CN105039950A - Environment-friendly metal surface treatment agent - Google Patents
Environment-friendly metal surface treatment agent Download PDFInfo
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- CN105039950A CN105039950A CN201510475486.9A CN201510475486A CN105039950A CN 105039950 A CN105039950 A CN 105039950A CN 201510475486 A CN201510475486 A CN 201510475486A CN 105039950 A CN105039950 A CN 105039950A
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- treatment agent
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Abstract
Provided is an environment-friendly metal surface treatment agent. The metal surface treatment agent can form an even and compact chemical conversion coating with superior corrosion resistance and coating adaptation on the surface of metal. The metal surface treatment agent is used for iron, aluminum and zinc type metal materials and comprises (A) hexafluorozirconic acid or fluorozirconate thereof; (B) hexafluorotitanic acid or fluotitanate thereof; (C) 1,2-Bis(trimethoxysilyl)ethane or Bis(triethoxysilyl)ethane hydrolysis products; (D) molybdate; and (E) one or more of nitrate of beryllium, nitrate of magnesium, nitrate of calcium, nitrate of strontium, nitrate of aluminum, nitrate of vanadium, nitrate of manganese, nitrate of copper and nitrate of zinc.
Description
Technical field
The present invention relates to and a kind ofly can form the environmental protective metal treatment agent and treatment process thereof that erosion resistance is strong, coating adhesion is good in metallic surface.
Background technology
Usually when implementing application to metal (metallic substance, metallic structures), from the viewpoint of the close attachment guaranteeing solidity to corrosion and film, can implement to metallic surface the surface treatment chemically forming chemical conversion epithelium.
Traditional treatment method carries out Passivation Treatment with chromic salt, or carry out bonderizing with Phosphating Solution.Chromic salt is the extremely strong carcinogenic substance of toxicity, and extremely difficult disaggregating treatment, uses links all to produce strong and fatal Health hazard to environment and human body at production, discharge of wastewater, Solid state fermentation, product.There is the problem that phosphorus pollutes in Phosphating Solution, also usually there is the problem of the heavy metal contaminations such as such as nickel.Along with the lasting raising of various countries' environmental protection standard, continue to use the production technique containing chromium or phosphatization to be subject to strict supervision, the cost of sewage disposal is also very expensive.
The more inorganic salt of current research are as molybdate, silicate, rare-earth salts, zirconium titanium salt etc., and organic is as silane, silicon sol, phytic acid, Weibull etc.Although wherein a lot of technology under certain conditions can substitute chromium passivation or bonderizing, but there is the problems such as such as solidity to corrosion is poor, treatment time length, poor stability, high cost.In all achievements in research, zirconium titanium salt technology, silane technology, with good treatment effect and over-all properties, have more application in actual production process.
But at some, prior art requires that higher field still exists the problems such as solidity to corrosion, application sticking power is not enough.Some technology is used by the interworking of zirconium titanium salt and silane, can effectively promote application sticking power, but solidity to corrosion still has deficiency, does not particularly do the field of application at some, cannot meet needs of production.
Summary of the invention
Object of the present invention, is to provide a kind of rotproofness and the good environmental protective metal treatment agent of application adaptation.
The technical scheme adopted is:
A kind of environmental protective metal treatment agent is solvent with deionized water, Yu Shuizhong contains (A) fluorine zirconic acid or its salt; (B) hydrofluotitanic acid or its salt; (C) hydrolysate of 1,2-two silica-based ethane of trimethoxy or 1,2-bis-(triethoxy is silica-based) ethane; (D) molybdate; (E) at least a kind in the nitrate of beryllium, magnesium, calcium, strontium, aluminium, vanadium, manganese, copper, zinc.
The preparation method of described high anti-corrosion environmental protective metal treatment agent, first silane hydrolysates (C) is prepared, again (A), (B), (C), (D), (E) are added in deionized water successively, mixing and stirring.
Film forming treatment process steps of the present invention is:
The first step: degreasing
Second step: washing
3rd step: chemical conversion
4th step: washing
5th step: dry
Wherein, the first step degreasing adopts commercial metals grease-removing agent, is cleaned up by metal surface greasy dirt.Second step washing adopts deionization washing 0.5-1 minute, is cleaned by the residual grease-removing agent of former process.3rd step chemical conversion, metal to be processed is fully contacted with the metal conditioner described in this patent, treatment agent contact operation is not particularly limited, the method such as pickling process, spraying process can be adopted, temperature processes within the scope of 10-50 DEG C, treatment time is 5-300 second, preferred 15-180 second.4th step washing adopts deionization washing 0.5-1 minute.5th step drying process can adopt the modes such as seasoning, cold air drying, warm air drying, oven dry.
