CN101705040B - Fluorine-modified methacrylic acid epoxy powder paint and preparation method thereof - Google Patents
Fluorine-modified methacrylic acid epoxy powder paint and preparation method thereof Download PDFInfo
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- CN101705040B CN101705040B CN200910153758A CN200910153758A CN101705040B CN 101705040 B CN101705040 B CN 101705040B CN 200910153758 A CN200910153758 A CN 200910153758A CN 200910153758 A CN200910153758 A CN 200910153758A CN 101705040 B CN101705040 B CN 101705040B
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Abstract
The invention relates to a preparation method of a fluorine-modified methacrylic acid epoxy powder paint, which comprises the following steps of: mixing following raw materials by weight percent: 50-70 percent of hexafluorobutyl methacrylate modified epoxy resin, 1-4 percent of curing agent, 0.5-1.5 percent of polyacrylicester flatting agent, 0.5-1.5 percent of acrylate copolymer moistening accelerator, 0.1-0.3 percent of anti-yellowing benzoin, 5-25 percent of titanium white powder, 5-20 percent of barium sulphate, 0.5-1.5 percent of flow promoter, 1-20 percent of pigment and 0.1-1 percent of assistant; melt-mixing the raw materials at 90-115 DEG C and extruding; feeding the raw materials to a pulverizer to grind after sheeting and crushing; and screening to obtain the needed powder paint. When the powder paint prepared by adopting the invention is used, a coating film has thesurface properties of hydrophobicity, oleophobic and the like, as well as luminous and flat appearance. Compared with a common epoxy powder paint, the invention has the advantages of more excellent performances of stain resistance, weather resistance, corrosion resistance, scumbling, low cost, and favorable application prospect in the fields of home appliances, transports, metals machinery and the like.
Description
Technical field
The present invention relates to art of powder coatings, be specifically related to a kind of fluorine-modified methacrylic acid epoxy powder paint and preparation method thereof.
Background technology
Powder coating is as a kind of coating variety of fast development, and advantage such as have solvent-free, pollution-free, less energy-consumption, coating efficiency is high, storing is convenient has great market potential.Along with the sustained, stable growth of China's economy and improving constantly of living standards of the people, the powder coating business also constantly increases.
Wherein epoxy powder coating is widely used in household electrical appliances, the vehicles with strong, the high temperature resistant and excellent electrical insulation capability of its bonding force, and fields such as hardware machinery are one of of paramount importance coating types in the powder coating.
The electronegativity of fluorine atom is extremely strong in the fluoropolymer; C-F key bond energy is very big; Polarizability is low, and the F atomic radius is little, shows special surface properties such as good weather resistance, weathering resistance, chemical proofing, low surface tension and hydrophobic, oleophobic property; But, limited its Application and Development because the fluoro-resin price is higher.And, preservative property, resistance to soiling and the cost of epoxy powder coating are had higher requirement at coated metal etc.The ordinary epoxy resin powder coating because have that coating is thick partially, problems such as resistant and loss of properties on aging, receive certain limitation in corresponding application techniques field.
Summary of the invention
The technical problem that the present invention will solve is the deficiency to existing common epoxide powder coating resistant, antiseptic property on the hardware application techniques, provides a kind of antifouling property, coating antiseptic and decorate properties excellent powder coating.
For solving the problems of the technologies described above, the present invention provides a kind of fluorine-modified methacrylic acid epoxy powder coating preparation method to comprise step: supply raw materials, composition that said raw material comprises and corresponding weight percent are: methylacrylic acid hexafluoro butyl ester modified epoxy 50%～70%; Solidifying agent 1%～4%, polyacrylate flow agent 0.5%～1.5%, Yodo Sol GH 28 wetting enhancer 0.5%～1.5%; Anti-xanthochromia st-yrax 0.1%～0.3%; White titanium pigment 5%～25%, permanent white 5%～20%, flow improver additive 0.5%～1.5%; Pigment 1%～20%, auxiliary agent 0.1%～1%;
With the above-mentioned raw materials thorough mixing evenly after, mixingly melt extrude at 90 ℃～115 ℃ by screw extrusion press; With sending pulverizing mill to grind after the material cooling compressing tablet of extruding, the fragmentation, obtain required powder coating after sieving.
Alternatively, said methylacrylic acid hexafluoro butyl ester graft modification epoxy resin molecule comprises/has following structure:
Wherein n is a natural number.
