CN104987467A - Acrylate modified hydroxyl-terminated butadiene resin with low infrared emissivity, and preparation method thereof - Google Patents
Acrylate modified hydroxyl-terminated butadiene resin with low infrared emissivity, and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an acrylate modified hydroxyl-terminated butadiene resin with low infrared emissivity, and a preparation method thereof. The acrylate modified hydroxyl-terminated butadiene resin is obtained through free radical copolymerization of hydroxyl-terminated polybutadiene and an acrylate monomer and/or a methacrylate monomer, and the solid content of the obtained acrylate modified hydroxyl-terminated butadiene resin with low infrared emissivity is 40-60wt%. The acrylate modified hydroxyl-terminated butadiene resin with low infrared emissivity has the advantages of low glossiness and good weather ability, can be used to prepare dual-component infrared camouflage coatings, and can be used to coat military use devices, machines, engineering, barracks and other places to realize a camouflage purpose.
Description
Technical field
The present invention relates to a kind of resin, acrylate modified hydroxy-terminated polybutadienes resin being specifically related to a kind of low infrared emissivity and preparation method thereof.
Background technology
Along with the development of science and technology, investigation is day by day advanced, in order to avoid military target and weaponry are found by enemy, use stealthy technique improves its viability and penetration ability becomes the simplest and effective means, and the research of stealthy technique becomes the important directions of military technique development.Infrared stealth coating is a kind of stealthy technique making the infra-red detection equipment of 3 μm ~ 5 μm and 8 μm ~ 14 μm of service bands be difficult to detect or cause illusion, also referred to as thermal stealth coating.For a large amount of land Low Temperature Targets, mainly from the threat of 8 μm ~ 14 μm of thermal infrared imagers.By infrared stealth coating for the outside of target, camouflage net and thermofin, make infrared stealth coating, can reduce, change the heat-radiating properties of target self, the comprehensive scattering properties of target and Beijing can be made again to adapt, and there is the features such as easy construction, cost are low, superior performance.The major function of infrared stealth coating is that coating has low-launch-rate high-reflectivity.
More and the infrared stealth coating being applied to military use of current research is primarily of absorbing material and tackiness agent composition, and the effect of absorbing material mainly absorbs can through the hertzian wave of infrared detector, and the reflected signal strength that detection equipment is obtained reduces greatly.The Main Function of tackiness agent be mix with absorber material, film forming, to be coated on military target and weaponry surface, play stealthy effect.
Tackiness agent for Infrared stealthy materials has inorganic and organic two types.Inorganic adhesive is inorganic silicate and inorganic phosphate mainly, compared with organic binder bond, inorganic adhesive physical and mechanical properties and processing performance poor, some inorganic adhesive needs hot setting film forming, can have influence on the microwave absorbing property of absorption agent.Therefore, mostly the tackiness agent for invisible coating is organic binder bond.
In general, the organic binder bond for infrared stealth coating should have following fundamental characteristics: 1, have lower infrared emittance; 2, good physical and mechanical properties is had; 3, there is good outdoor weatherability; 4, there is good workability.
Used infrared stealth coating organic binder bond has polyolefins (polyethylene, Chloropolystyrene, ethene and cinnamic multipolymer) and rubber-like (isoprene-isobutylene rubber, chlorinated rubber and terpolymer EP rubber) and other polymkeric substance (Synolac, epoxy resin etc.).
Such as Chinese patent literature CN 103290684 A (application number 201310248696.5) discloses a kind of Low-infrared-emissivgreen green stealth paint and preparation method thereof, in coating, tackiness agent is polyacrylic ester, polystyrene, urethane and polyacrylonitrile, these polyolefins tackiness agent weathering resistancies are poor, open air can not be used for, and many military applications use all out of doors, time length can affect infrared emission performance.
Rubber adhesive molecular weight is large, and viscosity is large, and paint film fullness ratio is inadequate, and weathering resistance is also poor, bad for outdoor effect; Such as the reflectivity of Synolac wherein, epoxy resin itself is high, and need a large amount of absorbing material to fill, and weathering resistance is also bad, the infrared stealth coating effect of preparation is not fine.
