CN102838913A - Organosilicone modified heat-resistant self-cleaning waterborne electrochemistry corrosion-resistant paint and preparation method thereof - Google Patents
Organosilicone modified heat-resistant self-cleaning waterborne electrochemistry corrosion-resistant paint and preparation method thereof Download PDFInfo
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- CN102838913A CN102838913A CN2012102939049A CN201210293904A CN102838913A CN 102838913 A CN102838913 A CN 102838913A CN 2012102939049 A CN2012102939049 A CN 2012102939049A CN 201210293904 A CN201210293904 A CN 201210293904A CN 102838913 A CN102838913 A CN 102838913A
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Abstract
Provided is organosilicone modified heat-resistant self-cleaning waterborne electrochemistry corrosion-resistant paint. The raw material comprises a resin emulsion. The organosilicone modified heat-resistant self-cleaning waterborne electrochemistry corrosion-resistant paint is characterized in that the resin emulsion is an MPM modified acrylic acid resin microemulsion, the raw material further comprises a coupling agent gamma-methacrylonitrile acyloxy trimethoxy silane, and the adding proportion of the coupling agent gamma-methacrylonitrile acyloxy trimethoxy silane is 0.5-3% of the raw material by mass. The organosilicone modified heat-resistant self-cleaning waterborne electrochemistry corrosion-resistant paint has the advantages that the organosilicone modified heat-resistant self-cleaning waterborne electrochemistry corrosion-resistant paint has perfect waterborne rusted, rust conversion and antirust characteristics; high hiding rate is integrated with high glossiness; weather resistance is high, and for example the products are acid-resisting, alkali-resisting, radiation-resistant and high-low temperature resistant; water repellency and a self-cleaning function are superstrong; the paint film is good in hardness, and the hardness is more than 2H; and organic solvents do not exist, volatile organic compounds (VOC) are low, and environmental protection is benefited.
Description
Technical field
This invention relates to the antifouling paste preparation field.
Technical background
Along with development of human society; Metal to be utilized in people's productive life field ubiquitous; People also go together with development and use to the protection of metal mutually for a long time; But because the metal protection coating that past resin technology and other material technology limitation cause makes metal protection seriously lag behind the utilization to metal because of problems such as comprehensive weathering resistance differences, a large amount of metals has been corroded in noiseless place.
Oxidizing reaction that takes place between metal and water and oxygen and material that chemical corrosivity is arranged make the electronics of metal lose under electrochemical effect like acid, alkali, salt etc., become oxidizing substance or other salt of loose suction, thereby metal is corroded rapidly.According to data, the whole world has 1,000,000,000 tons of metals to be corroded every year approximately, is equivalent to when 20% of YO, and can't recycles, and causes surprising waste and environmental pollution.Thereby to the protection meaning of metal as many as made.Traditional antifouling paste has disadvantage:
1. mostly traditional antifouling paste is solvent borne, and the construction in summer is prone to workman's health is caused damage, and is also unfriendly to environment.
2. traditional antifouling paste is the end, face separately, secondary construction type, and efficiency is low.
3. all there is following problem in emerging in recent years (comprising disclosed water-based patent antifouling paste) water-repellent preservation lacquer according to our scientific research personnel's repeated authentication repeatedly:
1.
hiding rare and glossiness are attended to one thing and lose sight of another.
paint film dependency is not strong, is prone to come off.
non-refractory.
Summary of the invention
The object of the invention is exactly to traditional above-mentioned deficiency of antifouling paste, and a kind of vinyl resin microemulsion that can be used for preparing the modification of high temperature automatically cleaning antifouling paste is provided.
Advantage of the present invention is: characteristics of the present invention are that not only its perfection has broken through the water-repellent preservation lacquer " parcel with bonding " the conventional physical way; Electrochemistry molecule bridging technology and double salt and chelating technology have been introduced; For the first time methylphenyl siloxane is incorporated into the anti-corrosion of metal industry, its finished product have following characteristics:
1, perfect aqueous rusty, commentaries on classics rust, antirust characteristic;
2, the unification of high hiding rare and high-luster;
3, high-weatherability (having acidproof, alkaline-resisting, radiation hardness, high-low temperature resistant);
4, have superpower water repellency and self-cleaning function;
5, hardness of paint film is good, and its hardness surpasses 2H;
6, organic solvent-free, low VOC, environmental.