Alternatively; Described methylacrylic acid hexafluoro butyl ester graft modification epoxy resin is methylacrylic acid hexafluoro butyl ester and bisphenol A type epoxy resin, or the epoxy acrylic resin of one or more monomers fluorine-containing side chain of synthetic under the effect of peroxide initiator in methylacrylic acid hexafluoro butyl ester, bisphenol A type epoxy resin and vinylbenzene, methyl acrylate, Bing Xisuandingzhi, vinylformic acid ethylhexyl, acrylic amide, the Hydroxyethyl acrylate.
Alternatively, described solidifying agent is for being Dyhard RU 100.
Alternatively, described permanent white is process white or ultra-fine barium sulfate.
Alternatively, described white titanium pigment is a Rutile type Titanium Dioxide.
Alternatively, described flow improver additive can be the waxy organic cpds, for example can be the commercially available prod W-1 type flow of powder auxiliary agent of the South Sea, Ningbo chemistry ltd, as surface conditioner, reduces melt viscosity, increases the masking liquid flowability, removes gas.
Alternatively, said anti-xanthochromia st-yrax is used as air release agent, and effect is the bubble of eliminating in the melted powder masking liquid, also promptly eliminates the principal element that forms the needle pore defect of filming.
Alternatively, described pigment can be all kinds of conventional organic or inorganic pigment, and mainly the requirement according to painting color adds according to a certain percentage.
Alternatively, described auxiliary agent can be to increase in hard agent, growth agent, glossing agent, the matting agent one or more.
Fluorine-modified methacrylic acid epoxy powder paint of the present invention adopts the electrostatic spraying constructional method to act on the steel substrate of sandblast or ball blast, phosphatization, chromaking pre-treatment; Solidified 15 minutes through 180 ℃-200 ℃; Naturally cool to room temperature, behind the placement 24h, coating reaches working strength.
The fluorine-modified methacrylic acid epoxy powder paint that the method for the invention is prepared, its fluorine-containing side chain can concentrate on coatingsurface after film forming; Bring into play the effect of fluorine atom to greatest extent, make coating have the hydrophobic of excellence, oleophobic surface characteristic; Compare with the ordinary epoxy resin powder coating; Its quiet contact angle improved at least 15 °, can significantly improve the contamination resistance of body surface, has excellent corrosion resistance nature and surface abrasion resistance simultaneously.
Embodiment
In following examples, contact angle is measured and is adopted German Data physics OCA20 video optics contact angle measurement.Testing method is: contact medium adopts deionized water, and droplet size is 5 μ L, and drop contacts 30 seconds with coating begins take off data later on, selects carry out normal temperature Static Contact angular measurement at 12 of the coatingsurface different positions.
Embodiment 1
Material rate (wt%)
Methylacrylic acid hexafluoro butyl ester graft modification epoxy resin 68
Dyhard RU 100 3
Polyacrylate flow agent 0.5
Yodo Sol GH 28 wetting enhancer 0.5
Anti-xanthochromia st-yrax 0.3
Rutile type Titanium Dioxide 20
Permanent white 6
Flow improver additive 0.5
Ultramarine 1.2
Each component pre-mixing in the above-mentioned prescription is disperseed, melt extrude 115 ℃ of twin screw extruders, compressing tablet, fragmentation, 160 eye mesh screens sieve, white fluorin modified crylic acid epoxide powder coating.
The coating performance test result of utilizing above-mentioned fluorin modified crylic acid epoxide powder coating to make is following:
Appearance of film: smooth smooth, no shrinkage cavity, free of pinholes;
Coating thickness: 35-60um;
Impact strength: 50kgcm;
Test is just recoiling: through;
Pencil hardness test: 2H does not have scuffing;
Bending hardness test: 0T is curved to be passed through;
Sticking power: 1 grade;
The salt spray resistance test: corrosion strength was not more than 1 grade in 1000 hours;
Cupping: protruding height is not less than 8mm;
Contact angle: 97 °.
Embodiment 2
Material rate (wt%)
Methylacrylic acid hexafluoro butyl ester graft modification epoxy resin 57
Dyhard RU 100 3
Polyacrylate flow agent 1.5
Yodo Sol GH 28 wetting enhancer 0.5
Anti-xanthochromia st-yrax 0.7
Rutile type Titanium Dioxide 5
Permanent white 25
Flow improver additive 1.5
Carbon black 3.2
Phthalein cyanogen green 0.6
E-H red 0.5
Matting agent 1.5
Above-mentioned prescription is pressed the working method preparation among the embodiment 1, can obtain a kind of grey powder coating.
