CN104231902A - Preparation method for light resistance polyurethane coating - Google Patents
Preparation method for light resistance polyurethane coating Download PDFInfo
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- CN104231902A CN104231902A CN201410559491.3A CN201410559491A CN104231902A CN 104231902 A CN104231902 A CN 104231902A CN 201410559491 A CN201410559491 A CN 201410559491A CN 104231902 A CN104231902 A CN 104231902A
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Abstract
The invention relates to a preparation method for light resistance polyurethane coating. The nano cerium oxide is modified through the phosphate for preparing the modified nano cerium oxide; the modified nano cerium oxide is used for preparing the polyurethane coating. The prepared polyurethane coating has excellent light resistance, and the heat-resistant quality of the coating is improved for the addition of the nano cerium oxide.
Description
Technical field
The present invention relates to a kind of preparation method of polyurethane coating, particularly a kind of preparation method of sunproof polyurethane coating.
Background technology
Polyurethane coating is widely used in the fields such as woodwork coating, automobile repairing paint, protective system, building coating, floor paint, electronic paint, speciality coating, waterproof paint.But because use field often contacts sunlight, containing UV-light harmful to light object in a large number in solar ray, its wavelength 290 ~ 460nm, these UV-light, by redoxomorphism chemically, make material surface generation colour-change, affect appearance.
The method preparing sunproof polyurethane coating be at present by urethane and nano material as composite in nano titanium oxide, nano zine oxide, carbon nanotube etc., but due to nano material emulsion intercalation method poor, the standby urethane stability in storage of this legal system is poor.Also have research to adopt modification by coupling to nano oxidized cerium modified, be applied to polyurethane coating, but operation is various, cost is high.
Summary of the invention
Present invention employs following technical scheme.
1. a preparation method for sunproof polyurethane coating, is characterized in that, described method phosphoric acid ester carries out modification to nano-cerium oxide, prepares modified nano cerium oxide; Recycling modified nano cerium oxide prepares polyurethane coating.The step of described method is:
(1) modified nano cerium oxide is prepared:
(1.1) according to weight percent, the mixture of modified nano cerium oxide is composed as follows:
Nano-cerium oxide 15 ~ 20%;
Dispersion agent 79.7 ~ 83.5%;
Phosphoesterase 30 .3 ~ 1.5%;
(1.2) nano-cerium oxide is added in dispersion agent, dispersed with stirring 10 ~ 30min under 600 ~ 1000rpm rotating speed;
(1.3) phosphonate oligomers slowly added in the nano-cerium oxide solution after dispersion, stirred at ambient temperature is even, obtains modified nano cerium oxide;
(2) nano-cerium oxide polyurethane coating is prepared:
(2.1) prepare component first, according to weight percent meter, component first comprises following component and content:
Solvent 0 ~ 75%;
Solidifying agent 25 ~ 100%;
Film coalescence aid 0 ~ 10%
With solvent, solidifying agent is diluted to 80%, film coalescence aid is joined in above-mentioned solution, under 600 ~ 1000 rotating speeds, disperse 10min, obtained component first;
(2.2) prepare component second, according to weight percent, component second comprises the content of following component:
Modified nano cerium oxide 1 ~ 10%;
Polyhydroxy resin 80 ~ 95%;
Auxiliary agent 5 ~ 10%;
The modified nano cerium oxide solution first step (1) prepared, Hydroxylated acrylic resin mix, put into coating dispersion machine, under 2000rpm rotating speed, lower dispersion 1h is to realize Homogeneous phase mixing, use liquid spheres grinding machine ball milling 0.5h again, auxiliary agent is added in said mixture, under 2000rpm rotating speed, disperse 20min, obtain component second;
(2.3) when using by component first and component second in proportion NCO:OH=1.2:1 mix, be namely prepared into phosphate modified nano-cerium oxide/polyurethane Composite Coating.
2. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, its particle diameter of described nano-cerium oxide is 10 ~ 100nm.
3. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, described dispersion agent is acetone, methylethylketone, vinyl acetic monomer, N-BUTYL ACETATE, toluene, dimethylbenzene, one or more mixtures mixed in any proportion of vinylbenzene.
4. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, described phosphoric acid ester is the one of alkyl polyoxyethylene ether phosphate ester salt and alkyl phosphate salt.
5. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, in described component first, solidifying agent is isocyanates curing agent toluene vulcabond, 1, the one of hexamethylene-diisocyanate, xylylene diisocyanate, solvent is 3-ethoxyl ethyl propionate; Film coalescence aid is propandiol butyl ether, 1-Methoxy-2-propyl acetate, dme one wherein.
6. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, in described component second, polyhydroxy resin is the one in Hydroxylated acrylic resin, organic hydroxy silicate resin, epoxy resin.
7. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, the auxiliary agent micronized silica in described component second, acetate butyrate fiber.
The present invention has following characteristics:
(1), prepared polyurethane coating except there is excellent photostabilization because the interpolation of nano-cerium oxide, the resistance toheat of coating is also improved;
(2), the film forming speed of polyurethane coating is accelerated in the interpolation of phosphoric acid ester;
(3), adopt dispersion agent to disperse nano-cerium oxide, because of this dispersion agent this as the solvent prepared polyurethane coating needs and use, modified nano-cerium oxide, without the need to washing, the operation such as dry, has saved operation, solvent, saving cost.Whole process is without the need to heating, and modified solution can directly be applied, and does not need post-treatment, saves fuel, solvent and operation;
(4), adopt 3-ethoxyl ethyl propionate to replace traditional urethane and synthesize the DMF solvent used, more environmental protection.
Embodiment further illustrates the present invention below in conjunction with example.
Embodiment one:
Be that the nano-cerium oxide of 10nm is added in 8.35ml vinylbenzene by 1.5g particle diameter, dispersed with stirring 10min under 600rpm rotating speed; Slowly added in the nano-cerium oxide solution after dispersion by 0.15g alkyl polyoxyethylene ether phosphate ester salt, stirred at ambient temperature is even;
The tolylene diisocyanate of 1.0g is added in the 3-ethoxyl ethyl propionate of 9.0ml, under 600rpm rotating speed, disperse 10min, obtained component first;
Get the modified nano cerium oxide solution and the mixing of 8.0g Hydroxylated acrylic resin that are equivalent to containing nano-cerium oxide 1.0g, put into coating dispersion machine, 1h is disperseed under under 2000rpm rotating speed, use liquid spheres grinding machine ball milling 0.5h again, by 0.85g micronized silica, acetate butyrate fiber: toluene is that the solution of 0.15g:1.5ml adds in said mixture, under 2000rpm rotating speed, disperse 20min, obtain component second;
During use, component first is mixed by 1.5:1 with component second, be namely prepared into phosphate modified nano-cerium oxide/polyurethane Composite Coating.
Embodiment two:
Be that the nano-cerium oxide of 100nm is added in 7.97ml vinyl acetic monomer by 2.0g particle diameter, dispersed with stirring 30min under 1000rpm rotating speed; Slowly added by 0.03g alkyl phosphate salt in the nano-cerium oxide solution after dispersion, stirred at ambient temperature is even;
The hexamethylene diisocyanate of 3.0g is added in the 3-ethoxyl ethyl propionate of 6.0ml, then 1ml propandiol butyl ether is added in above-mentioned solution, under 1000rpm rotating speed, disperse 30min, obtained component first;
Get the modified nano cerium oxide solution and 8.0g organic hydroxy silicate mixed with resin that are equivalent to containing nano-cerium oxide 1.0g, put into coating dispersion machine, 1h is disperseed under under 2000rpm rotating speed, use liquid spheres grinding machine ball milling 0.5h again, by 0.85g micronized silica, acetate butyrate fiber: toluene is that the solution of 0.15g:1.5ml adds in said mixture, under 2000rpm rotating speed, disperse 20min, obtain component second;
During use, component first is mixed by 0.48:1 with component second, be namely prepared into phosphate modified nano-cerium oxide/polyurethane Composite Coating.
Embodiment three:
Be that the nano-cerium oxide of 100nm is added in 7.97ml vinyl acetic monomer by 2.0g particle diameter, dispersed with stirring 30min under 1000rpm rotating speed; Slowly added by 0.03g alkyl phosphate salt in the nano-cerium oxide solution after dispersion, stirred at ambient temperature is even;
The xylylene diisocyanate of 5.0g is added in the 3-ethoxyl ethyl propionate of 5.0ml, under 1000rpm rotating speed, disperse 30min, obtained component first;
Get the modified nano cerium oxide solution and the mixing of 9.5g epoxy resin that are equivalent to containing nano-cerium oxide 0.1g, put into coating dispersion machine, 1h is disperseed under under 2000rpm rotating speed, use liquid spheres grinding machine ball milling 0.5h again, by 0.3g micronized silica, acetate butyrate fiber: toluene is that the solution of 0.1g:1.0ml adds in said mixture, under 2000rpm rotating speed, disperse 20min, obtain component second;
During use, component first is mixed by 1:2 with component second, be namely prepared into phosphate modified nano-cerium oxide/polyurethane Composite Coating.
