CN101358097A - Nano composite powder coatings and dispersion polymerization preparation method thereof - Google Patents
Nano composite powder coatings and dispersion polymerization preparation method thereof Download PDFInfo
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Abstract
The present invention relates to the field of nano-powder composite material preparation, in particular to a composite nano-powder coating and a preparation method adopting dispersion polymerization thereof. The ingredients used to prepare the nano-powder coating include water, alcohol, monomer mixture, inorganic nano-particles, pigment filler and assistant. Surface treatment is first carried out on the nano-particles and the pigment filler, which are then added into the monomer mixture and dispersed by ultrasonic so that mixed solution is produced. Then, the mixed solution is added into alcohol-water mixed solution containing dispersion stabilizer and dispersed by ultrasonic, and after six hours of temperature reaction, the product undergoes centrifugation and vacuum drying so that the final product is prepared. The present invention resolves the defects of the prior art, including large powder particle diameter, uneasy scumbling and uneven coating, and avoids the problems of the complexity of the traditional preparation technique and the easy agglomeration of nano-particles in organic polymers. The preparation method adopting dispersion polymerization has the advantages of short process flow, little investment, energy saving, no powder pollution, etc.; the prepared powder coating is characterized by neat particle shape, small particle diameter and easy scumbling and has functions such as antibacterial function and ultraviolet-resisting function; the powder coating in use has good leveling property.
Description
Technical field
The present invention relates to a kind of nano powder composite material and make field, particularly nano composite powder coatings and dispersion polymerization preparation method thereof.
Background technology
Powder coating has the advantage of environmental protection and energy saving and economical and efficient, in producing and constructing, there is not solvent contamination, the environmental protection coating material that belongs to a quasi-representative, be widely used in that oil and gas pipeline is anticorrosion, manufacturing field such as automobile making, air-conditioning, refrigerator, washing machine and five metals household electrical appliances, make powder coating obtain fast development along with energy-saving and emission-reduction are strict in recent years.
Powder coating adds pigment by resin and a little auxiliary is a raw material, and melt extrude postcooling through mix heating up and be broken into strip, the powder that becomes to need through mechanical disintegration again, it belongs to the physical mechanical breaking method.Common technology comprises six big processing steps such as resin is synthetic, mixing of materials, heating and melting, cooling granulation, mechanical disintegration, mistake screen sizing.Obviously, there is long flow path in traditional technology, and facility investment is big, waste man-hour, shortcoming such as waste energy, and in addition, also easily produces dust pollution in process of production.
Yet there are some restrictions at present in the application of powder coating, the one, can not obtain liquid coating smooth coatingsurface like that; The 2nd, can not obtain liquid coating like that than shallow layer thickness, this has just limited its use on a lot of expensive goods, has also limited the further reduction of painting cost.Its major cause is that the big and out-of-shape of the particle diameter of powder coating particle causes, and conventional powder coating particle diameter is at the 30-70 micron, and coat-thickness is the 60-100 micron, and the liquid coating coating is generally at the 20-30 micron.If the powder coating thickness is below 50 microns, coating can tangerine peel or part grinning effect occur because of uneven thickness.If make ultrafine powder paint below 20 microns, and coating particle be the rule the ball-type structure, just can overcome its top coat unfairness and the too thick shortcoming of coating.