The coating performance test result of utilizing above-mentioned fluorin modified crylic acid epoxide powder coating to make is following:
Appearance of film: smooth smooth, no shrinkage cavity, free of pinholes;
Coating thickness: 35-50um;
Impact strength: 50kgcm
Test is just recoiling: through;
Pencil hardness test: 2H does not have scuffing
Bending hardness test: 0T is curved to be passed through
Sticking power: 1 grade
The salt spray resistance test: corrosion strength was not more than 1 grade in 1000 hours;
Cupping: protruding height is not less than 8mm;
Contact angle: 92 °.
Embodiment 3
Material rate (wt%)
Methylacrylic acid hexafluoro butyl ester graft modification epoxy resin 50
Dyhard RU 100 2
Polyacrylate flow agent 1.5
Yodo Sol GH 28 wetting enhancer 1.5
Anti-xanthochromia st-yrax 0.5
Rutile type Titanium Dioxide 25
Permanent white 15
Flow improver additive 1.5
Organic yellow 0.5
Phthalein cyanogen green 0.6
Scratching resistant 1.9
Above-mentioned prescription by pre-mixing, is melt extruded in twin screw extruder, mixing, cooling, compressing tablet, coarse breaking then, preferred ACM air classifying barreling mill, classification, 160 orders sieve, and obtain qualified scratching resistant fluorin modified crylic acid epoxide powder coating.
The coating performance test result of utilizing above-mentioned fluorin modified crylic acid epoxide powder coating to make is following:
Appearance of film: smooth smooth, no shrinkage cavity, free of pinholes;
Coating thickness: 35-50um;
Impact strength: 50kgcm;
Test is just recoiling: through;
Pencil hardness test: 2H does not have scuffing;
Bending hardness test: 0T is curved to be passed through;
Sticking power: 1 grade;
The salt spray resistance test: corrosion strength was not more than 1 grade in 1000 hours;
Cupping: protruding height is not less than 8mm;
Contact angle: 92 °;
Acid resistance test: 3%HCl solution soaking, 250 hours no changes;
Alkali resistance test: 5%NaOH solution soaking, 180 hours no changes.
Embodiment 4
Material rate (wt%)
Methylacrylic acid hexafluoro butyl ester graft modification epoxy resin 60
Dyhard RU 100 3
Polyacrylate flow agent 0.8
Yodo Sol GH 28 wetting enhancer 1.0
Anti-xanthochromia st-yrax 0.5
Rutile type Titanium Dioxide 5
Permanent white 15
Lime carbonate 7
Flow improver additive 1.5
Carbon black 4.5
Phthalein cyanogen green 0.6
Sand streak agent 1.1
Above-mentioned prescription is pressed pre-mixing; In twin screw extruder, melt extrude then, mixing, cooling, compressing tablet, coarse breaking; After preferred ACM air classifying barreling mill, classification, 160 orders sieve, and obtain qualified black sand streak type fluorin modified crylic acid epoxide powder coating.
The coating performance test result of utilizing above-mentioned fluorin modified crylic acid epoxide powder coating to make is following:
Appearance of film: smooth smooth, no shrinkage cavity, free of pinholes;
Coating thickness: 40-55um;
Impact strength: 50kgcm;
Test is just recoiling: through;
Pencil hardness test: 2H does not have scuffing;
Bending hardness: 0T is curved to be passed through;
Sticking power: 1 grade;
The salt spray resistance test: corrosion strength was not more than 1 grade in 1000 hours;
Cupping: protruding height is not less than 8mm;
Contact angle: 94 °;
Acid resistance test: 3%HCl solution soaking, 250 hours no changes;
Alkali resistance test: 5%NaOH solution soaking, 180 hours no changes.
Though the present invention with preferred embodiment openly as above; But it is not to be used for limiting claim; Any those skilled in the art are not breaking away from the spirit and scope of the present invention; Can make possible change and modification, so protection scope of the present invention should be as the criterion with the scope that claim of the present invention was defined.
