent for neodymium iron boron and application method of special surface treating agent |
| CN105220204A (en) * | 2015-09-28 | 2016-01-06 | 合肥常菱汽车零部件有限公司 | A kind of automobile cathode electrophoresis coating process |
| CN107604417A (en) * | 2017-10-21 | 2018-01-19 | 北京雁阳汽车配件有限责任公司 | A kind of electrophoresis phosphating solution and preparation method thereof |
| CN111349920A (en) * | 2020-03-16 | 2020-06-30 | 辽宁工程技术大学 | Environment-friendly phosphating solution containing rare earth composite accelerator and using method |
| CN112410772A (en) * | 2020-11-04 | 2021-02-26 | 安徽瑞荣汽车零部件有限公司 | Polishing and phosphating treatment method for steel backing |
| CN113088953A (en) * | 2019-12-23 | 2021-07-09 | 绵阳海立电器有限公司 | Surface treatment method for compressor |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103668145A (en) * | 2012-09-03 | 2014-03-26 | 洛阳艾笛曼机械设备有限公司 | Phosphorization and phosphorization deslagging integrated device and process |
| CN103114282A (en) * | 2013-02-27 | 2013-05-22 | 湖南中骏科技有限公司 | Washing-free normal-temperature phosphating solution after steel workpiece phosphating and preparation method thereof |
| CN103114282B (en) * | 2013-02-27 | 2015-04-29 | 湖南中骏科技有限公司 | Washing-free normal-temperature phosphating solution after steel workpiece phosphating and preparation method thereof |
| CN104451635A (en) * | 2014-11-05 | 2015-03-25 | 泰伦特生物工程股份有限公司 | Special surface treating agent for neodymium iron boron and application method of special surface treating agent |
| CN104451635B (en) * | 2014-11-05 | 2017-06-16 | 泰伦特生物工程股份有限公司 | A kind of neodymium iron boron special surface treating agent and its application method |
| CN105220204A (en) * | 2015-09-28 | 2016-01-06 | 合肥常菱汽车零部件有限公司 | A kind of automobile cathode electrophoresis coating process |
| CN107604417A (en) * | 2017-10-21 | 2018-01-19 | 北京雁阳汽车配件有限责任公司 | A kind of electrophoresis phosphating solution and preparation method thereof |
| CN107604417B (en) * | 2017-10-21 | 2019-08-16 | 北京雁阳汽车配件有限责任公司 | A kind of electrophoresis phosphating solution and preparation method thereof |
| CN113088953A (en) * | 2019-12-23 | 2021-07-09 | 绵阳海立电器有限公司 | Surface treatment method for compressor |
| CN111349920A (en) * | 2020-03-16 | 2020-06-30 | 辽宁工程技术大学 | Environment-friendly phosphating solution containing rare earth composite accelerator and using method |
| CN111349920B (en) * | 2020-03-16 | 2022-05-03 | 辽宁工程技术大学 | Environment-friendly phosphating solution containing rare earth composite accelerator and using method |
| CN112410772A (en) * | 2020-11-04 | 2021-02-26 | 安徽瑞荣汽车零部件有限公司 | Polishing and phosphating treatment method for steel backing |
| CN112410772B (en) * | 2020-11-04 | 2023-01-20 | 安徽瑞荣汽车零部件有限公司 | Polishing and phosphating treatment method for steel backing |
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Application publication date: 20110622 |