CN101235245B - Method for preparing silicone-acrylate dope - Google Patents
Method for preparing silicone-acrylate dope Download PDFInfo
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- CN101235245B CN101235245B CN2008100706086A CN200810070608A CN101235245B CN 101235245 B CN101235245 B CN 101235245B CN 2008100706086 A CN2008100706086 A CN 2008100706086A CN 200810070608 A CN200810070608 A CN 200810070608A CN 101235245 B CN101235245 B CN 101235245B
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Abstract
A preparation process of silicon acrylic acid coating relates to a preparation process of coating, providing a preparation process of silicon acrylic acid coating which has high hardness and abrasion resistance, and can be used to on surface coating of plastic rubber and wood-ware. The preparation process comprises firstly adding toluene or isobutyl alcohol or the mixing solution of both into a reactor, and stirring and heating to reflux, secondly mixing acrylic esters monomer and acrylic ester monomer which comprises epoxy radical, then adding initiating agent whose weight is 0.1%-10% of the weight of monomer, stirring to dissolve and mix evenly, thirdly adding mixed monomer solution in the second step into the reactor in the way of one-time adding or dripping, keeping warm for 2-3h, and obtaining acrylic acid resin after stopping reaction, and fourthly mixing acrylic acid with curing agent, and evenly stirring to use.
Description
Technical field
The present invention relates to a kind of preparation method of coating, especially a kind of preparation method who is used for the novel high-energy silicon-acrylic coatings of plastic cement, woodenware.
Background technology
Because electronic industry fast development in recent years, and it is more and more higher to the demand of house fitting-up condition, the topcoating that requirement is used as these products has various more superior rerum naturas, and therefore developing the high-performance coating that meets social desirability is modern coating developing direction.The high-performance of coating comprises high-decoration, high preservative property, super weather resistance, multifunction and good performances such as application property.The electronic product sealer adopts esters of acrylic acid plastic cement lacquer basically at present, though its gloss is beautiful, fastness to rubbing is lower.Because wear resistance is not enough, top coat just is worn in the short period of time and fades, and until show-through, loses original color and luster and aesthetic feeling, also causes the product minimizing in work-ing life simultaneously; And the use of electronic product is generally at several years and even many decades, thus electronic product and most of be that the product of shell is badly in need of wearing face coating with the plastic cement.
Acrylic resin has high reaction activity and high, and therefore good stability to hydrolysis and light stability are a kind of protection of electronic product casing and coating types that woodenware beautifies of being widely used in.But esters of acrylic acid coating on its chemical constitution, can not have good wear resistance, can't satisfy the service requirements of high-wear resistance.Along with the development in market, the user is more and more higher to the requirement of product, and corresponding producer is also more and more stricter to the performance requriements of coating, therefore how to improve the important research direction that the plastic coating performance has become present coating material.
Summary of the invention
Purpose of the present invention is intended to provide a kind of have high rigidity and wear resisting property, can be used for the preparation method of the silicon-acrylic coatings of plastic cement, woodenware external coating.
The preparation method of described silicon-acrylic coatings is as follows:
1) toluene or isopropylcarbinol or the mixing solutions of the two are joined in the reactor, be heated with stirring to backflow;
2) acrylic ester monomer and the acrylate monomer that contains epoxide group are mixed, the initiator that adds monomer total mass 0.1%~10% then, stirring and dissolving, mix, by mass percentage, acrylic ester monomer: the acrylate monomer that contains epoxide group is (80%~99%): (1%~20%);
3) mixed monomer solution in the step 2 is added in the reactor in the mode of disposable adding or dropping, insulation 2~3h, stopped reaction gets acrylic resin;
4) acrylic resin is mixed with solidifying agent, stir, can use, by mass percentage, acrylic resin: solidifying agent is (5~25): 1.
Described acrylic ester monomer is at least a in vinylformic acid, methacrylic acid, butyl acrylate, methyl acrylate, methyl methacrylate, n-BMA, Propenoic acid, 2-methyl, isobutyl ester, 2-ethylhexyl methacrylic ester, methacrylic acid moon silicon ester, methacrylic acid benzyl ester, cyclohexyl methacrylate etc.
The described acrylate monomer that contains epoxide group is a glycidyl methacrylate, at least a in the methyl propenoic acid glycidyl ether etc.
Described initiator is preferably benzoyl peroxide etc.
Described solidifying agent is preferably quadrol, γ-An Bingjisanyiyangjiguiwan or diethylamine etc.
Rate of addition in the step 3) is preferably 0.5~1h/50g.
The mixing solutions of toluene and isopropylcarbinol can be arbitrary proportion.
The mixture of glycidyl methacrylate and methyl propenoic acid glycidyl ether can be arbitrary proportion.
