CN1400265A - Solvent type organic silicone modified acrylate coating material and its production method - Google Patents
Solvent type organic silicone modified acrylate coating material and its production method Download PDFInfo
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- CN1400265A CN1400265A CN 01127683 CN01127683A CN1400265A CN 1400265 A CN1400265 A CN 1400265A CN 01127683 CN01127683 CN 01127683 CN 01127683 A CN01127683 A CN 01127683A CN 1400265 A CN1400265 A CN 1400265A
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Abstract
The solvent type organic silicon modified acrylate paint for wall surface of high-rise building, bridge, road guard and fence is characterized by that in the acid medium the metasilicate is hydrolyzed and polycondensed into organic silicon oligomer, then the organic silicon oligomer, acrylate monomer and organic silicon monomer containing unsaturated double bond are copolymerized to obtain the organic silicon modified acrylic resin, and said organic silicon modified acrylic resin is mixed with pigment filling material so as to obtain the invented product. Said invented acrylic resin paint has high adhesive force, good water-proofing property, contamination resistance, washing resistance, heat-resisting property and ageing resistance.
Description
The present invention relates to a kind of solvent type organic silicone modified acrylate coating material and production method thereof.
Acrylic resin has 30% to be used to prepare coating approximately, although its film have the transparency good, good mechanical property, anti-freezing, weather-proof and difficult jaundice under uviolizing, but the hardness of filming is on the low side, poor heat resistance, easily be clamminess after being heated (high temperature after-tacks), not only easily be stained with dust and moisture etc., but also can reduce its other performance.For this reason, there are many reports to mention the method for using organosilicon-modified acrylic coating in the literature.For example JP89-60618 makes the silicon intermediate with octamethylcyclotetrasiloxane and methyl ethylene cyclosiloxane, produces the organosilicon-modified acrylate resin with the method for acrylate monomer copolymerization again.JP95-196975 makes organosilicon-modified acrylate resin with the acrylate monomer copolymerization with 3-methacrylic acid group Trimethoxy silane in solvent.Above-mentioned organic-silicon-modified acrylate resin, common characteristic is to have introduced organosilicon functional group on its macromolecular main chain and the side chain, the bond energy that utilizes the Si-O covalent linkage is than the high 25Kcal/mol of C-C bond energy, improves acrylic resin greatly to heat, to the stability of light.By its coatings formulated, characteristics such as filming has the sticking power height, and contamination resistance is water-fast, and is heat-resisting and ageing-resistant.But silicon intermediate manufacturing technique requirent is tight, and gelatin phenomenon easily takes place the organosilicon-modified acrylate resin package stability instability that the silicon monomer that direct use contains unsaturated double-bond synthesizes.
The present invention is directed to above-mentioned two types and produce the weak point that the organosilicon-modified acrylate resin exists, adopt organosilicon oligopolymer and the silicon monomer bonded method that contains unsaturated double-bond to produce the organosilicon-modified acrylate resin.Purpose provides a kind of high adhesive force that has, and hard films, water tolerance, contamination resistance, abrasion resistance, solvent based coating that thermotolerance and ageing-resistant performance are good and production method thereof.
For achieving the above object, coating of the present invention is made up of organosilicon-modified acrylate resin and color stuffing etc., it is characterized in that the scope of the composition of its constituent is: organosilicon-modified acrylate resin 40～50% (weight); Color stuffing 20～25% (weight); Dispersion agent 0.5～1% (weight); Flow agent 0.5～1% (weight); Defoamer 0.5～1% (weight); UV light absorber 0.5～1% (weight); Solvent 15～30% (weight), the summation of each component are 100% (weight).
Color stuffing in the said components, dispersion agent, flow agent, defoamer, UV light absorber and solvent are commercially available product.