Embodiment
One, the vinyl resin preparation of microemulsion of MPM modification
(1) preparation method of methacryloxypropyl methoxymethyl phenyl silicone oil (MPM) is: the catalyzing and condensing method, and by HO (MephSiO)
nH and CH2=CMeCOOC3H6SiMe (OMe) 2 hydrolytic condensation and getting under granular sulfonic acid ion exchange resin catalysis.Reaction formula is:
HO(MephSiO)
n H+2CH2＝CMeCOOC3H6SiMe(OMe)2
H +
CH2＝CMeCOOC3H6（MeO）MeSiO(MephSiO)nSiMe(OMe)C3H6OCOCMe＝CH2 ,[MPM]
MPM prepares instance: by the HO (MephSiO) of 4.4mol
nThe CH2=CMeCOOC3H6SiMe (OMe) 2 of H (n about 300) and 9.1mol is at (mean pore size>=40 μ m) catalysis of granular sulfonic acid ion exchange resin and 60 ℃ of following reaction 1h, and the MPM transformation efficiency that promptly gets 4mol reaches as high as 95%.
(2) monomeric preparatory emulsification: get AEO-7 (AEO-7) 0.05-0.5kg, SDS (sodium lauryl sulphate) 0.25-1 kg, AES (polyoxyethylenated alcohol sodium sulfate) 0.25-1kg and PEG-400 (PEG 400) 0.4-0.75kg, MAA (TEB 3K) 1.2-1.4kg, ST (vinylbenzene) 0.5-0.8 kg, AN (vinyl cyanide) 1.0-2.0kg, mix to stir and process newborn pre-emulsion I; Get again among AEO-7 (AEO-7) 0.05-0.5kg, SDS (sodium lauryl sulphate) 0.2.5-1 kg, AES (polyoxyethylenated alcohol sodium sulfate) 0.25-1kg and AEO-3 (AEO-3) 0.1-1kg, PEG-400 (PEG 400) 0.4-0.75kg adding MMA (TEB 3K) 1.2-1.4kg, BA (n-butyl acrylate) 5-12kg, 2-EHA (vinylformic acid one 2 one ethylhexyls) 5-12kg, the MPM1.4-1.8kg; Under agitation slowly add entry 2-4kg, process the pre-emulsion II with the phase inversion dispersion method;
(3) micro-emulsion polymerization: in the four-hole bottle that TM, whisking appliance, prolong are housed, add entry 2-4kg, stir, add the pre-emulsion I of total amount 1/2; With ammoniacal liquor adjust pH to 7, begin to heat up, add initiator A PS (ammonium persulphate) 0.4-0.6kg when being warming up to 57-63 ℃; Continue to heat up and add residue pre-emulsion I and initiator A PS (ammonium persulphate) 0.4-0.6kg, temperature is controlled at 87-93 ℃, continues to add pre-emulsion II and APS (ammonium persulphate) 0.4-0.6kg; And maintenance reaction 1.5h; Naturally cooling filters, and obtains the vinyl resin microemulsion of MPM modification.
Two, organic-silicon-modified high temperature resistant automatically cleaning water electrochemical antifouling paste
The powder stock pre-treatment:
Get the containing hydrogen silicone oil of powder stock total mass 1.5%,
Get the tensio-active agent OP-10 of silicone oil total mass 3%,
Get the deionized water of 10 times of silicone oil total masses;
Quantitative containing hydrogen silicone oil is dropped in the high speed dispersion still, drop into quantitative tensio-active agent OP-10 then, open low-speed mixer; Raw materials mix is even, close low-speed mixer then, open high speed dispersor; After the high speed dispersion 5 minutes; Begin to drip deionized water, through phase conversion method containing hydrogen silicone oil is emulsified into the containing hydrogen silicone oil emulsion, it is subsequent use to put into spray tank after the filtration;
Powder is dropped into stirred pot, the containing hydrogen silicone oil emulsion is sprayed onto stirred pot with atomizer, stir, stir and get final product while spraying;
Powder stock is respectively white titanium pigment, mica powder, kaolin, permanent white, every kind of independent pre-treatment of powder stock, and pretreated powder is the pre-treatment powder stock of organic-silicon-modified high temperature resistant automatically cleaning water electrochemical antifouling paste.
