CN104004429B - Based on the normal temperature solidified composite coating and preparation method thereof of modification 107 silicon rubber - Google Patents
Based on the normal temperature solidified composite coating and preparation method thereof of modification 107 silicon rubber Download PDFInfo
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- CN104004429B CN104004429B CN201410202106.XA CN201410202106A CN104004429B CN 104004429 B CN104004429 B CN 104004429B CN 201410202106 A CN201410202106 A CN 201410202106A CN 104004429 B CN104004429 B CN 104004429B
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Abstract
The invention discloses a kind of normal temperature solidified composite coating based on modification 107 silicon rubber and preparation method thereof, this coating by mass percentage by: 107 silicon rubber are 35 ~ 50%wt, dimethylbenzene is 15 ~ 20%wt, γ-methacryloxypropyl trimethoxy silane is 2 ~ 10%wt, tetraethoxy is 5 ~ 25%wt, vinylbenzene is 5 ~ 10%wt, methyl methacrylate is 5 ~ 10%wt, aerosil is 1 ~ 5%wt, azo-bis-isobutyl cyanide is 0.4 ~ 5%wt, and dibutyl tin laurate is 0.05 ~ 0.1%wt composition.Preparation method be first by acrylic resin graft polymerization in 107 silicon rubber segments, then system adds aerosil and tetraethoxy, under the effect of dibutyltin dilaurate catalyst, composite coating film-forming.The normal temperature solidified film forming of composite coating of the present invention, is applicable to protection and the decoration of different metal ground.
Description
Technical field
The invention belongs to technical field of coatings, relate to a kind of special high-performance coating, more specifically relate to a kind of composite coating normal temperature solidified based on modification 107 silicon rubber and preparation method thereof.
Background technology
According to a large amount of Research statistics, the iron and steel that the whole world produces every year still has 30% to be corroded, and wherein the iron and steel of 10% will become scrap iron.As metallic corrosion reaches several hundred million pounds every year in Britain, account for 4.2% of gross national product in the U.S., account for 4% of gross national product in China, exceeded the damnous summation of fire, disaster caused by a windstorm and earthquake.Along with the development of iron and steel, metallurgy, machinery manufacturing industry, antirust, consumption reduction problem is the emphasis that scientific research personnel pays close attention to and studies always.
Traditional organic polymer resin, owing to having good film-forming properties, snappiness, base material sticking power and lower cost, so be the main film forming matter of coating always.But traditional coating resin is mainly with acrylic resin, epoxy resin, urethane resin is main, and the weathering resistance of segment, ageing resistance poor-performing, use in long term outdoor or hot environment, easily molecular rupture occurs, and film efflorescence destroys.And 107 silicon rubber are because the bond energy of Si-O key is higher than C-C key and C-O key, it has good thermotolerance and weathering resistance, but due to the bond distance of Si-O-Si key, bond angle large, Chain Flexibility is good, and 107 silicon rubber become film dynamic performance not good, and hardness is poor, film-forming temperature is higher simultaneously, solidification difficulty.This is also one of defect of having limited to commercial applications further.107 silicon rubber are carried out grafting modification, by the chemical bond bridge joint effect of silane coupling agent, make methyl methacrylate/vinylbenzene mix monomer graft polymerization on 107 silicon rubber segments, then aerosil is dispersed in compound resin, using tetraethoxy as solidifying agent, obtain the compound coating with excellent properties through catalyst crosslinking curing, the composite coating of preparation has commercial applications feasibility in metal protection field.
Summary of the invention
Object of the present invention, mainly for the defect that current technology exists, provides a kind of composite coating normal temperature solidified based on modified silicon rubber and preparation method thereof.
In order to achieve the above object, the present invention realizes the technical scheme that object adopts and is:
A kind of composite coating normal temperature solidified based on modification 107 silicon rubber, content is 35 ~ 50%wt by component 107 silicon rubber by mass percentage, dimethylbenzene is 15 ~ 20%wt, γ-methacryloxypropyl trimethoxy silane is 2 ~ 10%wt, tetraethoxy is 5 ~ 25%wt, vinylbenzene is 5 ~ 10%wt, methyl methacrylate is 5 ~ 10%wt, aerosil is 1 ~ 5%wt, Diisopropyl azodicarboxylate is 0.4 ~ 5%wt, and dibutyl tin laurate is 0.05 ~ 0.1%wt composition.