In order to improve the performance of tackiness agent, the domestic people of having carries out modification or grafted propylene acid resin with terpolymer EP rubber, although the tackiness agent weathering resistance obtained slightly improves, can be used for open air, but without hydroxyl structure in molecule, cannot crosslinking curing, with the patience of the paint film of its obtained paint spraying is inadequate, weather-proof, water-fast, erosion resistance is all inadequate.Somebody prepares invisible coating with high solid content and low viscosity Hydroxylated acrylic resin, and because the C-O key stretching vibration of acrylic resin absorbs, resin itself does not have low infrared emissivity, therefore bad as infrared stealth binder performance.
And for example Chinese patent literature CN 102925050 (application number 201210459422.6) disclose a kind of water-based infrared-preparation method of Laser Compatible Camouflage Paints, wherein tackiness agent is polycarbonate polyurethane polycarbonate diol and isoflurane chalcone diisocyanate, dimethylol propionic acid are obtained by reacting.Compared with the polyurethane material synthesized by traditional dibasic alcohol, polycarbonate polyurethane has the optical property of excellent mechanical property, hydrolytic resistance, thermotolerance, wear resistance and excellence.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of acrylate modified hydroxy-terminated polybutadienes resin that can be used as the low infrared emissivity of tackiness agent in infrared stealth coating and preparation method thereof.
The technical scheme realizing the object of the invention is a kind of acrylate modified hydroxy-terminated polybutadienes resin of low infrared emissivity, by hydroxy-terminated polybutadienes and acrylate monomer and/or methacrylate monomer by free-radical polymerized acquisition, in free radicals copolymerization reaction, each raw material dosage is as follows: hydroxy-terminated polybutadienes 5wt% ~ 15wt%, acrylate monomer and/or methacrylate monomer 25wt% ~ 55wt%, solvent 35wt% ~ 65wt%, initiator 0.5wt% ~ 2wt%, the acrylate modified hydroxy-terminated polybutadienes resin solid content of the low infrared emissivity of gained is 40 ~ 60wt%.
Described hydroxy-terminated polybutadienes is the homopolymer of divinyl, and number-average molecular weight is 2000 ~ 3000; On average there is two or more hydroxyl at each macromole two ends.
Described acrylate monomer is one or more the composition in vinylformic acid, ethyl propenoate, butyl acrylate, Isooctyl acrylate monomer, glycidyl acrylate, isobornyl acrylate; Methacrylate monomer is one or more the composition in methyl methacrylate, butyl methacrylate, Propenoic acid, 2-methyl, isobutyl ester, isobornyl methacrylate.
As optionally, that reacts with hydroxy-terminated polybutadienes together with acrylate monomer and/or methacrylate monomer also comprises modified monomer, and modified monomer is tertiary carbonic acid glycidyl ester, tertiary ethylene carbonate or vinylbenzene; The mixture of modified monomer and acrylate monomer and/or methacrylate monomer and hydroxy-terminated polybutadienes react, and modified monomer and acrylate monomer and/or methacrylate monomer consumption account for the 25wt% ~ 55wt% reacting total consumption.
Described solvent is one or more the composition in varsol, ketones solvent, esters solvent, ether solvent, solvent of ether ester type.
Described initiator is Diisopropyl azodicarboxylate, benzoyl peroxide, one or more the composition in peroxidized t-butyl perbenzoate or ditertiary butyl peroxide.
A kind of preparation method of acrylate modified hydroxy-terminated polybutadienes resin of low infrared emissivity as above, step is as follows: in reaction flask, add the part in hydroxy-terminated polybutadienes and solvent, stir, heating makes material in reaction flask be warming up to 80 DEG C ~ 130 DEG C; Then drip acrylate monomer and/or methacrylate monomer and the mixture of the part in initiator, dropwise in 3 ~ 5h, dropwising rear first time is incubated 1h; Insulation terminates the rear mixture continuing to drip residual solvent and residue initiator, and dropwise in 0.5 ~ 1h, cooling discharge be again incubated 2 ~ 3h at 80 DEG C ~ 130 DEG C after, obtains product.