In order to the light fastness of quantitative description urethane, adopt spectrophotometer to detect, to obtain inverse difference △ E, describe the photostabilization of urethane.△ E represents colour-change degree, and △ E is larger, and color change is more obvious.In general, △ E value is the slight change of 0 ~ 1.5 genus; △ E value is that 1.5 ~ 3.0 genus can feel change; △ E value be 3.0 ~ 6.0 belong to considerable changes (see Wang Fang, party's climax, Wang Liqin, the photodegradation [J] of several organic historical relic's protection polymer coating. Northwest University's journal, 2005,35 (5): 56 ~ 58).
The resistance toheat of polyurethane coating adopts thermogravimetry to measure, and decomposition temperature is higher, proves that its thermotolerance is better.Thermogravimetry is shown in (Jia Mengqiu, Bai Hongying, Wang Jinling, the research [J] of epoxy organosilicon anticorrosive coating thermotolerance. material protection, 2003,36 (4): 54 ~ 56).
Film forming speed characterizes with film surface drying time, and film surface drying time is shorter, and film forming is faster.The mensuration of film surface drying time is with reference to GB/T 1728-1979 (1989) standard.
Embodiment one is designated as A, B, C respectively to the sunproof polyurethane of embodiment three gained, selects the sunproof polyurethane PODESENG 513MS on market to contrast with it.
Under the table one different UV-irradiation time, the value of chromatism △ E of polyurethane film changes
| Time/min | PODESENG 513MS | A | B | C |
| 90 | 0.7 | 0.3 | 0.2 | 0.7 |
| 150 | 0.9 | 0.4 | 0.3 | 0.9 |
| 270 | 1 | 0.5 | 0.4 | 0.9 |
| 330 | 1.1 | 0.5 | 0.5 | 1.1 |
| 390 | 1.3 | 0.7 | 0.6 | 1.1 |
| 450 | 1.5 | 0.7 | 0.7 | 1.3 |
| 510 | 1.8 | 0.9 | 0.9 | 1.5 |
| 540 | 2.1 | 1.1 | 1.1 | 1.7 |
| 600 | 2.3 | 1.3 | 1.2 | 1.8 |
Can find from table one, embodiment one all in slight variation range, show good photostabilization, and the sunproof polyurethane on market is at more than 510min, has belonged to and can feel change to 3 kinds of urethane photostabilization prepared by embodiment three.
The decomposition temperature of table two polyurethane coating
| PODESENG 513MS | A | B | C | |
| Decomposition temperature/DEG C | 302.14 | 332.51 | 339.64 | 317.52 |
Can find from table two, 3 kinds of urethane decomposition temperatures prepared by embodiment one to embodiment three all obtain larger lifting.
The surface drying time of table three polyurethane coating
| PODESENG 513MS | A | B | C | |
| Surface drying time/min | 82 | 69 | 67 | 76 |
Can find from table three, the surface drying time of 3 kinds of polyurethane coatings prepared by embodiment one to embodiment three is all less than the polyurethane coating on market.
