CN106637174A - Silane self-assembly treating agent for metal coating pretreatment and application of silane self-assembly treating agent - Google Patents
Silane self-assembly treating agent for metal coating pretreatment and application of silane self-assembly treating agent Download PDFInfo
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- CN106637174A CN106637174A CN201610864027.4A CN201610864027A CN106637174A CN 106637174 A CN106637174 A CN 106637174A CN 201610864027 A CN201610864027 A CN 201610864027A CN 106637174 A CN106637174 A CN 106637174A
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- Prior art keywords
- silane
- acid
- silane self
- self assembly
- inorganic agent
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Classifications
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
-
- 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
Abstract
The invention discloses a silane self-assembly treating agent for metal coating pretreatment and application of the silane self-assembly treating agent. The components of the silane self-assembly treating agent are silane, an organic acid catalyst, alcohol, a water-soluble polymer stabilizer, a chelating agent, auxiliaries and the balance water. The silane self-assembly treating agent is a non-phosphorus and non-chromium metal coating pretreatment agent without heavy metal ions. A self-assembly film of a special structure can be formed on the metal surface by adopting the silane self-assembly treating agent. The silane self-assembly film is compact in structure and can play a very good role in anticorrosion for the metal surface, the adhesive force and the corrosion resistance of a coating can be improved after washing-free coating, and a novel metal surface protection method is achieved.
Description
Technical field
The present invention relates to a kind of metal surface treatment technology, more particularly to a kind of silane for coated metal pre-treatment
Self assembly inorganic agent and its application.
Technical background
Metal erosion is the Tough questions that the world today faces.In metal pretreatment processes, most commonly phosphorus
Change and surface passivation.Because phosphatization and surface passivation pollute more serious, therefore the friendly replacement phosphatization of research environment and surface are blunt
The metal pretreatment processes of change become current problem urgently to be resolved hurrily.Self assembly (self-assembly) technology is in recent years one
Emerging pre-treating technology, during self assembly, basic structural unit under the interaction based on non-covalent bond from
The tissue sent out is collected as a stable, structure with certain regular geometric outward appearance.Protection of the self-assembled film to metallic matrix
Effect is an importance of self-assembled film application.Organic active molecule metal surface spontaneously form densification, in order and
With hydrophobic self-assembled film, the corrosive medium in solution is effectively prevented to migrate to metal surface and spread.Simultaneously as
Self-assembling technique has the advantages that film layer simple to operate, that homogeneous covering can be formed in the substrate surface of arbitrary shape, becomes most
The potential method for replacing phosphatization and chromaking, has broad application prospects in corrosion of metal protection field.
In the self-assembling technique of the active metals such as iron and steel, aluminium and copper, silane self-assembling technique is one and relatively studies more
Film technique, but research work more adopt electrochemical deposition (need to be by certain instrument and equipment), or in a large number use second
Alcohol, isopropanol, three benzene kind solvent non-environmental protection systems, in addition self assembly film formation time length (more in 4-24h), is unfavorable for that industrialization should
With；Or using the high silicon fluoride of the cost of raw material, though super hydrophobic surface (contact angle is larger) can be obtained, to metal works
Follow-up application it is unfavorable, although also have using short carbon chain silane coupler can metal surface obtain self-assembled film,
Film layer is too thin, and the barrier effect corroded Korrosionsmedium is limited, and does not possess self-healing ability, limits its use range.
CN02113026.4 proposes a kind of composite self-assembling method of organic superthin corrosion inhibiting film, in the organic promotion of platinum
In the presence of agent, in clean metallic surfaces self assembly polysiloxane film (2-3h), small molecule sulfhydrylation is then inserted at 70-80 DEG C
Compound (12-24h), obtains the good composite self-assembly thin film of ultra-thin Corrosion Protection, but operation has high demands, and it is permanent to take,
Condition is harsh, is unfavorable for popularization and application.
CN201210257884.X proposes a kind of preparation method of pure titanium metal surface self-organization silanization, and the method is adopted
Silane coupler configures (volume ratio 1 with toluene:49～9), due to using the toluene being harmful to health in a large number as solvent, also not
Promote beneficial to production application.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of silane for coated metal pre-treatment is certainly
Assembling inorganic agent and its application, the silane self assembly inorganic agent can form self-assembled film in metal surface, with following
Advantage：(1) need not be washed；(2) aqueous, environmental protective；(3) film forming efficiency is high, process time short (0.5-10min)；(4) operate
Simple and fast, metal structure workpiece strong adaptability is wide to the range of choice of base shape；(5) silane obtained in metal surface
Self-assembled film is fine and close, and naked film corrosion resisting property is excellent, and can improve the adhesive force and corrosion resistant of metallic matrix and various organic coatings
Corrosion energy, and all other physical and chemical indexs.