For solving the shortcoming that the powder coating manufacturing process flow is long and use, many researchists have carried out some explorations and trial.We had once invented micro-suspension one-step manufacture method (CN14556613A), though can overcome the long deficiency of manufacturing process flow, the powder diameter big (greater than 30 microns) of this method preparation.Nishida etc. have invented the method (USP5,567,521) of adding lubricant, make powder have good mobility, obtained the product of small particle size good fluidity, but it is too many to add the lubricant dosage, bringing negative interaction aspect gloss and the levelling property, difficult realization industrialization.Guo Lixiao etc. (200410024952.3) adopt organic solvent that coating resin is dissolved, add color stuffing, carry out the pressurized spray drying through high speed dispersion and obtain powder coating, though powder diameter less (10-25 micron), this method need use a large amount of organic solvents to come dissolving resin.In recent years,, some nanometer powder coating also occurred,, realized the functionalization of coating by some special performances of nano material along with going deep into of nano materials research, as uviolresistance, germ resistance, antistatic performance etc.Patent CN1462783A has prepared epoxide powder coating by add inorganic nano antiseptic in coating, and coating has tangible anti-microbial property; It is the nano inorganic nano composite material of 10～100nm that patent ZL 03117985.1 uses particle diameter, the weather resistant polyurethane powder coating of modification, the polyurethane powder coating that its anti-aging index does not more contain inorganic nano composite material has improved 100%～200%, and the powder coating that hardness, sticking power, shock strength etc. more do not contain inorganic nano composite material is improved to some extent.But the manufacturing process of these nanometer powder coating all is a traditional technology, by pre-mixing, melt extrude mixing, cooling, fragmentation, fine powder is broken, classification is sieved etc., and six procedures are realized.
Nano titanium oxide, nano material such as nano zine oxide and nano silicon oxide has good shielding ultraviolet rays, photochemical catalysis, antibacterial and deodouring and electric property, utilize these nano materials can prepare functional powder coating, but nano particle diameter is little, specific surface area and surface energy are very big, be easy to reunite, even the primary particle size that obtains by chemical process reaches nano level, but these primary particles still can be reunited very well in processing powder coating process, become hundreds of nanometer even larger sized coacervate, so simple inorganic nano-particle is difficult for being scattered in the organic polymer, and between organic polymer and the inorganic particulate serious phenomenon of phase separation is often arranged.This has seriously hindered the performance of nanoparticle performance, and therefore improving the dispersion of nanoparticle in the powder coating polymkeric substance seems particularly important.In addition, irregular by the powder coating particle shape that melt extrudes comminuting method preparation, contain sheet, triangle, cubic shape or spherical etc. multiple, this can influence powder coating levelling property in use.
Summary of the invention
The objective of the invention is to overcome that above traditional powder coating manufacturing process is numerous and diverse, thick coating unfairness and nanoparticle be difficult for dispersive deficiency in polymkeric substance, provide a kind of novel nano composite powder coatings and manufacture method.Present method is carried out copolymerization will contain vinyl monomer, and will contain treated inorganic nano-particle and pigment in the presence of relevant auxiliary agent as required, by similar diffuse-aggregate technology one-step synthesis powder coating as feature.Because monomer can be dissolved in pure water hybrid reaction medium, treated inorganic particulate is scattered in reaction system under the dispersion stabilizer effect, monomer begins to carry out polyreaction under the initiator effect, the polymer chain molecular weight that generates becomes big gradually, cause that self polarity changes, mix principle as can be known by similar, the solubleness that increases in reaction medium along with the molecular weight of polymer chain reduces gradually, reach after the critical chain length, precipitating is come out from medium, under function of stabilizer, very easily become entangled in and form stable nuclear on the nano inoganic particle of modification, be suspended in the elementary growth nuclear that forms in the medium, monomer in the absorption reaction medium and free radical, monomer and free radical are proceeded polyreaction in nuclear, the volume of particle constantly increases, and finally generates the composite powder of polymer overmold inorganic nano-particle.
The nanometer powder system component is among the present invention:
Nano composite powder coatings, it comprises the component of following unit mass part:
Water 100～150 pure 20-80 mix monomer 50～100 inorganic nano-particle 5-20
Color stuffing 5-40 dispersion stabilizer 5-30 initiator 0.5-5 surface-modifying agent 1～10
Wherein mix monomer is the mixed thing of hard monomer, soft monomer and function monomer, and auxiliary agent is dispersion stabilizer, initiator and surface-modifying agent.