This antifouling paste prepares instance (1)
Remove ionized water 230g, PH regulator AMP-951g, ammonium salt dispersion agent 1.7g, sodium salt dispersion agent 5g, wetting agent PE-1001g; Terepthaloyl moietie 5g, film coalescence aid lauryl alcohol fat 18g, skimmer NXZ1g, pretreated white titanium pigment 130g; Pretreated kaolin 80g, pretreated permanent white 30g, modified phosphate aluminium 47g, zn phosphate 47g; Pretreated mica powder 50g, flow agent RM-20203.3g drops into above-mentioned raw materials in the high speed dispersion still high speed dispersion 1h successively; Under expect the paint still, add MPM modified emulsion 500g, skimmer NXZ1g, deionized water 35g; Under the stirring at low speed, drop into X-405 (dispersion wetting agent) 2g, anti-rust agent 5g, the preferred silane coupling agent γ-methacryloxy Trimethoxy silane 3g of dodging; Add anticorrosion and bactericidal agent 3g, add each an amount of viscosity of regulating of alkali swelling and polyurethane type thickening material, filter and package, promptly get white waterborne organic silicon modified, high temperature resistant automatically cleaning water electrochemical antifouling paste to desired value.
This antifouling paste prepares instance (2)
Remove ionized water 230g, PH regulator AMP-951g, ammonium salt dispersion agent 1.7g, sodium salt dispersion agent 5g, wetting agent (PE-100) 1g; Terepthaloyl moietie 5g, film coalescence aid lauryl alcohol fat 18g, skimmer NXZ1g, pretreated white titanium pigment 150g, pretreated permanent white 80g; Modified phosphate aluminium 50g, zn phosphate 40g, pretreated mica powder 60g, middle yellow 10g, pretreated kaolin 50g; Bright red 10g, flow agent (RM-2020) 3g drops into above-mentioned raw materials in the high speed dispersion still high speed dispersion 1h successively; Under expect the paint still, add MPM modified emulsion 550g, skimmer NXZ1g, deionized water 35g; Under the stirring at low speed, drop into X-405 (dispersion wetting agent) 2g, anti-rust agent 5g, the preferred silane coupling agent γ-methacryloxy Trimethoxy silane 3.3g of dodging; Add anticorrosion and bactericidal agent 3g, add each an amount of viscosity of regulating of alkali swelling and polyurethane type thickening material, filter and package, promptly get orange waterborne organic silicon modified, high temperature resistant automatically cleaning water electrochemical antifouling paste to desired value.
This antifouling paste prepares instance (3)
Remove ionized water 300g, PH regulator (AMP-95) 1g, ammonium salt dispersion agent 2.2g, sodium salt dispersion agent 4.8g, wetting agent (PE-100) 1g; Terepthaloyl moietie 5g, film coalescence aid lauryl alcohol fat 19g, skimmer NXZ1g, pretreated white titanium pigment 110g; Ferrophosphorus powder 130g, pretreated kaolin 60g, modified phosphate aluminium 50g, zn phosphate 40g; Carbon black 5g, flow agent (RM-2020) 3g drops into above-mentioned raw materials in the high speed dispersion still high speed dispersion 1h successively; Under expect the paint still, add MPM modified emulsion 530g, skimmer NXZ1g, deionized water 50g; Under the stirring at low speed, drop into X-405 (dispersion wetting agent) 2g, anti-rust agent 4.7g, the preferred silane coupling agent γ-methacryloxy Trimethoxy silane 2.9g of dodging; Add anticorrosion and bactericidal agent 3g, add each an amount of viscosity of regulating of alkali swelling and polyurethane type thickening material, filter and package, promptly get iron gray waterborne organic silicon modified, high temperature resistant automatically cleaning water electrochemical antifouling paste to desired value.
More than be the optimized embodiment of the present invention, comprise synthesis technique, the prescription of MPM (organosilicon) modified acrylic acid emulsion; Preparation technology, the formula for a product of finished product lacquer; According to the disclosed content of the present invention, the replacement scheme that those skilled in the art can consider, identical embodiment is category of the present invention.The MPM modified acrylic resin emulsion also can be used as the important source material in the high-end leather production among the present invention.
Characteristics of the present invention and principle are set forth:
Accomplish the coating protection of metal under harsh environment, must start with from the following aspects research:
1.
dense film must be formed to isolate the vapor , oxygen, and acid, alkali, salt intrusion of atmospheric gas, which requires the film-forming resin, crosslinking has sufficient strength in close, and the resin itself must be acid, alkali and salt corrosion. film resin once destroyed in harsh environments, the metal will be exposed naked and quickly corroded, at present, the traditional acrylic system (including the more popular epoxy-modified series) film formed by the emulsion, the degree of corrosion resistance are not satisfactory.The present invention has introduced organic-silicon-modified acrylic acid resin, has comparatively perfectly solved the erosion resistance ability problem of paint film self.And make paint film obtain the outstanding characteristic of silicone resin.
2.