Claims (7)
1. a preparation method for sunproof polyurethane coating, is characterized in that, described method phosphoric acid ester carries out modification to nano-cerium oxide, prepares modified nano cerium oxide; Recycling modified nano cerium oxide prepares polyurethane coating, and the step of described method is:
(1) modified nano cerium oxide is prepared:
(1.1) according to weight percent, the mixture of modified nano cerium oxide is composed as follows:
Nano-cerium oxide 15 ~ 20%;
Dispersion agent 79.7 ~ 83.5%;
Phosphoesterase 30 .3 ~ 1.5%;
(1.2) nano-cerium oxide is added in dispersion agent, dispersed with stirring 10 ~ 30min under 600 ~ 1000rpm rotating speed;
(1.3) phosphonate oligomers slowly added in the nano-cerium oxide solution after dispersion, stirred at ambient temperature is even, obtains modified nano cerium oxide;
(2) nano-cerium oxide polyurethane coating is prepared:
(2.1) prepare component first, according to weight percent meter, component first comprises following component and content:
Solvent 0 ~ 75%;
Solidifying agent 25 ~ 100%;
Film coalescence aid 0 ~ 10%
With solvent, solidifying agent is diluted to 80%, film coalescence aid is joined in above-mentioned solution, under 600 ~ 1000 rotating speeds, disperse 10min, obtained component first;
(2.2) prepare component second, according to weight percent, component second comprises the content of following component:
Modified nano cerium oxide 1 ~ 10%;
Polyhydroxy resin 80 ~ 95%;
Auxiliary agent 5 ~ 10%;
The modified nano cerium oxide solution first step (1) prepared, Hydroxylated acrylic resin mix, put into coating dispersion machine, under 2000rpm rotating speed, lower dispersion 1h is to realize Homogeneous phase mixing, use liquid spheres grinding machine ball milling 0.5h again, auxiliary agent is added in said mixture, under 2000rpm rotating speed, disperse 20min, obtain component second;
(2.3) when using by component first and component second in proportion NCO:OH=1.2:1 mix, be namely prepared into phosphate modified nano-cerium oxide/polyurethane Composite Coating.
2. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, its particle diameter of described nano-cerium oxide is 10 ~ 100nm.
3. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, described dispersion agent is acetone, methylethylketone, vinyl acetic monomer, N-BUTYL ACETATE, toluene, dimethylbenzene, one or more mixtures mixed in any proportion of vinylbenzene.
4. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, described phosphoric acid ester is the one of alkyl polyoxyethylene ether phosphate ester salt and alkyl phosphate salt.
5. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, in described component first, solidifying agent is isocyanates curing agent toluene vulcabond, 1, the one of hexamethylene-diisocyanate, xylylene diisocyanate, solvent is 3-ethoxyl ethyl propionate; Film coalescence aid is propandiol butyl ether, 1-Methoxy-2-propyl acetate, dme one wherein.
6. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, in described component second, polyhydroxy resin is the one in Hydroxylated acrylic resin, organic hydroxy silicate resin, epoxy resin.
7. according to the preparation method of a kind of sunproof polyurethane coating described in claim 1, it is characterized in that, the auxiliary agent micronized silica in described component second, acetate butyrate fiber.
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| CN201410559491.3A CN104231902A (en) | 2014-10-18 | 2014-10-18 | Preparation method for light resistance polyurethane coating |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106189770A (en) * | 2016-07-11 | 2016-12-07 | 赵艳丽 | A kind of high light wearable oil polish and preparation technology thereof |
| CN107603451A (en) * | 2017-10-10 | 2018-01-19 | 国网江苏省电力公司南通供电公司 | The preparation method of Nano titanium nitride modified polyurethane paint |
| CN113214637A (en) * | 2021-05-17 | 2021-08-06 | 福建师范大学泉港石化研究院 | Polyurethane with uvioresistant performance and preparation method thereof |
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| CN103589311A (en) * | 2013-10-16 | 2014-02-19 | 国家电网公司 | Preparation method of titanate-modified nano cerium oxide/polyurethane composite paint |
| CN103937308A (en) * | 2014-04-23 | 2014-07-23 | 苏州羽帆新材料科技有限公司 | Wear-resistant and heat-resistant machine coating and preparation method thereof |
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2014
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Patent Citations (4)
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| US20120225298A1 (en) * | 2007-07-16 | 2012-09-06 | University Of Kentucky | In-situ nanoparticle formation in polymer clear coats |
| CN103589311A (en) * | 2013-10-16 | 2014-02-19 | 国家电网公司 | Preparation method of titanate-modified nano cerium oxide/polyurethane composite paint |
| CN103937308A (en) * | 2014-04-23 | 2014-07-23 | 苏州羽帆新材料科技有限公司 | Wear-resistant and heat-resistant machine coating and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106189770A (en) * | 2016-07-11 | 2016-12-07 | 赵艳丽 | A kind of high light wearable oil polish and preparation technology thereof |
| CN107603451A (en) * | 2017-10-10 | 2018-01-19 | 国网江苏省电力公司南通供电公司 | The preparation method of Nano titanium nitride modified polyurethane paint |
| CN113214637A (en) * | 2021-05-17 | 2021-08-06 | 福建师范大学泉港石化研究院 | Polyurethane with uvioresistant performance and preparation method thereof |
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Application publication date: 20141224 |