Metal after above-mentioned art breading, directly can obtain the good rete of solidity to corrosion, also can carry out application with known coating further, comprise organic coatings volatile organic compounds, water-borne coatings, powder coating etc.
Advantage of the present invention is:
1, the present invention is not completely containing heavy metal elements such as chromium, not phosphate-containing composition, free from extraneous odour, safety and environmental protection;
2, metal conditioner of the present invention can form even, fine and close rete in metallic surface, has excellent erosion resistance and the advantage of application adaptation.
First the test of chemical membrane solidity to corrosion is carried out.
Embodiment
Embodiment one
Prepare the cold-reduced sheet sample block that the trade mark is Q225, size is 150mm × 80mm × 1mm.
The first step skimming treatment, adopts Henkel KGaA RT-1022 grease-removing agent, carries out skimming treatment in 10 minutes at 40 DEG C to described metallic substance.
Second step is washed, and carries out 30 seconds cleaning showers with deionized water to sample block.
3rd step chemical conversion treatment.
25 part 1,2-bis-(triethoxy is silica-based) ethane is slowly added in 75 parts of deionized waters, stirs, 25 DEG C reaction 24 hours for subsequent use.By ammonium fluozirconate, hydrofluotitanic acid, prepare 1,2-bis-(triethoxy is silica-based) ethane hydrolyzate, ammonium molybdate, magnesium nitrate dissolve in deionized water successively, concentration is respectively ammonium fluozirconate 1g/L, hydrofluotitanic acid 1g/L, 1,2-bis-(triethoxy is silica-based) ethane 3g/L, ammonium molybdate 0.5g/L, magnesium nitrate 3g/L, mixing and stirring, by nitric acid, ammoniacal liquor adjust ph to 3.5.
Be impregnated in by sample block in the metal conditioner prepared, Li Wendu controls at 20 DEG C, 90 seconds treatment times.
4th step washing, carries out 30 seconds cleaning showers with deionized water to sample block.
5th step is dry, drying 10 minutes at 100 DEG C.
Embodiment two
25 part 1,2-bis-(triethoxy is silica-based) ethane is slowly added in 75 parts of deionized waters, stirs, 25 DEG C reaction 24 hours for subsequent use.By ammonium fluozirconate, hydrofluotitanic acid, prepare 1,2-bis-(triethoxy is silica-based) ethane hydrolyzate, ammonium molybdate, magnesium nitrate dissolve in deionized water successively, concentration is respectively ammonium fluozirconate 2g/L, hydrofluotitanic acid 2g/L, 1,2-bis-(triethoxy is silica-based) ethane 1g/L, ammonium molybdate 0.5g/L, magnesium nitrate 3g/L, mixing and stirring, by nitric acid, ammoniacal liquor adjust ph to 4.
Be impregnated in by sample block in the metal conditioner prepared, Li Wendu controls at 25 DEG C, 90 seconds treatment times.
Other steps are with embodiment one.
Embodiment three
25 part of 1,2-two silica-based ethane of trimethoxy is slowly added in 75 parts of deionized waters, stirs, for subsequent use 25 DEG C of reactions 24 hours.By ammonium fluozirconate, hydrofluotitanic acid, prepare 1, the two silica-based ethane hydrolyzate of trimethoxy of 2-, ammonium molybdate, magnesium nitrate dissolve in deionized water successively, concentration is respectively ammonium fluozirconate 1.5g/L, the two silica-based ethane 1g/L of trimethoxy of hydrofluotitanic acid 1.5g/L, 1,2-, ammonium molybdate 0.5g/L, magnesium nitrate 2.5g/L, mixing and stirring, by nitric acid, ammoniacal liquor adjust ph to 4.
Be impregnated in by sample block in the metal conditioner prepared, Li Wendu controls at 25 DEG C, 90 seconds treatment times.
Other steps are with embodiment one.
Embodiment four
40 part 1,2-bis-(triethoxy is silica-based) ethane is slowly added in 60 parts of deionized waters, stirs, 25 DEG C reaction 24 hours for subsequent use.By fluorine zirconic acid, titanium sodium fluoride, prepare 1,2-bis-(triethoxy is silica-based) ethane hydrolyzate, ammonium molybdate, magnesium nitrate dissolve in deionized water successively, concentration is respectively fluorine zirconic acid 2g/L, titanium sodium fluoride 1.5g/L, 1,2-bis-(triethoxy is silica-based) ethane 1g/L, ammonium molybdate 0.5g/L, magnesium nitrate 3g/L, mixing and stirring, by nitric acid, ammoniacal liquor adjust ph to 4.