107 silicon rubber described above are with the polydimethylsiloxane of hydroxyl dimethylsilyloxy end group, and the range of viscosities at 25 DEG C is 80000 ~ 500000cs.
Aerosil described above is goldschmidt chemical corporation product, and its model is: any one in A200, A300 and A380.
In order to achieve the above object, the present invention realizes another technical scheme that object adopts and is:
The preparation method of a kind of composite coating normal temperature solidified based on modification 107 silicon rubber of the present invention, comprises the steps:
(1) 107 silicon rubber dissolvings are scattered in xylene solvent, stir 5 ~ 10 minutes dissolve be uniformly dispersed after, be added dropwise to the 20%wt of γ-methacryloxypropyl trimethoxy silane and dibutyl tin laurate total content, reaction system is at 50 ~ 70 DEG C, heat while stirring, react 2 ~ 4 hours to obtain reaction product;
(2) by Diisopropyl azodicarboxylate dispersed with stirring in methyl methacrylate/cinnamic mix monomer, to be mixed evenly after, be progressively added dropwise in the reaction product of step (1) gained; During dropping, system keeps whipped state and temperature of reaction controls at 60 ~ 80 DEG C, and the time controling of dropping was at 10 ~ 60 minutes, after dropwising, the temperature of reaction system controls, at 70 ~ 100 DEG C, to heat while stirring, and the reaction times is obtain reaction product in 8 ~ 12 hours;
(3) at room temperature, progressively aerosil is added in the product of step (2) gained, stir 25 ~ 60 minutes with the rotating speed of 2000 ~ 5000 revs/min, and then ultrasonic disperse 10 ~ 30 minutes, the dibutyl tin laurate mixture of the tetraethoxy finally added and residue 80%wt, stir, namely obtain the normal temperature solidified composite coating based on modification 107 silicon rubber.
Coating of the present invention can adopt brushing, and the methods such as roller coating are painted on substrate surface, at room temperature solvent flashing crosslinking curing film forming.
A kind of normal temperature solidified composite coating based on modification 107 silicon rubber of the present invention and preparation method thereof major advantage compared to existing technology and beneficial effect are:
1, by the chemical bonds effect of silane coupling agent, there is 107 silicon rubber that polarity is low, surface tension is low and the acrylic resin graft copolymerization with mechanical properties strength, make compound coating based on this modified resin while having certain mechanical strength, film tension is low, heatproof good weatherability.
Adding 2, due to nano silicon, the hydrogen bond action of powder and modified resin, is conducive to the mechanical property improving paint film, the existence of tetraethoxy solidifying agent, compound resin can be made to be at room temperature drying and forming-film, be easy to brushing solidification.
Embodiment
Below in conjunction with embodiment, further specific descriptions are done to the present invention, but be not limited to this.
Embodiment 1
One, raw material and mass percentage content are:
Two, preparation method
(1) 107 silicon rubber dissolvings are scattered in xylene solvent, stir 5 minutes dissolve be uniformly dispersed after, be added dropwise to the 20%wt of γ-methacryloxypropyl trimethoxy silane and dibutyl tin laurate total content, reaction system is at 50 DEG C of temperature, heat while stirring, react 2 hours.
(2) by Diisopropyl azodicarboxylate dispersed with stirring in methyl methacrylate/cinnamic mix monomer, to be mixed evenly after, be progressively added dropwise in the reaction product of step (1).During dropping, system keeps whipped state and temperature of reaction controls at 75 DEG C, and the time controling of dropping was at 10 minutes, and after dropwising, the temperature of reaction system controls, at 80 DEG C, to heat while stirring, and the reaction times is 8 hours.
(3) at room temperature, progressively aerosil is added in step (2) product, 25 minutes are stirred with the rotating speed of 4000 revs/min, and then ultrasonic disperse 10 minutes, finally add the dibutyl tin laurate mixture of tetraethoxy and residue 80%, stir, namely obtain the normal temperature solidified composite coating based on modification 107 silicon rubber.