Preparation method of the present invention is:
The dispersion polymerization manufacturing process of nano composite powder coatings comprises following processing step:
A, earlier inorganic nano-particle and color stuffing are carried out surface treatment, again in the inorganic nano-particle that will handle and the color stuffing adding mix monomer,, make that to give dispersion liquid stand-by by ultrasonic dispersing 30 minutes;
B, dispersion stabilizer, water and pure mixed solvent are added reaction flask according to the order of sequence, add prepare in the A step give dispersion liquid and initiator, ultra-sonic dispersion 20 minutes, start stirring heating, 75 ℃ of reactions 2.5～4.5 hours, be warming up to 80 ℃ of afterreactions 2～3 hours, cooling, discharging, centrifugal, oven dry promptly get product.
The concrete technical parameter of each component is among the present invention:
Each composition weight proportioning is in the mix monomer:
Hard monomer 60～90, soft monomer 20～50, function monomer 2～10
Wherein hard monomer is including, but not limited to selecting one or more the mixture in methyl methacrylate, methyl acrylate, vinylbenzene, vinyl toluene, vinyl acetate between to for plastic, acrylonitrile, the methacrylic eyeball for use;
Soft monomer is including, but not limited to selecting one or more the mixture in ethyl propenoate, butyl acrylate, Ethyl acrylate, Octyl acrylate, Isooctyl acrylate monomer, the 2-EHA for use; Function monomer is including, but not limited to selecting one or more the mixture in vinylformic acid, methacrylic acid, propenoic acid beta-hydroxy ethyl ester, propenoic acid beta-hydroxy propyl ester, Jia Jibingxisuanβ-Qiang Yizhi, methacrylic acid β-hydroxypropyl acrylate, N hydroxymethyl acrylamide, the N-methoxymethyl acrylamide for use.
Inorganic nano-particle is including, but not limited to selecting one or more mixtures in nano titanium oxide, nano zine oxide, nano silicon, nano-sized iron oxide, nano calcium oxide, nano-calcium carbonate, the nano alumina particles for use.
Described alcohol is including, but not limited to selecting more than one mixture of a kind of in the short chain alcohol or its for use.Wherein particularly preferably be more than one mixture of a kind of in methyl alcohol, ethanol, the propyl alcohol or its.
The color stuffing particle diameter is below 1 micron, comprise tinting pigment and pigment extender, tinting pigment is including, but not limited to selecting one or more the mixture in titanium dioxide, zinc sulfide white, iron oxide red, iron oxide yellow, ultramarine, the chrome green for use, pigment extender is including, but not limited to selecting one or more the mixture in lime carbonate, china clay, talcum powder, ground barium sulfate, the superfine alumina silicate for use, and tinting pigment and pigment extender are oleophylic water repellency pigment after treatment.
Dispersion stabilizer is including, but not limited to selecting one or more the mixture in hydroxy propyl cellulose, polyethylene pyrrolidone, the polymethyl acrylic acid for use, azo two isobutyls are fine including, but not limited to selecting for use for initiator, two different heptan of benzoyl peroxide, lauroyl peroxide, di-isopropyl peroxydicarbonate, di-cyclohexylperoxy dicarbonate, azo one or more the mixture in fine.
This nano composite powder coatings wherein also has surface treatment agent, and surface treatment agent is including, but not limited to selecting one or more the mixture in stearic acid, trieline base silane, triethoxyl silane, titanate ester, the aluminium esters of gallic acid coupling agent for use.
Nano particle diameter scope described in the present invention is shaped as regular spherical, good flowing properties at 5～15 microns.Coatingsurface is smooth, and thickness reaches 10～30 microns, has significantly antibiotic and anti-ultraviolet function.
Preparation method's concrete processing condition are among the present invention:
Described surface treatment is to adopt surface treatment agent that inorganic nano-particle and color stuffing surface are handled.
The obtained technical progress of the present invention is:
(1) manufacture method with traditional powder coating changes 1 footwork into from 6 footworks, compares with the conventional fabrication processes of powder coating, and technical process is short, facility investment is few, save the man-hour and the energy, and dust pollution is lighter.