The production method of coating of the present invention is characterized in that may further comprise the steps:
(a) positive silicon ester being dissolved in the alcohol, is under 50～100 ℃ of conditions with diluted acid in temperature again, hydrolysis 1～3 hour; In temperature is 120～170 ℃, and polycondensation is 2～4 hours under the vacuum condition, makes the organosilicon oligopolymer;
(b) with the organosilicon oligopolymer, acrylate monomer with contain the dissolving of the organosilane monomer of unsaturated double-bond and initiator after, be added to temperature and be in 120～150 ℃ the solvent polyase 13～6 hour, make the organosilicon-modified acrylate resin;
(c) with the organosilicon-modified acrylate resin, color stuffing, dispersion agent, flow agent, defoamer, UV light absorber and solvent are made into coating.
Above-mentioned production method, the positive silicon ester of its use can be methyl silicate, tetraethoxy or positive silicic acid propyl ester; Used alcohol can be methyl alcohol, ethanol or n-propyl alcohol; Used diluted acid is a dilute hydrochloric acid; Used acrylate monomer can be methyl methacrylate, methyl acrylate, ethyl propenoate, propyl acrylate or butyl acrylate; The used organosilane monomer that contains unsaturated double-bond can be vinyltrimethoxy silane, vinyltriethoxysilane or 3-methacryloxy Trimethoxy silane; Used initiator can be benzoyl peroxide or azo isobutyronitrile.
Coating of the present invention is by the organosilicon oligopolymer, acrylate monomer and contain organosilicon-modified acrylate resin that the silicon monomer copolymerization of unsaturated double-bond forms and color stuffing etc. formulated.Therefore this coating has high sticking power, outstanding contamination resistance, abrasion resistance, water tolerance, thermotolerance and ageing resistance.
The present invention is further illustrated below in conjunction with embodiment:
(1) preparation organosilicon oligopolymer
Having reflux exchanger, in the there-necked flask of thermometer and stirring, adding after tetraethoxy 104 grams and ethanol 35 grams mix, adding 0.05% hydrochloric acid, 7.5 grams again, be warmed up to 50～100 ℃ and be hydrolyzed and reacted 1-3 hour.Temperature is raised to 120-170 ℃ subsequently, takes ethanol away under vacuum, condensation reaction 2～4 hours obtains the organosilicon oligopolymer.
(2) preparation organosilicon-modified acrylate resin
Having Dropping feeder, stir, in the four-hole boiling flask of reflux exchanger and thermometer, add dimethylbenzene and N-BUTYL ACETATE mixed solvent (3: 1 proportionings) 100 grams, be warmed up to 120～150 ℃, drip mixed solution down: methyl methacrylate 75 grams, butyl acrylate 13 grams, 3-methacryloxy Trimethoxy silane 7 grams, organosilicon oligopolymer 5 grams and benzoyl peroxide 0.7 gram.After the polyreaction 5 hours, be cooled to 50 ℃ with bottom discharge.
(3) preparation Silicone Modified Acrylate Resin Coating
With organosilicon-modified acrylate resin (solids content is 50%) 50 grams, titanium dioxide 20 grams, dimethylbenzene 21 grams, N-BUTYL ACETATE 7 grams, dispersion agent 0.5 gram, defoamer 0.5 gram, UV light absorber 1 gram, after blending dispersion was even, being ground to fineness at sand mill was 45≤μ m, obtains whitewash.
Claims (10)
1. a solvent type organic silicone modified acrylate coating material is made up of organosilicon-modified acrylate resin and color stuffing etc., the invention is characterized in that the scope of these compositions is: organosilicon-modified acrylate resin 40～50% (weight); Color stuffing 20～25% (weight); Dispersion agent 0.5～1% (weight); Flow agent 0.5～1% (weight); Defoamer 0.5～1% (weight); UV light absorber 0.5～1% (weight); Solvent 15～30% (weight), the summation of each component are 100% (weight).
2. organic silicone modified acrylate coating material according to claim 1 is characterized in that used solvent is commercially available solvent.
3. organic silicone modified acrylate coating material according to claim 1 is characterized in that used dispersion agent, flow agent, and defoamer and UV light absorber are commercially available dispersion agent, flow agent, defoamer and UV light absorber.
