CN101701336B - Environment-friendly metal surface treating agent and using method thereof - Google Patents
Environment-friendly metal surface treating agent and using method thereof Download PDFInfo
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- CN101701336B CN101701336B CN2009101856314A CN200910185631A CN101701336B CN 101701336 B CN101701336 B CN 101701336B CN 2009101856314 A CN2009101856314 A CN 2009101856314A CN 200910185631 A CN200910185631 A CN 200910185631A CN 101701336 B CN101701336 B CN 101701336B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
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Abstract
The invention discloses an environment-friendly metal surface treating agent and a using method thereof. The treating agent comprises fluoride, zircon salt, silane, silicon dioxide, accelerating agent, dispersing agent and stabilizing agent. A conversion coating having the advantages of being compact and even, strong in corrosion resistance and excellent in adhesive force of the coating is respectively formed on the metal surface of steel and zinc; a treatment method of the metal surface treating agent is simple and is operated at the normal temperature; the original phosphating treatment equipment can be used without any change; and strong acid and strong base are not used as the treating agent; therefore, the environment-friendly metal surface treating agent is safe in production without emission, and is the best substitute product of the phosphating treatment technique and an energy-saving type environment-friendly product.
Description
Technical field
The invention belongs to metal conditioner and using method thereof, more specifically is a kind of metal conditioner and using method thereof of without phosphorus Chrome-free.
Background technology
Phosphatization is as Coating Pretreatment, and the history in existing more than 100 year was authorized the English Patent of Ross in 1869, be in the world first about the patent of phosphatization.China begins to introduce the application phosphorization technology in the eighties in last century, and along with China's household electrical appliances, rapid development of automobile industry, phosphatization liquid uses in a large number in China, and phosphatization liquid manufacturer is also innumerable; Chromium passivating also because of self-repair function is arranged, shows very strong solidity to corrosion, is used widely in the surface treatment industry.But phosphatization and chromium passivating also bring serious environmental to pollute, and contain a large amount of inorganic phosphorus in the phosphatization liquid, along with the discharging of waste water, cause that the eutrophication of river pool pollutes, even have caused threat for the drinking water safety of China urban and rural residents in the use; The heavy metal that also contains harm humans health such as zinc, manganese, nickel in the phosphatization liquid, can produce a large amount of waste residues in the parkerizing process also can serious environment pollution, even the use Waste Water Treatment not only can increase the running cost of enterprise, can not eliminate influence fully to environment; The sexavalent chrome of chromium passivating product has extremely strong toxicity, and all use in the strictness restriction countries in the world.In the face of the situation that China's environmental pollution is on the rise, reach China to the promise that the world reduces discharging, press for the energy-conserving and environment-protective product and the technology that work out alternative phosphatization, chromium passivating.
Summary of the invention:
The object of the present invention is to provide the without phosphorus chromium-free metal surface treatment agent of a kind of energy-saving and environmental protection type, can be quickly form the conversion film of one deck densification in the metallic surface, this conversion film has extremely strong solidity to corrosion and various coating bonding force good.
Technical scheme of the present invention:
1) fluoride ion source 0.001-10%
2) zirconium ion and/or titanium ion compound 0.001-10%
3) silane coupling agent 0.01-20%
4) silicon-dioxide 0.001-10%
5) all the other are tap water.
Percentage concentration of the present invention is weight percent concentration.
The fluorion constituent is not particularly limited, and is in Sodium Fluoride, Sodium tetrafluoroborate, Sodium Silicofluoride, fluorine zirconic acid, ammonium fluozirconate, hydrofluotitanic acid, ammonium titanium fluoride, the potassium fluotitanate one or more; The consumption of fluoride ion constituent is 0.001-10%, is preferably 0.1-5%, is lower than 0.1% and is difficult to film forming, is higher than 5% film forming and becomes inhomogeneous and easily return rust;
The zirconium ion constituent is not particularly limited, can be in zirconium carbonate, carbonic acid gas base zirconium ammonium, fluorine zirconic acid, the ammonium fluozirconate one or more, the consumption of zirconium ion constituent is 0.001-10%, be preferably 0.1-5%, be lower than 0.1% and can not form fine and close zirconium film, be higher than 5% pair of film forming without any benefit, also can increase cost;
Silicon-dioxide is the hydrolysis condensation product of nano silicon, water-dispersible silica or silane, the consumption of silicon-dioxide is 0.001-10%, be preferably 0.05-5%, be lower than 0.05% and can not form the fine and close strong conversion film of solidity to corrosion with zirconium ion effectively, being higher than 5% pair of film forming can the increase effect, also can increase cost, cause the colloidal unstable;
Silane coupling agent is not particularly limited, can be in vinyl methoxy silane, vinyl Ethoxysilane, 3-aminopropyltriethoxywerene werene, 3-glycidoxypropyltrimewasxysilane, 3-glycidoxypropyl triethoxyl silane, the 3-aminopropyl trimethoxysilane one or more, dosage of silane coupling agent is 0.01-20%, be preferably 0.5-10%, be lower than 0.5%, be difficult to form and the good conversion film of coating bonding force in the metallic surface, it is easy to crack to be higher than 10% conversion film that forms, and working fluid becomes unstable.