Claims (5)
1. the preparation method of a fluorine-modified methacrylic acid epoxy powder coating is characterized in that, comprises step:
Supply raw materials, composition that said raw material comprises and corresponding weight percent are: methylacrylic acid hexafluoro butyl ester modified epoxy 50% to 70%, solidifying agent 1% to 4%; Polyacrylate flow agent 0.5% to 1.5%, Yodo Sol GH 28 wetting enhancer 0.5% to 1.5%, anti-xanthochromia st-yrax 0.1% to 0.3%; White titanium pigment 5% to 25%, permanent white 5% to 20%, flow improver additive 0.5% to 1.5%; Pigment 1% to 20%, auxiliary agent 0.1% to 1%;
With the above-mentioned raw materials thorough mixing evenly after, mixingly melt extrude at 90 ℃ ~ 115 ℃ by screw extrusion press;
With sending pulverizing mill to grind after the material cooling compressing tablet of extruding, the fragmentation and sieving;
Said methylacrylic acid hexafluoro butyl ester modified epoxy molecule has following structure:
Wherein n is a natural number;
Perhaps; Described methylacrylic acid hexafluoro butyl ester modified epoxy is methylacrylic acid hexafluoro butyl ester and bisphenol A type epoxy resin, or the epoxy acrylic resin of one or more monomers fluorine-containing side chain of synthetic under the effect of peroxide initiator in methylacrylic acid hexafluoro butyl ester, bisphenol A type epoxy resin and vinylbenzene, methyl acrylate, Bing Xisuandingzhi, vinylformic acid ethylhexyl, acrylic amide, the Hydroxyethyl acrylate.
2. the preparation method of fluorine-modified methacrylic acid epoxy powder coating as claimed in claim 1 is characterized in that: described solidifying agent is a Dyhard RU 100.
3. the preparation method of fluorine-modified methacrylic acid epoxy powder coating as claimed in claim 1 is characterized in that: described permanent white is process white or ultra-fine barium sulfate.
4. the preparation method of fluorine-modified methacrylic acid epoxy powder coating as claimed in claim 1 is characterized in that: described white titanium pigment is a Rutile type Titanium Dioxide.
5. according to the prepared epoxy powder coating of each described preparation method in the aforementioned claim.
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| CN200910153758A CN101705040B (en) | 2009-11-05 | 2009-11-05 | Fluorine-modified methacrylic acid epoxy powder paint and preparation method thereof |
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| CN200910153758A CN101705040B (en) | 2009-11-05 | 2009-11-05 | Fluorine-modified methacrylic acid epoxy powder paint and preparation method thereof |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286131B (en) * | 2011-05-07 | 2013-04-24 | 大连交通大学 | Organic fluorine monomer modified epoxy acrylate emulsion and preparation method thereof as well as antifouling paint containing the emulsion and preparation method thereof |
| CN102732124A (en) * | 2012-06-04 | 2012-10-17 | 上海大学 | Fluorine-containing heavy-duty anticorrosive coating and its application |
| CN104194430A (en) * | 2014-07-24 | 2014-12-10 | 蚌埠市鸿安精密机械有限公司 | High hydrophobic and oleophobic powder coating |
| CN104130666A (en) * | 2014-07-29 | 2014-11-05 | 丹阳市海信涂料化工厂 | Formula for preparation of low-temperature curing heavy-duty anticorrosion epoxy powdery coating |
| CN104293063A (en) * | 2014-10-14 | 2015-01-21 | 苏州洛特兰新材料科技有限公司 | Thermosetting acrylic resin powder coating for ceramic |
| CN104927590A (en) * | 2015-07-09 | 2015-09-23 | 张作玮 | Preparation method for powder coating |
| CN104946096A (en) * | 2015-07-09 | 2015-09-30 | 张作玮 | Prepetition method of protective powder coating |
| CN106010143A (en) * | 2016-06-08 | 2016-10-12 | 合肥市燕美粉末涂料有限公司 | Anti-souring corrosion-resistant powder paint and preparing method thereof |
| CN108341621A (en) * | 2018-02-28 | 2018-07-31 | 无锡金久泓科技有限公司 | A kind of resin concrete and preparation method thereof that fluorine monomer is modified |
| CN109306201B (en) * | 2018-09-29 | 2022-08-26 | 黄山华惠科技有限公司 | High-temperature-resistant and boiling-resistant leveling agent and application thereof in preparation of powder coating |
| CN112322152A (en) * | 2020-11-11 | 2021-02-05 | 惠州市惠阳区嘉泰涂料有限公司 | Corrosion-resistant powder coating and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560278A (en) * | 2009-05-25 | 2009-10-21 | 河北工业大学 | Methyl methacrylate-styrene copolymer containing fluoro-acrylate and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560278A (en) * | 2009-05-25 | 2009-10-21 | 河北工业大学 | Methyl methacrylate-styrene copolymer containing fluoro-acrylate and preparation method thereof |
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Inventor after: Wu Xuedong Inventor after: Xu Xiaolong Inventor after: Li Baosong Inventor before: Li Baosong Inventor before: Xu Xiaolong Inventor before: Wu Xuedong |
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