4. the production method of a solvent type organic silicone modified acrylate coating material is characterized in that production method may further comprise the steps:
(a) positive silicon ester being dissolved in the alcohol, is under the 50-100 ℃ of condition hydrolysis 1-3 hour with diluted acid in temperature again; In temperature is 120-170 ℃, under the vacuum condition polycondensation 2-4 hour, makes the organosilicon oligopolymer.
(b) with the organosilicon oligopolymer, acrylate monomer with contain the dissolving of the organosilane monomer of unsaturated double-bond and initiator after, be 120-150 ℃ in temperature and be added in the solvent that polyase 13-6 hour makes the organosilicon-modified acrylate resin.
(c) with this resin, color stuffing, dispersion agent, flow agent, defoamer, UV light absorber and solvent are made into coating.
5. production method according to claim 4 is characterized in that used positive silicon ester is a methyl silicate, tetraethoxy or positive silicic acid propyl ester.
6. production method according to claim 4 is characterized in that used alcohol is methyl alcohol, ethanol or n-propyl alcohol.
7. production method according to claim 4 is characterized in that used diluted acid is a dilute hydrochloric acid.
8. production method according to claim 4 is characterized in that used acrylate monomer is methyl methacrylate, methyl acrylate, ethyl propenoate, propyl acrylate or butyl acrylate.
9. production method according to claim 4 is characterized in that the used organosilane monomer that contains unsaturated double-bond is a vinyltrimethoxy silane, vinyltriethoxysilane or 3-methacryloxy Trimethoxy silane.
10. production method according to claim 4 is characterized in that used initiator is benzoyl peroxide or azo isobutyronitrile.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011276835A CN1174059C (en) | 2001-08-01 | 2001-08-01 | Solvent type organic silicone modified acrylate coating material and its production method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011276835A CN1174059C (en) | 2001-08-01 | 2001-08-01 | Solvent type organic silicone modified acrylate coating material and its production method |
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| CN1400265A true CN1400265A (en) | 2003-03-05 |
| CN1174059C CN1174059C (en) | 2004-11-03 |
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| CNB011276835A Expired - Fee Related CN1174059C (en) | 2001-08-01 | 2001-08-01 | Solvent type organic silicone modified acrylate coating material and its production method |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059313A (en) * | 2012-12-17 | 2013-04-24 | 中山大桥化工集团有限公司 | Method for preparing organosilicon modified acrylic resin |
| CN102746467B (en) * | 2008-04-22 | 2015-01-14 | 东亚合成株式会社 | Curable composition and process for production of organosilicon compound |
| CN104540905A (en) * | 2012-03-22 | 2015-04-22 | 3M创新有限公司 | Polymethylmethacrylate based hardcoat composition and coated article |
| CN105237693A (en) * | 2015-11-05 | 2016-01-13 | 浩力森涂料（上海）有限公司 | Organic-inorganic hybrid silica modified acrylic resin and coating thereof |
| CN106280626A (en) * | 2016-08-12 | 2017-01-04 | 太仓市美航涂料有限公司 | A kind of environment-friendly type high adhesion force waterborne glass coatings |
| CN107207897A (en) * | 2014-12-02 | 2017-09-26 | 巴斯夫涂料有限公司 | Copolymer and the coloured coating agent comprising copolymer |
| CN109505198A (en) * | 2018-12-20 | 2019-03-22 | 广东玉兰集团股份有限公司 | A kind of transparent slurry, wallpaper and preparation method thereof |
| CN109593420A (en) * | 2018-11-19 | 2019-04-09 | 深圳市烯世传奇科技有限公司 | Organosilicon modified crylic acid resin antifouling paint and preparation method thereof |