Embodiment 2
One, raw material and mass percentage content are:
Two, preparation method
(1) 107 silicon rubber dissolvings are scattered in xylene solvent, stir 10 minutes dissolve be uniformly dispersed after, be added dropwise to the 20%wt of γ-methacryloxypropyl trimethoxy silane and dibutyl tin laurate total content, reaction system is at 70 DEG C of temperature, heat while stirring, react 4 hours.
(2) by Diisopropyl azodicarboxylate dispersed with stirring in methyl methacrylate/cinnamic mix monomer, to be mixed evenly after, be progressively added dropwise in the reaction product of step (1).During dropping, system keeps whipped state and temperature of reaction controls at 60 DEG C, and the time controling of dropping was at 60 minutes, and after dropwising, the temperature of reaction system controls, at 100 DEG C, to heat while stirring, and the reaction times is 12 hours.
(3) at room temperature, progressively aerosil is added in step (2) product, 60 minutes are stirred with the rotating speed of 2500 revs/min, and then ultrasonic disperse 30 minutes, finally add the dibutyl tin laurate mixture of tetraethoxy and residue 80%, stir, namely obtain the normal temperature solidified composite coating based on modified silicon rubber.
Embodiment 3
One, raw material and mass percentage content are:
Two, preparation method
(1) 107 silicon rubber dissolvings are scattered in xylene solvent, stir 7 minutes dissolve be uniformly dispersed after, be added dropwise to the 20%wt of γ-methacryloxypropyl trimethoxy silane and dibutyl tin laurate total content, reaction system is at 60 DEG C of temperature, heat while stirring, react 3 hours.
(2) by Diisopropyl azodicarboxylate dispersed with stirring in methyl methacrylate/cinnamic mix monomer, to be mixed evenly after, be progressively added dropwise in the reaction product of step (1).During dropping, system keeps whipped state and temperature of reaction controls at 70 DEG C, and the time controling of dropping was at 30 minutes, and after dropwising, the temperature of reaction system controls, at 90 DEG C, to heat while stirring, and the reaction times is 9 hours.
(3) at room temperature, progressively aerosil is added in step (2) product, 45 minutes are stirred with the rotating speed of 2000 revs/min, and then ultrasonic disperse 20 minutes, finally add the dibutyl tin laurate mixture of tetraethoxy and residue 80%, stir, namely obtain the normal temperature solidified composite coating based on modification 107 silicon rubber.
Embodiment 4
One, raw material and mass percentage content are:
Two, preparation method
(1) 107 silicon rubber dissolvings are scattered in xylene solvent, stir 9 minutes dissolve be uniformly dispersed after, be added dropwise to the 20%wt of γ-methacryloxypropyl trimethoxy silane and dibutyl tin laurate total content, reaction system is at 65 DEG C of temperature, heat while stirring, react 4 hours;
(2) by Diisopropyl azodicarboxylate dispersed with stirring in methyl methacrylate/cinnamic mix monomer, to be mixed evenly after, be progressively added dropwise in the reaction product of step (1).During dropping, system keeps whipped state and temperature of reaction controls at 80 DEG C, and the time controling of dropping was at 45 minutes, and after dropwising, the temperature of reaction system controls, at 80 DEG C, to heat while stirring, and the reaction times is 10 hours
(3) at room temperature, progressively aerosil is added in step (2) product, 45 minutes are stirred with the rotating speed of 5000 revs/min, and then ultrasonic disperse 25 minutes, finally add the dibutyl tin laurate mixture of tetraethoxy and residue 80%, stir, namely obtain the normal temperature solidified composite coating based on modification 107 silicon rubber.
Film curing and Performance comparision thereof
According to embodiment 1 ~ 4, synthesize and prepare based on the normal temperature solidified composite coating of modification 107 silicon rubber, by it by spraying or brushing mode, be coated in tinplate version, room temperature leaves standstill 4 ~ 8 hours film-formings, and mechanical property and weather-proof test performance are in table one.