The technology of the present invention side is specific as follows：
A kind of silane self assembly inorganic agent and its application for coated metal pre-treatment, the quality of constitutive material each component
Relative content is：
Preferably, the preparation method of the inorganic agent is：The pH value of water is adjusted to 1-6, then add with organic acid in advance
Enter water-soluble polymer stabilizer, after dissolving or being well mixed, the mixture of silane and alcohol is slowly added in water, and constantly
Stirring, after solution clarification chelating agent and auxiliary agent are added into again, and are stirred, and finally supply excess water.
Preferably, described silane is selected from one or more in following structural formula：
R-(CH2)x-Si-(OR’)n, wherein x=3～20, n=1,2,3；
- R is the one kind in hydrogen, alkyl, amino, epoxy radicals, urea groups, isocyanate group, alkene acyloxy, vinyl；
- OR' is methoxyl group, ethyoxyl or acyloxy.
Preferably, described organic acid is silane hydrolyzate accelerator, is selected from：Formic acid, acetic acid, ethanedioic acid, citric acid, grass
One or more in acid, tartaric acid, glycolic, acrylic acid, sulfonic acid, benzene sulfonic acid.
Preferably, described alcohol is selected from：Methyl alcohol, ethanol, one or more in isopropanol, described auxiliary agent is selected from：Sulphur
One or more in urea, hydroxylamine hydrochloride, nitroguanidine.
Preferably, described water-soluble polymer stabilizer is selected from：Polyvinyl alcohol, polyethylene glycol, polypropylene glycol, hydroxyl is fine
One or more in dimension element and its sodium salt.
Preferably, described polyvinyl alcohol is one or more in 75%～90% polyvinyl alcohol selected from alcoholysis degree；
The molecular weight of polyethylene glycol is one or more in 200-10000；The molecular weight of polypropylene glycol is the one kind in 200-8000
Or it is various；Hydroxylated cellulose is the one kind or many in sodium carboxymethylcellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose
Kind.
Preferably, described chelating agent is selected from：EDTA (ethylenediamine tetra-acetic acid), NTA (nitrilotriacetic acid), DTPA (diethyls
Alkene pentaacetic acid), PDTA (trimethylen-edinitrilo-tetraacetic acid), HEDTA (hydroxyethylethylene diamine tri-acetic acid), AEEA (ethoxy second two
Amine), one or more in TEDA (Gu amine, triethylene diamine) and its salt.
The invention also discloses application of the described silane self assembly inorganic agent in protecting metallic surface.
The application is preferably：Silane self assembly inorganic agent is sprayed or impregnating metal base material 0.5-10min；Naturally it is cloudy
Dry, relative air humidity is not higher than 80%；Or heated-air drying, 80-120 DEG C of baking temperature, i.e., formed certainly in metallic substrate surface
Component film, the membrane structure is fine and close, and good corrosion-resisting function can be played to metal surface.
Metal works to being disposed carry out organic coating application, can improve every physicochemical property of organic coating.
Compared with excellent technology is selected, the application of the present invention has following advantage：(1) need not be washed again；(2) it is aqueous
Environmental protection；(3) process time flexibly (0.5-10min), can simultaneously be applied to spray and impregnation technology；(4) it is simple and quick, gold
Category form workpiece strong adaptability, it is wide to the range of choice of base shape；(5) the silane self-assembled film obtained in metal surface is caused
Close, naked film corrosion resisting property is excellent, and can improve the adhesive force and decay resistance of metallic matrix and various organic coatings, Yi Jiqi
Its every physical and chemical index.
Specific embodiment
Embodiment 1：
A) in terms of 100 parts of weight, 40 parts of water are added toward in stirred tank, 1.5 parts of formic acid of addition adjust its pH value for 3；Then
It is added into 20 parts of hydroxyethyl celluloses；By 30 parts of propyl trimethoxy silicanes and butyl trimethoxy silane (mixed proportion 1：1)
It is slowly added in above-mentioned water after being well mixed with 5 parts of ethanol, and is stirred continuously until solution clarification；It is added into 0.5 part of EDTA
With 1.5 parts of hydroxylamine hydrochlorides, the water of surplus is finally supplied.