The present invention is from functional group reactions mechanism, cut out by molecular designing and molecule, on original acrylate backbone, increased an active functional group-epoxide group, and and be with the combination of amino class solidifying agent, design a kind of bi-component acrylic ester coating, it is good that it has the acrylate resin weather resistance, cohesiveness is good, advantages such as good decorative property, product is after spraying, will be by epoxy and the amino chemical crosslink reaction that takes place, wear resisting property is considerably beyond the esters of acrylic acid coating of the single component of same molecular amount, simultaneously in alcohol resistance, coating fundamental property aspects such as hardness all are greatly improved.And preparation technology is simple, can on original coating apparatus basis, produce, and be a kind of at higher coating varieties of professional price ratio such as plastic cement, woodenware.
Embodiment
Following examples will the present invention is further illustrated.
Embodiment 1
In four-hole boiling flask, add 100ml toluene heated and stirred to refluxing; Take by weighing 75g methyl methacrylate, 20g n-BMA, 5g glycidyl methacrylate and be made into mix monomer, the benzoyl peroxide that adds 1g again, stirring and dissolving mixes, speed by the every 50g of 0.5h/ is added dropwise in the four-hole boiling flask, and 1h drips off; Drip off the back and be incubated 2h under reflux state, stopped reaction gets acrylic resin.During use by curing agent ethylene diamine: resin is to mix at 1: 25, stirs, and towards rare, can spray.Film behind baking 12h under 60 ℃, testing its wear resisting property of filming is 50, improves 5 times than the acrylate paint before the modification.
Embodiment 2
In four-hole boiling flask, add the isopropylcarbinol of 100g, heated and stirred is to refluxing; Take by weighing 90g n-BMA, 5g glycidyl methacrylate, 5g methyl propenoic acid glycidyl ether again and be made into mix monomer, the benzoyl peroxide that adds 0.1g again, stirring and dissolving mixes, speed by the every 50g of 1h/ is added dropwise in the four-hole boiling flask, and 2h drips off; Drip off the back and be incubated 3h under reflux state, stopped reaction gets acrylic resin.During use by curing agent ethylene diamine: resin is to mix at 1: 5, stirs, and towards rare, can spray.The wear resisting property of filming sees Table 1.
Embodiment 3
In four-hole boiling flask, add the isopropylcarbinol of 100g, heated and stirred is to refluxing; Take by weighing 90g n-BMA, 5g glycidyl methacrylate, 5g methyl propenoic acid glycidyl ether again and be made into mix monomer, add the benzoyl peroxide of 10g again, stirring and dissolving mixes, in the disposable adding four-hole boiling flask; Drip off the back and be incubated 3h under reflux state, stopped reaction gets acrylic resin.During use by curing agent ethylene diamine: resin is to mix at 1: 5, stirs, and towards rare, can spray.The wear resisting property of filming sees Table 1.
Embodiment 4
In four-hole boiling flask, add the toluene of 50g, the isopropylcarbinol of 50g, heated and stirred is to refluxing; Take by weighing 30g n-BMA, 40g Propenoic acid, 2-methyl, isobutyl ester, 15g2-ethylhexyl methacrylic ester, 7g glycidyl methacrylate, 8g methyl propenoic acid glycidyl ether again and be made into mix monomer, the benzoyl peroxide that adds 5g again, stirring and dissolving, mix, be added dropwise in the four-hole boiling flask, 1h drips off; Drip off the back and be incubated 2.5h under reflux state, stopped reaction gets acrylic resin.During use by the solidifying agent γ-An Bingjisanyiyangjiguiwan: resin is to mix at 1: 5, stirs, and towards rare, can spray.The wear resisting property of filming sees Table 1.
Embodiment 5
In four-hole boiling flask, add the toluene of 75g, the isopropylcarbinol of 25g, heated and stirred is to refluxing; Take by weighing 84g methyl methacrylate, 15g methacrylic acid moon silicon ester, 1g methyl propenoic acid glycidyl ether again and be made into mix monomer, add the benzoyl peroxide of 0.1g again, stirring and dissolving mixes, and is added dropwise in the four-hole boiling flask, and 1.5h drips off; Drip off the back and be incubated 2.5h under reflux state, stopped reaction gets acrylic resin.During use by the solidifying agent γ-An Bingjisanyiyangjiguiwan: resin is to mix at 1: 5, stirs, and towards rare, can spray.The wear resisting property of filming sees Table 1.
Embodiment 6
In four-hole boiling flask, add the toluene of 25g, the isopropylcarbinol of 75g, heated and stirred is to refluxing; Take by weighing 60g methacrylic acid laurate, 10g methacrylic acid benzyl ester, 10g cyclohexyl methacrylate, 20g methyl propenoic acid glycidyl ether again and be made into mix monomer, the benzoyl peroxide that adds 10g again, stirring and dissolving mixes, be added dropwise in the four-hole boiling flask, 1.5h drips off; Drip off the back and be incubated 3h under reflux state, stopped reaction gets acrylic resin.During use by the solidifying agent diethylamine: resin is to mix at 1: 25, stirs, and towards rare, can spray.The wear resisting property of filming sees Table 1.