Be speed up processing, also can add promotor in treatment agent, described promotor is one or more in molybdate, rare earth compound, the cobalt salt, and its consumption is 0.001-0.1%.
For guaranteeing the package stability of this invention treatment agent, also can in treatment agent, add stablizer, described stablizer is a kind of in Repone K, sodium-chlor, polyvinyl alcohol, the glycerol, its consumption is 0.001-0.1%.
Using method of the present invention is:
Step 1: alkaline without phosphorus degreasing;
Step 2: twice washing;
Step 3: surface treatment, processing parameter: pH value 4.0-6.0, total acidity 2-10 point, normal temperature is handled, and treatment time 0.5-10 divides kind, processing mode: soak, spray;
Step 4: washing;
Step 5: oven dry;
Step 6: spraying;
Step 7: solidify.
Zirconium (titanium) salt conversion film technology is to utilize the transition metal composite salt to produce film in base metal surface, this layer film play the solidity to corrosion that improves metal and with the ability of coating adhesion.Particularly the reaction product fluorine zirconic acid of zirconium and fluorine can produce fine and close rete in metallic surfaces such as iron, zinc, aluminium.Consanguinity titanium salt, hafnium salt have same filming function.
The sol-gel film-forming process is to produce organic polymer or metal oxide (also can both have) with suitable precursor compound through hydrolysis, polymerization, form colloid liquid, further gelation takes place in reaction, can form corrosion resistant film in the metallic surface, development along with nano material technology, originally be mainly used in this technology of stupalith modification, now begun to be applied to various material surface process field, so this technology also has the nano ceramics of being called transformation technology.
The silane treatment technology: silane is called as industrial monosodium glutamate, uses very extensive.Silane contains two kinds of different chemical functional groups, and an end can generate covalent linkage with the hydroxyl reaction on inorganic materials (as glass fibre, silicate, metal and oxide compound thereof) surface; The other end can generate covalent linkage with resin, thereby two kinds of very big materials of nature difference are closely combined.The environmental protection of the application of this technology aspect surface treatment, development prospect is very good.But the application of single silane finish aspect the pre-treatment of metallic surface be development also.
Without phosphorus chromium-free metal surface treatment agent provided by the invention is integrated application zirconates treatment technology, silane treatment technology and sol-gel film technique.
Fluorion among the present invention is at first slightly soluble iron and steel, zinc-base surface the time, and zirconium (titanium) ion forms fine and close conversion rete in the dissolved metallic surface under certain acidity condition; Silane coupling agent in the colloid and dispersive nano silicon synergy also forms hybrid organic-inorganic film in the metallic surface and since nanometer two change silicon great specific surface area arranged, in 30 seconds, can form complete conversion film.
After cold-reduced sheet that the present invention handles, hot-rolled sheet, the application of galvanized sheet part, sticking power reaches 0 grade, draws the fork cold drawing of anti-neutral salt spray test the 500 hours, galvanized sheet was peeled off and is no more than 1mm in 1000 hours.
The present invention compared with prior art, form at steel, zinc metallic surface that one deck is fine and close evenly, solidity to corrosion is strong and the fabulous conversion film of coating adhesion, its treatment process is simple, operation at normal temperatures, original bonderizing plant just can use without any change, and treatment agent does not use strong acid and strong base, and production safety does not have discharging, being the best substitute products of phosphorization treatment process, also is a kind of energy-saving environmentfriendly products.
Embodiment
Following examples specify surface treatment agent of the present invention, but scope of the present invention is not limited:
Our bright surface treatment agent preparation method and step are as follows:
What 1, add total amount 2/3rds in reactor goes dried uply, and the compound that adds fluoride ion, zirconium ion and/or titanium ion more fully stirs until being dissolved into limpid solution fully.
2, in above-mentioned limpid solution, add silane coupling agent, dispersion agent and fully stir 2 hours to limpid;
3, in aforesaid liquid, add nano silicon and be stirred well to limpid colloid, add the deionized water of stablizer, promotor and residual content, fully stir into limpid colloid and get final product.
Embodiment 1:
Sodium Fluoride 2%
Carbonic acid gas base zirconium ammonium 5%
Vinyl Ethoxysilane 8%
Nano silicon 4%
Polyvinyl alcohol 0.3%
Sodium-chlor 0.3%
All the other are tap water
The workpiece of handling produces cold-reduced sheet for the horse steel, and its operation is:
Step 1: alkaline without phosphorus degreasing;
Step 2: twice washing;
Step 3: surface treatment, processing parameter: pH value 5.5, total acidity 5 points, normal temperature is handled, 5 minutes treatment times, processing mode: soak;
Step 4: washing;
Step 5: oven dry;
Step 6: spraying;
Step 7: solidify.
The surface treatment result is: 0 grade of hundred lattice method sticking power, draw monolateral the peeling off of fork neutral salt spray test 240h less than 0.5mm.