The amount of the initiator wherein dripped in reaction flask is for the first time for the second time to 1.8 ~ 2.5 times of dripping quantity in reaction flask.
The amount of the solvent wherein dripped in reaction flask is for the first time for the second time to 4 ~ 11 times of dripping quantity in reaction flask.
As optionally, after heating makes material in reaction flask be warming up to 80 DEG C ~ 130 DEG C, drip the mixture of the part in modified monomer and/or acrylate monomer and/or methacrylate monomer and initiator, dropwise in 3 ~ 5h;
Described modified monomer is tertiary carbonic acid glycidyl ester, tertiary ethylene carbonate or vinylbenzene; Described acrylate monomer is one or more the composition in vinylformic acid, ethyl propenoate, butyl acrylate, Isooctyl acrylate monomer, glycidyl acrylate, isobornyl acrylate; Methacrylate monomer is one or more the composition in methyl methacrylate, butyl methacrylate, Propenoic acid, 2-methyl, isobutyl ester, isobornyl methacrylate.
The present invention has positive effect: (1) acrylate modified hydroxy-terminated polybutadienes resin of the present invention is obtained by hydroxy-terminated polybutadienes and acrylic ester copolymer: the hydroxy-terminated polybutadienes in resin has Linear Double bond structure, infrared transparent is good, gloss is low, reflectivity is low, is desirable stealth material; Hydroxy-terminated polybutadienes by with acrylic ester copolymer modification, improve the weathering resistance of resin, can be used for the occasions such as outdoor; Because the strong primary hydroxyl of reactive behavior is contained at hydroxy-terminated polybutadienes molecule two ends, can with cured with isocyanates, after being made into polyurethane coating, the weathering resistance of the paint film that institute's application obtains, water tolerance, the more general polyurethane coating of salt fog resistance strengthen further, and the infrared stealth coating of preparation is better long-lasting; The polybutadiene configuration good toughness of long-chain in acrylate modified hydroxy-terminated polybutadienes resin of the present invention, mechanical property are superior, are desirable infrared stealth tackiness agents.
(2) low, the good weatherability of the acrylate modified hydroxy-terminated polybutadienes resinous luster of low infrared emissivity of the present invention, can be used for the infrared stealth coating preparing two component, for the application in the places such as military equipment, machinery, engineering and barracks, play stealthy object.
Embodiment
Following examples raw materials is commercially available industrial goods, is buied by commercial channel.
(the acrylate modified hydroxy-terminated polybutadienes resin of embodiment 1, low infrared emissivity)
The acrylate modified hydroxy-terminated polybutadienes resin of the low infrared emissivity of the present embodiment by hydroxy-terminated polybutadienes and acrylate monomer and/or methacrylate monomer by free-radical polymerized acquisition.In free radicals copolymerization reaction, each raw material dosage is as follows: hydroxy-terminated polybutadienes 5wt% ~ 15wt%, acrylate monomer or methacrylate monomer 25wt% ~ 55wt%, solvent 35wt% ~ 65wt%, initiator 0.5wt% ~ 2wt%, each raw material dosage sum is 100wt%, and the acrylate modified hydroxy-terminated polybutadienes resin solid content of the low infrared emissivity of gained is 40-60wt%.
Described hydroxy-terminated polybutadienes is the homopolymer of divinyl, and number-average molecular weight is 2000 ~ 3000.On average there is two or more hydroxyl at each macromole two ends, and the hydroxy-terminated polybutadienes that wherein hydroxy-terminated polybutadienes of Isosorbide-5-Nitrae-structure accounts for 80%, 1,2-vinyl structure of hydroxy-terminated polybutadienes total amount accounts for 20% of hydroxy-terminated polybutadienes total amount.