B) by step A) obtained in silane self assembly inorganic agent steel structural part is processed, using spray process, place
The reason time is 2.5min；Need not be washed after process；Heated-air drying, 120 DEG C of baking temperature are carried out before application.
C) steel structural part to being disposed carries out organic coating application, can improve the adhesive force of organic coating, reaches
To 0 grade；By the falling weight impact test of 1kg80cm, paint film is without ftractureing or the bad phenomenon that comes off；By neutral salt spray test
500h, monolateral corrosion diffusion is less than 2mm, meets the painting technical standard of iron and steel parts.
Embodiment 2：
A) in terms of 100 parts of weight, 30 parts of water are added toward in stirred tank, 2 parts of sulfonic acid of addition adjust its pH value for 1；Then add
Add 10 parts of polyethylene glycol (PEG400)；By 20 parts of 3- (oxygen of 2,3- epoxies third) propyl-triethoxysilicanes and 2.5 parts of methyl alcohol second
Alcohol (mixed proportion 95：5) during above-mentioned water is slowly added after being well mixed, and it is stirred continuously until solution clarification；It is added into 0.3
EDTA2Na and 2 part of thiocarbamide of part, finally supplies the water of surplus.
B) by step A) obtained in silane self assembly inorganic agent plated steel sheet is processed, using spray process, place
The reason time is 0.5min；Need not be washed after process；Dry in the shade naturally before application, relative air humidity 80%；
C) plated steel sheet to being disposed carries out organic coating application, can improve the adhesive force of organic coating, reach
To 0 grade；By the falling weight impact test of 1kg50cm, paint film is without ftractureing or the bad phenomenon that comes off；And neutral salt spray test
500h, monolateral corrosion diffusion is less than 1.5mm, meets the painting technical standard of galvanized part..
Embodiment 3：
A) in terms of 100 parts of weight, 35 parts of water are added toward in stirred tank, 0.1 part of citric acid of addition adjusts its pH value for 6；So
After be added into 5 parts of polypropylene glycols (PPG1000)；15 parts of vinyltriacetoxy silanes and 1.5 parts of isopropanols are well mixed
After be slowly added in above-mentioned water, and be stirred continuously until solution clarification；0.1 part of HEDTA and 0.5 part of hydroxylamine hydrochloride is added into,
Finally supply the water of surplus.
B) by step A) obtained in silane self assembly inorganic agent aluminium section bar is processed, using impregnation process, during process
Between be 8min；Need not be washed after process；Heated-air drying, 80 DEG C of baking temperature are carried out before application.
C) aluminium section bar to being disposed carries out organic coating application, can improve the adhesive force of organic coating, reaches 0
Level；By neutral salt spray test 1000h, monolateral corrosion diffusion is less than 1mm, by resistance to copper acetate accelerated test 120h, monolateral corruption
Erosion diffusion is less than 1mm, meets the painting technical standard of aluminium section bar.
Embodiment 4：
A) in terms of 100 parts of weight, 35 parts of water are added toward in stirred tank, 0.5 part of acetic acid of addition adjusts its pH value for 4；Then
It is added into 1 part of polyvinyl alcohol (alcoholysis degree 78%)；5 parts of isocyanatopropyl triethoxysilanes and 0.5 part of isopropanol mixing are equal
During above-mentioned water is slowly added after even, and it is stirred continuously until solution clarification；It is added into the mixed of 0.2 part of DTPA and DTPA5Na
Compound (mixed proportion 1：1) with 0.1 part of nitroguanidine, the water of surplus is finally supplied.
B) by step A) obtained in silane self assembly inorganic agent cold-rolled strip is processed, using impregnation process, process
Time is 10min；Need not be washed after process；Heated-air drying, 105 DEG C of baking temperature are carried out before application.
C) cold-rolled strip to being disposed carries out organic coating coating, can improve the adhesive force of organic coating, reaches 0
Level；By neutral salt spray test 360h, monolateral corrosion diffusion is less than 2mm；By the boiling test of 80 DEG C × 48h, film is without drum
Bubble or the bad phenomenon that comes off, meet the painting technical standard of cold-rolled strip.