(2) adopt the dispersion polymerization technology, reduced the particle diameter (5-15 micron) of powder, be convenient to the scumbling of powder, improve its planeness.In addition, this powder coating can be given the function of some nano materials, solved simultaneously nanoparticle easy reunion and with the compatibility issue of polymkeric substance, the powder particle particle diameter is the regular spherical shape of 5-15 micrometer range, have good mobility can powder.Prepared metallic coating thickness is the 10-30 micron, has even curface.By the absorption ultraviolet ray performance and the anti-microbial property of nanoparticle uniqueness, make the composite nanometre powder coating have significantly antibiotic and anti-ultraviolet function.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment
Each set of dispense ratio is:
Deionized water 250 ethanol 50 mix monomers 100 nano-ZnO particles 10
Color stuffing 20 dispersion stabilizers 10 initiators 1.5 surface treatment agents 1.0.
The ratio of components of above-mentioned mix monomer ingredient is:
Hard monomer 80 soft monomers 30 function monomers 2.
Wherein the inorganic nano antiseptic particle is selected nano zinc oxide powder for use, the consisting of of hard monomer:
Methyl methacrylate (polymerization-grade) 65 vinylbenzene (polymerization-grade) 15
Soft monomer is selected butyl acrylate (polymerization-grade) for use, and function monomer is selected vinylformic acid (polymerization-grade) for use, and the dispersion stabilizer in the auxiliary agent is for selecting polyvinylpyrrolidone alcohol for use, and initiator is selected benzoyl peroxide for use, and surface treatment agent is a silane coupling agent.
The preparation method is:
A, take by weighing methyl methacrylate, vinylbenzene, butyl acrylate, vinylformic acid, add initiator, the dissolving back adds through surface-treated inorganic nano-particle and color stuffing, makes with ultrasonic dispersing that to give dispersion liquid stand-by in 30 minutes;
B, 250 ml waters, 50 gram ethanol and 10 gram polyvinylpyrrolidones are added have in 500 milliliters the reactor of stirring, heating, stir and make dissolving stand-by.
C, will give dispersion liquid and initiator and add solvent polyvinylpyrrolidone alcohol solution, use ultrasonic dispersing again 20 minutes, and start and be heated with stirring to 75 ℃, constant temperature reaction 4 hours down; Then reacted 2 hours down at 80 ℃, cooling, discharging, centrifuge dehydration, oven dry promptly get product again.
Properties of sample:
[1] outward appearance: white powder;
[2] particle diameter: 5～15 μ m;
[3] particle shape: regular ball-type.
Claims (9)
1, nano composite powder coatings is characterized in that it comprises the component of following unit mass part:
Water 100～150 pure 20-80 mix monomer 50～100 inorganic nano-particle 5-20
Color stuffing 5-40 dispersion stabilizer 5-30 initiator 0.5-5 surface-modifying agent 1～10
Wherein mix monomer is the mixed thing of hard monomer, soft monomer and function monomer.
2, nano composite powder coatings according to claim 1 is characterized in that each composition weight proportioning is in the described mix monomer:
Hard monomer 60～90, soft monomer 20～50, function monomer 2～10
Wherein hard monomer is selected from one or more the mixture in methyl methacrylate, methyl acrylate, vinylbenzene, vinyl toluene, vinyl acetate between to for plastic, acrylonitrile, the methacrylic eyeball; Soft monomer is selected from one or more the mixture in ethyl propenoate, butyl acrylate, Ethyl acrylate, Octyl acrylate, Isooctyl acrylate monomer, the 2-EHA; Function monomer is selected from one or more the mixture in vinylformic acid, methacrylic acid, propenoic acid beta-hydroxy ethyl ester, propenoic acid beta-hydroxy propyl ester, Jia Jibingxisuanβ-Qiang Yizhi, methacrylic acid β-hydroxypropyl acrylate, N hydroxymethyl acrylamide, the N-methoxymethyl acrylamide.
3, nano composite powder coatings according to claim 1 is characterized in that described inorganic nano-particle is one or more mixtures in nano titanium oxide, nano zine oxide, nano silicon, nano-sized iron oxide, nano calcium oxide, nano-calcium carbonate, the nano alumina particles.