Paint film be the persistent key factor of preservative effect by the adherence of coating metal, because paint film belongs to organism, be inorganics by coating metal, be difficult between the two form firm chemical bonding force, only depend on faint Van der Waals force to connect, the easy Fen Hua of paint film comes off under harsh environment.
The present inventionPreferred silane coupling agent has formed firm electrochemistry key bridge joint at paint film with between by matel coated, to traditional " parcel is with bonding " principle and method afford revolutionary upgrading, the perfect solution
AdherenceThis
KeyProblem.
Traditional its prescription of water-repellent preservation lacquer is also unreasonable when selecting fillerSuch as adding lime carbonate; Under the erosion of empty G&W, can become Calcium hydrogen carbonate; Because Calcium hydrogen carbonate is slightly soluble in water, under rainwash, will causes running off and cause paint film cavity, formation defective. the present invention's unreasonable fillers such as lime carbonate of having forgone; On the basis of conventional packing, added preferred zn phosphate and modified phosphate aluminium etc. and can form double salt and fine and close inner complex with iron rust and free iron; Thereby stoped the further free of metal, the surfactivity that terminated free metal loses electronics and oxidized corrosive process, and inner complex can make the active metal atom lose activity; Double salt can make already oxidised each loose attitude red stone (metal) form dense structure; Thereby realized the band rust, changeed rust and antirust perfect function. be exactly that zn phosphate is and can forms complex compound Fe [Zn3 (P04) 3] beds of precipitation of adhere firmly and suppress anodic reaction in metallic surface and Fe3+ specifically; Simultaneously can with hydroxyl, carboxyl complexing in the coating, make to form Chemical bond between pigment-coating-ground and improve adhesive force of coatings and impermeability.Aluminium triphosphate is a white pigment, is slightly soluble in water, and ionization goes out when under coating, dissolving, and is combined into the insoluble chelate passive film at anode position and metals ion, and this film hardness is high, adhere firmly.
Organic-silicon-modified high temperature resistant automatically cleaning water electrochemical antifouling paste
The performance test table
Claims (5)
1. organic-silicon-modified high temperature resistant automatically cleaning water electrochemical antifouling paste; Its raw material comprises resin emulsion; It is characterized in that resin emulsion is the acrylic resin modified microemulsion of MPM; It also has coupling agent γ-methacryloxy Trimethoxy silane, and the adding proportion of coupling agent γ-methacryloxy Trimethoxy silane is the 0.5-3% of raw material total amount.
2. organic-silicon-modified high temperature resistant automatically cleaning water electrochemical antifouling paste synthesis technique according to claim 1; Comprise the antifouling paste synthesis technique, it is characterized in that it also has the powder stock pretreatment technology, pretreatment process is:
Get the containing hydrogen silicone oil of powder stock total mass 1.2-1.8%,
Get the tensio-active agent OP-10 of silicone oil total mass 2.5-3.5%,
Get silicone oil total mass 9-11 deionized water doubly;
Quantitative containing hydrogen silicone oil is dropped in the high speed dispersion still, drop into quantitative tensio-active agent OP-10 then, open low-speed mixer; Raw materials mix is even, close low-speed mixer then, open high speed dispersor; After high speed dispersion 4-6 minute; Begin to drip deionized water, through phase conversion method containing hydrogen silicone oil is emulsified into containing hydrogen silicone oil emulsion (promptly join promptly and use), it is subsequent use to put into spray tank after the filtration;
Powder is dropped into stirred pot, the containing hydrogen silicone oil emulsion is sprayed onto stirred pot with atomizer, stir, stir and get final product while spraying;
Powder stock is respectively white titanium pigment, mica powder, kaolin, permanent white; Every kind of independent pre-treatment of powder stock; Pretreated powder is the pre-treatment powder stock of organic-silicon-modified high temperature resistant automatically cleaning water electrochemical antifouling paste, gets into subsequent processing again---the dispersion mill slurry process.
3. organic-silicon-modified high temperature resistant automatically cleaning water electrochemical antifouling paste according to claim 1 is characterized in that the acrylic resin modified microemulsion parts by weight of raw materials of MPM proportioning is:
Methylacrylic acid (MAA) 1.5-2.0
Methacryloxypropyl methoxymethyl phenyl silicone oil (MPM) 1.4-1.8
TEB 3K (MMA) 1.2-1.4
Ammonium persulphate (APS) 0.1-1.0
Vinylbenzene (ST) 0.5-0.8
Concentration is 30% ammoniacal liquor 1.0-3.0
Vinyl cyanide (AN) 1.0-2.0 part
AEO-3 (AEO-3) 0.1-1
AEO-7 (AEO-7) 0.1-1
N-butyl acrylate (BA) 5-12
PEG 400 (PEG-400) 0.8-1.5
Polyoxyethylenated alcohol sodium sulfate (AES) 0.5-2.0
Vinylformic acid one 2 one ethylhexyls (2-EHA) 5-12
Sodium lauryl sulphate (SDS) 0.5-2
Water 4-8.