Claims (10)
1. a kind of silane self assembly inorganic agent for coated metal pre-treatment, it is characterised in that：The matter of constitutive material each component
Measuring relative content is：
2. silane self assembly inorganic agent as claimed in claim 1, it is characterised in that the preparation method of the inorganic agent is：In advance
The pH value of water is adjusted to 1-6, water-soluble polymer stabilizer is then added into, after dissolving or being well mixed, by silicon with organic acid
The mixture of alkane and alcohol is slowly added in water, and is stirred continuously, and after solution clarification chelating agent and auxiliary agent are added into again, and is stirred
Mix uniform, finally supply excess water.
3. silane self assembly inorganic agent as claimed in claim 1, it is characterised in that described silane is in following structural formula
One or more：
R-(CH2)x-Si-(OR’)n, wherein x=3～20, n=1,2,3；
- R is the one kind in hydrogen, alkyl, amino, epoxy radicals, urea groups, isocyanate group, alkene acyloxy, vinyl；
- OR' is methoxyl group, ethyoxyl or acyloxy.
4. silane self assembly inorganic agent as claimed in claim 1 or 2, it is characterised in that described organic acid is that silane hydrolyzate promotees
Enter agent, be selected from：In formic acid, acetic acid, ethanedioic acid, citric acid, oxalic acid, tartaric acid, glycolic, acrylic acid, sulfonic acid, benzene sulfonic acid one
Plant or various.
5. silane self assembly inorganic agent as claimed in claim 1 or 2, it is characterised in that described alcohol is selected from：Methyl alcohol, ethanol,
One or more in isopropanol, described auxiliary agent is selected from：One or more in thiocarbamide, hydroxylamine hydrochloride, nitroguanidine.
6. silane self assembly inorganic agent as claimed in claim 1 or 2, it is characterised in that described water-soluble polymer stabilizer
It is selected from：One or more in polyvinyl alcohol, polyethylene glycol, polypropylene glycol, hydroxylated cellulose and its sodium salt.
7. silane self assembly inorganic agent as claimed in claim 6, it is characterised in that described polyvinyl alcohol is selected from alcoholysis degree
One or more in 75%～90% polyvinyl alcohol；The molecular weight of polyethylene glycol is one or more in 200-10000；
The molecular weight of polypropylene glycol is one or more in 200-8000；Hydroxylated cellulose is sodium carboxymethylcellulose, ethoxy fibre
One or more in dimension element, hydroxypropyl methyl cellulose.
8. silane self assembly inorganic agent as claimed in claim 1 or 2, it is characterised in that described chelating agent is selected from：Ethylenediamine
Tetraacethyl, nitrilotriacetic acid, diethylene triamine pentacetic acid (DTPA), trimethylen-edinitrilo-tetraacetic acid, hydroxyethylethylene diamine tri-acetic acid, ethoxy second two
One or more in amine, solid amine, triethylene diamine and its salt.
9. application of a kind of silane self assembly inorganic agent as claimed in claim 1 or 2 in protecting metallic surface.
10. application as claimed in claim 9, it is characterised in that with silane self assembly inorganic agent spray or impregnating metal base material
0.5-10min；Naturally dry in the shade, relative air humidity is not higher than 80%；Or heated-air drying, 80-120 DEG C of baking temperature, i.e., in gold
Category substrate surface forms self-assembled film, and the membrane structure is fine and close, and good corrosion-resisting function can be played to metal surface.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610864027.4A CN106637174A (en) | 2016-09-29 | 2016-09-29 | Silane self-assembly treating agent for metal coating pretreatment and application of silane self-assembly treating agent |
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| CN201610864027.4A CN106637174A (en) | 2016-09-29 | 2016-09-29 | Silane self-assembly treating agent for metal coating pretreatment and application of silane self-assembly treating agent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107410545A (en) * | 2017-07-31 | 2017-12-01 | 浦江县元寿农业科技有限公司 | A kind of green tea cleaning equipment of low energy consumption |
| CN107523820A (en) * | 2017-07-04 | 2017-12-29 | 安徽腾龙泵阀制造有限公司 | A kind of inorganic acid passivating solution for electro-galvanized layer |
| CN108441114A (en) * | 2018-03-20 | 2018-08-24 | 粟飞 | A kind of silane antirust agent |
| CN112480814A (en) * | 2020-11-26 | 2021-03-12 | 汪元亮 | Surface treating agent and surface protection method for porous loose material |
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Cited By (5)
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Application publication date: 20170510 |