4. nano composite powder coatings according to claim 1 is characterized in that described alcohol is selected from more than one mixture of a kind of in the short chain alcohol or its.
5, nano composite powder coatings according to claim 1, it is characterized in that described color stuffing particle diameter is below 1 micron, comprise tinting pigment and pigment extender, tinting pigment is selected from one or more the mixture in titanium dioxide, zinc sulfide white, iron oxide red, iron oxide yellow, ultramarine, the chrome green, pigment extender is selected from one or more the mixture in lime carbonate, china clay, talcum powder, ground barium sulfate, the superfine alumina silicate, and tinting pigment and pigment extender are oleophylic water repellency pigment after treatment.
6, nano composite powder coatings according to claim 1, it is characterized in that described dispersion stabilizer is selected from one or more the mixture in hydroxy propyl cellulose, polyethylene pyrrolidone, the polymethyl acrylic acid, initiator is selected from that azo two isobutyls are fine, two different heptan of benzoyl peroxide, lauroyl peroxide, di-isopropyl peroxydicarbonate, di-cyclohexylperoxy dicarbonate, azo one or more the mixture in fine.
7, nano composite powder coatings according to claim 1, it is characterized in that wherein also having surface treatment agent, surface treatment agent is selected from one or more the mixture in stearic acid, trieline base silane, triethoxyl silane, titanate ester, the aluminium esters of gallic acid coupling agent.
8, according to the dispersion polymerization manufacturing process of the described nano composite powder coatings of claim 1-7, it is characterized in that comprising following processing step:
A, earlier inorganic nano-particle and color stuffing are carried out surface treatment, again in the inorganic nano-particle that will handle and the color stuffing adding mix monomer,, make that to give dispersion liquid stand-by by ultrasonic dispersing 30 minutes;
B, dispersion stabilizer, water and pure mixed solvent are added reaction flask according to the order of sequence, add prepare in the A step give dispersion liquid and initiator, ultra-sonic dispersion 20 minutes, start stirring heating, 75 ℃ of reactions 2.5～4.5 hours, be warming up to 80 ℃ of afterreactions 2～3 hours, cooling, discharging, centrifugal, oven dry promptly get product.
9,, it is characterized in that described surface treatment is to adopt surface treatment agent that inorganic nano-particle and color stuffing surface are handled according to the dispersion polymerization manufacturing process of claim 7 or 8 described nano composite powder coatings.
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| CN102532969A (en) * | 2010-12-30 | 2012-07-04 | 江苏考普乐新材料股份有限公司 | Preparation method of powder coating |
| CN102532969B (en) * | 2010-12-30 | 2014-02-26 | 江苏考普乐新材料有限公司 | Preparation method of powder coating |
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| JP2017518402A (en) * | 2014-04-30 | 2017-07-06 | アクゾ ノーベル コーティングス インターナショナル ビー ヴィ | Method for preparing acrylic powder coating resin system |
| CN104448994A (en) * | 2014-12-09 | 2015-03-25 | 苏州明轩地坪涂料有限公司 | Antibacterial and anti-mildew coating |
| CN104877510A (en) * | 2015-05-20 | 2015-09-02 | 苏州市贝克生物科技有限公司 | Anticorrosion antibacterial paint and preparation method thereof |
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| CN107151468B (en) * | 2016-03-04 | 2020-05-15 | 中国石油化工股份有限公司 | Acrylic resin powder composition, coating and application |
| CN106543794A (en) * | 2016-05-06 | 2017-03-29 | 刘秋雷 | A kind of multifunctional nano composite coating |
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| CN108707355A (en) * | 2017-10-17 | 2018-10-26 | 吴小再 | A kind of anticorrosive paint |
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| CN108587281A (en) * | 2018-03-30 | 2018-09-28 | 盐城科迈特新材料有限公司 | A kind of powdery paints heat-proof aging modifying agent and preparation method thereof |
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