Be impregnated in by sample block in the metal conditioner prepared, Li Wendu controls at 25 DEG C, 90 seconds treatment times.
Other steps are with embodiment one.
Embodiment five
Preparing the trade mark is the aluminium sheet of 5052, and size is 150mm × 80mm × 1mm
Other steps are with embodiment one.
Comparative example 1
Do not add silane, other are consistent with embodiment 1;
Comparative example 2
Change 1,2-bis-(triethoxy is silica-based) ethane into γ-aminopropyl triethoxysilane, other are consistent with embodiment 1;
Comparative example 3
Do not add ammonium fluozirconate, hydrofluotitanic acid, other are consistent with embodiment 1;
Comparative example 4
Do not add ammonium molybdate, other are consistent with embodiment 1;
Comparative example 5
Do not add magnesium nitrate, other are consistent with embodiment 1;
Comparative example 6
Do not add silane, other are consistent with embodiment 5;
Comparative example 7
Change 1,2-bis-(triethoxy is silica-based) ethane into γ-aminopropyl triethoxysilane,
Other are consistent with embodiment 5;
Comparative example 8
Do not add ammonium molybdate, other are consistent with embodiment 5;
The sample block of embodiment 1-5 and comparative example 1-8 is carried out neutral salt spray test, detects metallic surface after 100 hours and return rust area, by the scoring of 0-10 level, 0 grade for not return rust, 10 grades are returned rust for gross area, and N level represents returns N × 10% that the area that becomes rusty accounts for the total area.Test-results is as follows:
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Grading | 0 | 0 | 0 | 0 | 0 |
Carry out sticking power test further.Carry out electrostatic powder coating after drying, coating used is ippon A2000, and the process such as application, solidification meets powder coating technique specification.
Embodiment six
After drying treatment, carry out electrostatic powder coating, other are consistent with embodiment 1;
Embodiment seven
After drying treatment, carry out electrostatic powder coating, other are consistent with embodiment 2;
Embodiment eight
After drying treatment, carry out electrostatic powder coating, other are consistent with embodiment 3;
Embodiment nine
After drying treatment, carry out electrostatic powder coating, other are consistent with embodiment 4;
Embodiment ten
After drying treatment, carry out electrostatic powder coating, other are consistent with embodiment 5;
Comparative example 9
After drying treatment, carry out electrostatic powder coating, other are consistent with comparative example 1;
Comparative example 10
After drying treatment, carry out electrostatic powder coating, other are consistent with comparative example 2;
Comparative example 11
After drying treatment, carry out electrostatic powder coating, other are consistent with comparative example 3;
Comparative example 12
After drying treatment, carry out electrostatic powder coating, other are consistent with comparative example 4;
Comparative example 13
After drying treatment, carry out electrostatic powder coating, other are consistent with comparative example 5;
Comparative example 14
After drying treatment, carry out electrostatic powder coating, other are consistent with comparative example 6;
Comparative example 15
After drying treatment, carry out electrostatic powder coating, other are consistent with comparative example 7;
Comparative example 16
After drying treatment, carry out electrostatic powder coating, other are consistent with comparative example 8;
Adhesion test method: with sharp cutting knife by test board crosscut, to this brassboard neutral salt spray test 360 hours.After spraying terminates, measure the maximum swelling amplitude of both sides, crosscut portion.Expansion amplitude is less, and sticking power is better.
Summary, the present invention significantly can promote metal corrosion-resisting, has good application sticking power simultaneously.
Claims (10)
1. an environmental protective metal treatment agent, is characterized in that: described metal conditioner is solvent with deionized water, Yu Shuizhong contains (A) fluorine zirconic acid or its salt; (B) hydrofluotitanic acid or its salt; (C) hydrolysate of 1,2-two silica-based ethane of trimethoxy or 1,2-bis-(triethoxy is silica-based) ethane; (D) molybdate; (E) at least a kind in the nitrate of beryllium, magnesium, calcium, strontium, aluminium, vanadium, manganese, copper, zinc.
2. a kind of environmental protective metal treatment agent according to claim 1, it is characterized in that described (A) fluorine zirconic acid or its salt comprise at least one in fluorine zirconic acid, sodium fluozirconate, potassium fluozirconate, ammonium fluozirconate, its content is 0.2-8g/L, is preferably 0.5-5g/L.
3. a kind of environmental protective metal treatment agent according to claim 1, it is characterized in that described (B) hydrofluotitanic acid or its salt comprise at least one in hydrofluotitanic acid, titanium sodium fluoride, potassium fluotitanate, ammonium titanium fluoride, its content is 0.2-8g/L, is preferably 0.5-5g/L.