Embodiment 2
Fluorine zirconic acid (fluorion and zirconium ion are provided simultaneously) 10%
3-glycidoxypropyl triethoxyl silane 10%
Dispersed nano silicon 2%
Ammonium titanium fluoride 0.5%
All the other tap water
The workpiece of handling is a Baosteel heat production galvanized sheet, and its operation is:
Step 1: alkaline without phosphorus degreasing;
Step 2: twice washing;
Step 3: surface treatment, processing parameter: pH value 4.5, total acidity 5 points, normal temperature is handled, the treatment time: 1.5 minutes, processing mode: spray;
Step 4: washing;
Step 5: oven dry;
Step 6: spraying;
Step 7: solidify.
The surface treatment result is: 0 grade of hundred lattice method sticking power, draw monolateral the peeling off of fork neutral salt spray test 500h less than 0.5mm.
Embodiment 3:
Fluorine zirconic acid (fluorion and zirconium ion are provided simultaneously) 8%
Titanium tetrachloride 0.5%
3-aminopropyl triethoxysilane 10%
Dispersed silicon-dioxide 3%
Sodium orthomolybdate 0.05%
All the other tap water
The workpiece of handling is a Baosteel heat production galvanized sheet, and its operation is:
Step 1: alkaline without phosphorus degreasing;
Step 2: twice washing;
Step 3: surface treatment, processing parameter: pH value 4.5, total acidity 4 points, normal temperature is handled, the treatment time: 2 minutes, processing mode: spray;
Step 4: washing;
Step 5: oven dry;
Step 6: spraying;
Step 7: solidify.
The surface treatment result is: 0 grade of hundred lattice method sticking power, draw monolateral the peeling off of fork neutral salt spray test 1000h less than 1mm.
Claims (8)
1. the metal conditioner of an environmental protection is characterized in that: the material that contains following weight percent concentration:
1) fluoride ion source 0.1-10%
2) zirconium ion and/or titanium ion compound 0.1-10%
3) silane coupling agent 0.5-20%
4) silicon-dioxide 0.1-10%
5) all the other are tap water.
2. the metal conditioner of a kind of environmental protection according to claim 1, it is characterized in that: described fluorion constituent is one or more in Sodium Fluoride, Sodium tetrafluoroborate, Sodium Silicofluoride, fluorine zirconic acid, ammonium fluozirconate, hydrofluotitanic acid, ammonium titanium fluoride, the potassium fluotitanate, and its concentration is 0.1-5%.
3. the metal conditioner of a kind of environmental protection according to claim 1, it is characterized in that: described zirconium ion constituent is one or more in zirconium carbonate, carbonic acid gas base zirconium ammonium, fluorine zirconic acid, the ammonium fluozirconate, and its concentration is 0.1-5%.
4. the metal conditioner of a kind of environmental protection according to claim 1, it is characterized in that: described silicon-dioxide is the hydrolysis condensation product of nano silicon, water-dispersible silica or silane, its concentration is 0.1-5%.
5. the metal conditioner of a kind of environmental protection according to claim 1, it is characterized in that: described silane coupling agent is one or more in vinyl methoxy silane, vinyl Ethoxysilane, 3-aminopropyltriethoxywerene werene, 3-glycidoxypropyltrimewasxysilane, 3-glycidoxypropyl triethoxyl silane, the 3-aminopropyl trimethoxysilane, and its concentration is 0.5-10%.
6. the metal conditioner of a kind of environmental protection according to claim 1, it is characterized in that: in treatment agent, add promotor, described promotor is one or more in molybdate, rare earth compound, the cobalt salt, and its consumption is 0.001-0.1%.
7. the metal conditioner of a kind of environmental protection according to claim 1, it is characterized in that: add stablizer in treatment agent, described stablizer is a kind of in Repone K, sodium-chlor, polyvinyl alcohol, the glycerol, and its consumption is 0.001-0.1%.
8. the using method of the metal conditioner of the described a kind of environmental protection of claim 1 may further comprise the steps:
Step 1: alkaline without phosphorus degreasing;
Step 2: twice washing;
Step 3: surface treatment: processing parameter: pH value 4.0-6.0, total acidity 2-10 point, normal temperature is handled, and treatment time 0.5-10 minute, processing mode: soak, spray;
Step 4: washing;
Step 5: oven dry;
Step 6: spraying;
Step 7: solidify.
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| CN2009101856314A CN101701336B (en) | 2009-11-26 | 2009-11-26 | Environment-friendly metal surface treating agent and using method thereof |
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| CN2009101856314A CN101701336B (en) | 2009-11-26 | 2009-11-26 | Environment-friendly metal surface treating agent and using method thereof |
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| CN101701336B true CN101701336B (en) | 2011-04-13 |
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-
2009
- 2009-11-26 CN CN2009101856314A patent/CN101701336B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10125424B2 (en) | 2012-08-29 | 2018-11-13 | Ppg Industries Ohio, Inc. | Zirconium pretreatment compositions containing molybdenum, associated methods for treating metal substrates, and related coated metal substrates |
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