| CN109868026A (en) * | 2019-02-20 | 2019-06-11 | 中南大学 | A kind of Silicone-Modified Acrylate Resin and preparation method thereof and the hydrophobic weather-proof acrylic resin modified coating of sustained release |
| CN110093130A (en) * | 2018-01-31 | 2019-08-06 | 上海宝银电子材料有限公司 | A kind of electromagnetic shielding conductive silver glue and preparation method thereof |
| CN110332238A (en) * | 2019-07-11 | 2019-10-15 | 淄博恒星轴承有限公司 | A kind of electrical isolation high temperature resistant mixing ball bearing and preparation method thereof |
| CN110396341A (en) * | 2019-08-29 | 2019-11-01 | 华南理工大学 | A kind of super-hydrophobic dirt resistance coatings and preparation method thereof based on 3D microballoon |
| CN113480907A (en) * | 2021-07-01 | 2021-10-08 | 江西东维电气有限公司 | Preparation method of spherical stain-resistant pin insulator |
-
2001
- 2001-08-01 CN CNB011276835A patent/CN1174059C/en not_active Expired - Fee Related
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746467B (en) * | 2008-04-22 | 2015-01-14 | 东亚合成株式会社 | Curable composition and process for production of organosilicon compound |
| CN104540905A (en) * | 2012-03-22 | 2015-04-22 | 3M创新有限公司 | Polymethylmethacrylate based hardcoat composition and coated article |
| CN104540905B (en) * | 2012-03-22 | 2017-12-19 | 3M创新有限公司 | Hard coat film composition and coating product based on polymethyl methacrylate |
| US10072173B2 (en) | 2012-03-22 | 2018-09-11 | 3M Innovative Properties Company | Polymethylmethacrylate based hardcoat composition and coated article |
| CN103059313A (en) * | 2012-12-17 | 2013-04-24 | 中山大桥化工集团有限公司 | Method for preparing organosilicon modified acrylic resin |
| CN107207897A (en) * | 2014-12-02 | 2017-09-26 | 巴斯夫涂料有限公司 | Copolymer and the coloured coating agent comprising copolymer |
| CN107207897B (en) * | 2014-12-02 | 2021-02-26 | 巴斯夫涂料有限公司 | Copolymer and colored coating agent comprising copolymer |
| CN105237693A (en) * | 2015-11-05 | 2016-01-13 | 浩力森涂料（上海）有限公司 | Organic-inorganic hybrid silica modified acrylic resin and coating thereof |
| CN106280626A (en) * | 2016-08-12 | 2017-01-04 | 太仓市美航涂料有限公司 | A kind of environment-friendly type high adhesion force waterborne glass coatings |
| CN110093130A (en) * | 2018-01-31 | 2019-08-06 | 上海宝银电子材料有限公司 | A kind of electromagnetic shielding conductive silver glue and preparation method thereof |
| CN109593420A (en) * | 2018-11-19 | 2019-04-09 | 深圳市烯世传奇科技有限公司 | Organosilicon modified crylic acid resin antifouling paint and preparation method thereof |
| CN109505198A (en) * | 2018-12-20 | 2019-03-22 | 广东玉兰集团股份有限公司 | A kind of transparent slurry, wallpaper and preparation method thereof |
| CN109868026B (en) * | 2019-02-20 | 2020-06-16 | 中南大学 | Organic silicon modified acrylate resin, preparation method thereof and hydrophobic weather-resistant slow-release modified acrylic resin coating |
| CN109868026A (en) * | 2019-02-20 | 2019-06-11 | 中南大学 | A kind of Silicone-Modified Acrylate Resin and preparation method thereof and the hydrophobic weather-proof acrylic resin modified coating of sustained release |
| CN110332238A (en) * | 2019-07-11 | 2019-10-15 | 淄博恒星轴承有限公司 | A kind of electrical isolation high temperature resistant mixing ball bearing and preparation method thereof |
| CN110396341A (en) * | 2019-08-29 | 2019-11-01 | 华南理工大学 | A kind of super-hydrophobic dirt resistance coatings and preparation method thereof based on 3D microballoon |
| CN113480907A (en) * | 2021-07-01 | 2021-10-08 | 江西东维电气有限公司 | Preparation method of spherical stain-resistant pin insulator |
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| Publication number | Publication date |
|---|---|
| CN1174059C (en) | 2004-11-03 |
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