4. organic-silicon-modified high temperature resistant automatically cleaning water electrochemical antifouling paste according to claim 2 is characterized in that the acrylic resin modified preparation of microemulsion method of MPM is:
(1) monomeric preparatory emulsification: with a part of AEO-7 (AEO-7), sodium lauryl sulphate (SDS), polyoxyethylenated alcohol sodium sulfate (AES), PEG 400 (PEG-400), with TEB 3K (MMA), vinylbenzene (ST), vinyl cyanide (AN), mix to stir and process newborn pre-emulsion I; Again remaining AEO-7 (AEO-7) is added in AEO-3 (AEO-3), TEB 3K (MMA), n-butyl acrylate (BA), vinylformic acid one 2 one ethylhexyls (2-EHA), the methacryloxypropyl methoxymethyl phenyl silicone oil (MPM); Under agitation slowly add a part of water, process the pre-emulsion II with the phase inversion dispersion method;
(2) micro-emulsion polymerization: in the four-hole bottle that TM, whisking appliance, prolong are housed, add another part water, stir, add part pre-emulsion I; With ammoniacal liquor adjust pH to 7, begin to heat up, add initiator ammonium persulfate (APS) when being warming up to 57-63 ℃; Continue to heat up and add another part pre-emulsion I and initiator A PS, temperature is controlled at 87-93 ℃, continues to add pre-emulsion II and APS; And maintenance reaction 1.2-1.8h; Naturally cooling filters, and obtains the vinyl resin microemulsion of MPM modification.
5. according to claim 3 or 4 described organic-silicon-modified high temperature resistant automatically cleaning water electrochemical antifouling pastes, it is characterized in that the preparation method of methacryloxypropyl methoxymethyl phenyl silicone oil (MPM) is: the catalyzing and condensing method, by HO (MephSiO)
nH and CH2=CMeCOOC3H6SiMe (OMe) 2 hydrolytic condensation and getting under granular sulfonic acid ion exchange resin catalysis.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105063624A (en) * | 2015-08-21 | 2015-11-18 | 无锡乐华自动化科技有限公司 | Anti-rusting agent for wheel hub |
| CN107892856A (en) * | 2017-11-23 | 2018-04-10 | 江门市水星涂料科技有限公司 | A kind of water-based all-round conversion and prevention paint of rust and preparation method thereof |
| CN111019465A (en) * | 2019-12-27 | 2020-04-17 | 海安常州大学高新技术研发中心 | Preparation process of organic-inorganic composite water-based acrylic acid anticorrosive paint |
| CN117468268A (en) * | 2023-12-27 | 2024-01-30 | 湖南大道新材料有限公司 | Water-blocking paper bag and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5094889A (en) * | 1989-05-10 | 1992-03-10 | Ashland Oil, Inc. | Water based coating for roughened metal surfaces |
| CN101857753A (en) * | 2010-06-22 | 2010-10-13 | 深圳大学 | Anticorrosive coating as well as coating method and application thereof |
-
2012
- 2012-08-17 CN CN201210293904.9A patent/CN102838913B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5094889A (en) * | 1989-05-10 | 1992-03-10 | Ashland Oil, Inc. | Water based coating for roughened metal surfaces |
| CN101857753A (en) * | 2010-06-22 | 2010-10-13 | 深圳大学 | Anticorrosive coating as well as coating method and application thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105063624A (en) * | 2015-08-21 | 2015-11-18 | 无锡乐华自动化科技有限公司 | Anti-rusting agent for wheel hub |
| CN107892856A (en) * | 2017-11-23 | 2018-04-10 | 江门市水星涂料科技有限公司 | A kind of water-based all-round conversion and prevention paint of rust and preparation method thereof |
| CN111019465A (en) * | 2019-12-27 | 2020-04-17 | 海安常州大学高新技术研发中心 | Preparation process of organic-inorganic composite water-based acrylic acid anticorrosive paint |
| CN117468268A (en) * | 2023-12-27 | 2024-01-30 | 湖南大道新材料有限公司 | Water-blocking paper bag and preparation method and application thereof |
| CN117468268B (en) * | 2023-12-27 | 2024-03-22 | 湖南大道新材料有限公司 | Water-blocking paper bag and preparation method and application thereof |
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