Embodiment 7
In four-hole boiling flask, add the toluene of 90g, the isopropylcarbinol of 10g, heated and stirred is to refluxing; Take by weighing 65g methyl methacrylate, 20g vinylformic acid, 15g glycidyl methacrylate again and be made into mix monomer, add the benzoyl peroxide of 1g again, stirring and dissolving mixes, disposable joining in the four-hole boiling flask, and 2h drips off; Drip off the back and be incubated 2h under reflux state, stopped reaction gets acrylic resin.During use by the solidifying agent diethylamine: resin is to mix at 1: 5, stirs, and towards rare, can spray.The wear resisting property of filming sees Table 1.
Embodiment 8
In four-hole boiling flask, add the toluene of 30g, the isopropylcarbinol of 70g, heated and stirred is to refluxing; Take by weighing 50g methyl methacrylate, 20g2-ethylhexyl methacrylic ester, 15g methacrylic acid, 15 methyl propenoic acid glycidyl ethers again and be made into mix monomer, the benzoyl peroxide that adds 1g again, stirring and dissolving mixes, be added dropwise in the four-hole boiling flask, 1h drips off; Drip off the back and be incubated 2.5h under reflux state, stopped reaction gets acrylic resin.During use by the solidifying agent γ-An Bingjisanyiyangjiguiwan: resin is to mix at 1: 15, stirs, and towards rare, can spray.The wear resisting property of filming sees Table 1.
Behind 60 ℃ of following baking 12h of table 1, the wear resisting property of filming
Annotate: RCA: be the test result of the wear-resisting experimental machine of paper tape
Claims (4)
1. the preparation method of a silicon-acrylic coatings is characterized in that its step is as follows:
1) toluene or isopropylcarbinol or the mixing solutions of the two are joined in the reactor, be heated with stirring to backflow;
2) acrylic ester monomer and the acrylate monomer that contains epoxide group are mixed, the initiator that adds monomer total mass 0.1%~10% then, stirring and dissolving, mix, by mass percentage, acrylic ester monomer: the acrylate monomer that contains epoxide group is (80%~99%): (1%~20%), described acrylic ester monomer is a butyl acrylate, methyl acrylate, methyl methacrylate, n-BMA, Propenoic acid, 2-methyl, isobutyl ester, 2-ethylhexyl methacrylic ester, lauryl methacrylate(LMA), the methacrylic acid benzyl ester, at least a in the cyclohexyl methacrylate, the described acrylate monomer that contains epoxide group is a glycidyl methacrylate;
3) mixed monomer solution in the step 2 is added in the reactor in the mode of disposable adding or dropping, insulation 2~3h, stopped reaction gets acrylic resin;
4) acrylic resin is mixed with solidifying agent, the use that stirs, by mass percentage, acrylic resin: solidifying agent is 5~25: 1, described solidifying agent is a γ-An Bingjisanyiyangjiguiwan.
2. the preparation method of a kind of silicon-acrylic coatings as claimed in claim 1 is characterized in that described initiator is a benzoyl peroxide.
3. the preparation method of a kind of silicon-acrylic coatings as claimed in claim 1 is characterized in that the rate of addition in step 3) is 0.5~1h/50g.
4. the preparation method of a kind of silicon-acrylic coatings as claimed in claim 1, the mixing solutions that it is characterized in that toluene and isopropylcarbinol is an arbitrary proportion.
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CN2008100706086A CN101235245B (en) | 2008-02-02 | 2008-02-02 | Method for preparing silicone-acrylate dope |
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CN2008100706086A CN101235245B (en) | 2008-02-02 | 2008-02-02 | Method for preparing silicone-acrylate dope |
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CN101235245B true CN101235245B (en) | 2010-12-08 |
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CN101982512B (en) * | 2010-09-21 | 2014-07-09 | 常州大学 | Silicone acrylate coating resin and preparation method thereof |
CN102416373B (en) * | 2011-09-22 | 2014-03-12 | 东莞广泽汽车饰件有限公司 | High gloss coating process of surface of plastic substrate |
CN102417777A (en) * | 2011-11-22 | 2012-04-18 | 吴江市天源塑胶有限公司 | Preparation method of quick-drying coating for plastic shell of television |
CN110305326B (en) * | 2019-07-17 | 2022-07-15 | 上海应用技术大学 | Water-based acrylic resin for engineering machinery paint and preparation method thereof |
CN113831839B (en) * | 2021-10-15 | 2022-06-10 | 信和新材料(苏州)有限公司 | Concrete laitance reinforcer and preparation method and application thereof |
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