Table one. the performance of ambient cure weather-proof excellent in mechanical performance coating paint film
Claims (4)
1. based on a normal temperature solidified composite coating for modification 107 silicon rubber, it is characterized in that, be made up of following component and content by mass percentage:
Be scattered in xylene solvent by first 107 silicon rubber being dissolved, stir 5 ~ 10 minutes dissolve be uniformly dispersed after, be added dropwise to the 20%wt of γ-methacryloxypropyl trimethoxy silane and dibutyl tin laurate total content, reaction system is at 50 ~ 70 DEG C, heat while stirring, react 2 ~ 4 hours to obtain reaction product; Then by Diisopropyl azodicarboxylate dispersed with stirring in methyl methacrylate/cinnamic mix monomer, after stirring, progressively be added dropwise in the reaction product of above-mentioned gained, during dropping, system keeps whipped state and temperature of reaction controls at 60 ~ 80 DEG C, and the time controling of dropping was at 10 ~ 60 minutes, after dropwising, the temperature of reaction system controls, at 70 ~ 100 DEG C, to heat while stirring, and the reaction times is obtain reaction product in 8 ~ 12 hours; At room temperature, progressively aerosil is added again by the product of gained, stir 25 ~ 60 minutes with the rotating speed of 2000 ~ 5000 revs/min, and then ultrasonic disperse 10 ~ 30 minutes, finally add the dibutyl tin laurate of tetraethoxy and residue 80%wt, stir, obtain the normal temperature solidified composite coating based on modification 107 silicon rubber.
2. by a kind of normal temperature solidified composite coating based on modification 107 silicon rubber according to claim 1, it is characterized in that, 107 described silicon rubber are with the polydimethylsiloxane of hydroxyl dimethylsilyloxy end group, and the range of viscosities at 25 DEG C is 80000 ~ 500000cs.
3. by a kind of normal temperature solidified composite coating based on modification 107 silicon rubber according to claim 1, it is characterized in that, described aerosil is the product that goldschmidt chemical corporation is produced: any one in A200, A300 and A380.
4. a preparation method for the normal temperature solidified composite coating based on modification 107 silicon rubber as described in as arbitrary in claims 1 to 3, is characterized in that comprising the steps:
(1) 107 silicon rubber dissolvings are scattered in xylene solvent, stir 5 ~ 10 minutes dissolve be uniformly dispersed after, be added dropwise to the 20%wt of γ-methacryloxypropyl trimethoxy silane and dibutyl tin laurate total content, reaction system is at 50 ~ 70 DEG C, heat while stirring, react 2 ~ 4 hours to obtain reaction product;
(2) by Diisopropyl azodicarboxylate dispersed with stirring in methyl methacrylate/cinnamic mix monomer, to be mixed evenly after, progressively be added dropwise in the reaction product of step (1) gained, during dropping, system keeps whipped state and temperature of reaction controls at 60 ~ 80 DEG C, and the time controling of dropping was at 10 ~ 60 minutes, after dropwising, the temperature of reaction system controls, at 70 ~ 100 DEG C, to heat while stirring, and the reaction times is obtain reaction product in 8 ~ 12 hours;
(3) under room temperature, progressively aerosil is added in the product of step (2) gained, stir 25 ~ 60 minutes with the rotating speed of 2000 ~ 5000 revs/min, and then ultrasonic disperse 10 ~ 30 minutes, finally add the dibutyl tin laurate of tetraethoxy and residue 80%wt, stir, namely obtain the normal temperature solidified composite coating based on modification 107 silicon rubber.
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Effective date of registration: 20220415 Address after: 201800 358 Kefu Road, Jiading District, Shanghai_ Room j2644, Zone E, floor 1, building 4, No. 368 Patentee after: Shanghai Yiyou Information Technology Co.,Ltd. Address before: Meng Xi Road 212003 Zhenjiang city of Jiangsu province Jingkou District No. 2 Patentee before: JIANGSU University OF SCIENCE AND TECHNOLOGY Effective date of registration: 20220415 Address after: 518100 first floor, building 8, Xingwei (Phoenix) Third Industrial Zone, Fuyong street, Bao'an District, Shenzhen, Guangdong Province Patentee after: SHENZHEN JINLIAN TECHNOLOGY Co.,Ltd. Address before: 201800 358 Kefu Road, Jiading District, Shanghai_ Room j2644, Zone E, floor 1, building 4, No. 368 Patentee before: Shanghai Yiyou Information Technology Co.,Ltd. |