4. a kind of environmental protective metal treatment agent according to claim 1, it is characterized in that described (C) 1, the two silica-based ethane of trimethoxy or 1 of 2-, the hydrolysate of 2-bis-(triethoxy is silica-based) ethane is 1, the two silica-based ethane of trimethoxy or 1 of 2-, product after 2-bis-(triethoxy is silica-based) ethane is hydrolyzed in aqueous, hydrolysis refers to that silane and deionized water mix by a certain percentage, the product after 24 hours is reacted at 25 DEG C, silane contents is 10-90%, be preferably 20-50%, silane in metal conditioner (weighing scale with before being hydrolyzed) content is for 0.1-10g/L, be preferably 0.5-5g/L.
5. a kind of environmental protective metal treatment agent according to claim 1, it is characterized in that described (D) molybdate comprises at least one in Sodium orthomolybdate, potassium molybdate, ammonium molybdate, its content is 0.05-3g/L, is preferably 0.1-1g/L.
6. a kind of environmental protective metal treatment agent according to claim 1, it is characterized in that described metal conditioner contains at least a kind in the nitrate of (E) beryllium, magnesium, calcium, strontium, aluminium, vanadium, manganese, copper, zinc, its content is 0.5-10g/L, is preferably 1-5g/L.
7. a kind of environmental protective metal treatment agent according to claim 1-6, it is characterized in that the pH value of described metal conditioner is more than 1.5, less than 6.5, pH adjusting agent can use in nitric acid, hydrofluoric acid, sodium hydroxide, potassium hydroxide, ammoniacal liquor etc. one or more.
8. a kind of environmental protective metal treatment agent according to claim 1-7, is characterized in that the application of described metal conditioner, it is characterized in that: this metal conditioner is used for metal finishing, and using method comprises the following steps:
1) treatment agent contacts with metallic surface: be contacted with this metal conditioner by metallic substance;
2) wash: be that the metallic substance through described treatment agent contact procedure is washed.
9. a kind of environmental protective metal treatment agent according to claim 1-8, it is characterized in that described metallic substance refers in iron and iron alloy, aluminium and aluminium alloy thereof, zinc and alloy thereof any one; Treatment agent contacts with metallic surface, and temperature processes within the scope of 10-50 DEG C; Treatment time is 5-300 second.
10. a kind of environmental protective metal treatment agent according to claim 1-9, is characterized in that the metallic surface after this metal conditioner process can not spray, also can proceed electrostatic powder coating, sprays paint or electrophoretic painting process.
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| CN201510475486.9A CN105039950A (en) | 2015-08-06 | 2015-08-06 | Environment-friendly metal surface treatment agent |
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Cited By (6)
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| CN105483680A (en) * | 2015-12-04 | 2016-04-13 | 三达奥克化学股份有限公司 | Normal-temperature spraying type comprehensive treatment agent used before bonding of electrolysis plates and PC plates and preparation method |
| CN108998781A (en) * | 2018-07-18 | 2018-12-14 | 湖北大冶汉龙汽车有限公司 | A kind of car body coating front surface zirconium treatment technique |
| CN109097761A (en) * | 2018-10-23 | 2018-12-28 | 南京洁雅新材料有限公司 | Environment-friendly type nano film agent and preparation method thereof |
| CN109402619A (en) * | 2018-12-29 | 2019-03-01 | 帝业化学品（上海）有限公司 | A kind of without phosphorus nitrogen-free coating metal surfaces pre-treatment medicament and its method |
| CN113235078A (en) * | 2021-05-18 | 2021-08-10 | 中山市壹桥环保科技有限公司 | Washing-free silane agent and using method thereof |
| CN116083893A (en) * | 2023-02-09 | 2023-05-09 | 广汽埃安新能源汽车股份有限公司 | Treatment method of metal substrate and material for preparing vehicle |
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| CN109097761A (en) * | 2018-10-23 | 2018-12-28 | 南京洁雅新材料有限公司 | Environment-friendly type nano film agent and preparation method thereof |
| CN109402619A (en) * | 2018-12-29 | 2019-03-01 | 帝业化学品（上海）有限公司 | A kind of without phosphorus nitrogen-free coating metal surfaces pre-treatment medicament and its method |
| CN113235078A (en) * | 2021-05-18 | 2021-08-10 | 中山市壹桥环保科技有限公司 | Washing-free silane agent and using method thereof |
| CN116083893A (en) * | 2023-02-09 | 2023-05-09 | 广汽埃安新能源汽车股份有限公司 | Treatment method of metal substrate and material for preparing vehicle |
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