Described acrylate monomer is one or more the composition in vinylformic acid, ethyl propenoate, butyl acrylate, Isooctyl acrylate monomer, glycidyl acrylate, isobornyl acrylate; Methacrylate monomer is a kind of in methyl methacrylate, butyl methacrylate, Propenoic acid, 2-methyl, isobutyl ester, isobornyl methacrylate or or more than one composition.
As optionally, after acrylate monomer and/or methacrylate monomer mix with modified monomer and hydroxy-terminated polybutadienes react, modified monomer is tertiary carbonic acid glycidyl ester, tertiary ethylene carbonate or vinylbenzene.Modified monomer and acrylate monomer and/or methacrylate monomer consumption account for the 25wt% ~ 55wt% reacting total consumption.Described solvent is one or more the composition in varsol, ketones solvent, esters solvent, ether solvent, solvent of ether ester type.
Described initiator is Diisopropyl azodicarboxylate, benzoyl peroxide, one or more the composition in peroxidized t-butyl perbenzoate or ditertiary butyl peroxide.
(preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of embodiment 2, low infrared emissivity)
The preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of the low infrared emissivity of the present embodiment is as follows:
In four mouthfuls of reaction flasks of 500mL that agitator, thermometer, dropping funnel and condenser are housed; add solvent xylene 200g (accounting for the 40wt% reacting the total amount that feeds intake), hydroxy-terminated polybutadienes 50g (accounting for the 10wt% reacting the total amount that feeds intake); under nitrogen atmosphere protection; start agitator, heating makes material in reaction flask be warming up to 80 DEG C.
Open dropping funnel, start acrylate monomer at the uniform velocity addition funnel and/or or the mixed solution 200g of methacrylate monomer and initiator, mixed solution in the present embodiment in dropping funnel comprises methyl methacrylate 130g, butyl acrylate 68g and (amounts to 198g, account for the 39.6wt% reacting the total amount that feeds intake) and initiator Diisopropyl azodicarboxylate 2g (accounting for the 0.4wt% reacting the total amount that feeds intake), in dropping process, in bottle, material carries out polyreaction at 80 DEG C ~ 90 DEG C, 2.5h ~ 3h dropwises, and dropwises rear insulation 1 hour.
Insulation terminates the mixture 50g continuing to drip solvent and initiator in backward reaction flask, wherein solvent is dimethylbenzene 49g (accounting for the 9.8wt% reacting the total amount that feeds intake), initiator is Diisopropyl azodicarboxylate 1g (accounting for the 0.2wt% reacting the total amount that feeds intake), temperature in reaction flask is kept to drip at 80 DEG C ~ 90 DEG C, 1h drips off, cooling discharge after soaking time 3h at insulation 80 ~ 90 DEG C, the acrylate modified hydroxy-terminated polybutadienes resin 500g of obtained low infrared emissivity, gained resin solid content is 50wt%, saves backup.
(preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of embodiment 3, low infrared emissivity)
The preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of the low infrared emissivity of the present embodiment is as follows:
In four mouthfuls of reaction flasks of 500mL that agitator, thermometer, dropping funnel and condenser are housed; add solvent toluene 250g (accounting for the 50wt% reacting the total amount that feeds intake), hydroxy-terminated polybutadienes 50g (accounting for the 10wt% reacting the total amount that feeds intake); under nitrogen atmosphere protection; start agitator, heating makes material in reaction flask be warming up to 100 DEG C.
Open dropping funnel, start acrylate monomer at the uniform velocity addition funnel and/or or the mixed solution 150g of methacrylate monomer and initiator, mixed solution in the present embodiment in dropping funnel comprises methyl methacrylate 70g, Propenoic acid, 2-methyl, isobutyl ester 50g, butyl acrylate 27g (amounts to 147g, account for the 29.4wt% reacting the total amount that feeds intake) and initiator benzoyl peroxide 3g (accounting for the 0.6wt% reacting the total amount that feeds intake), in dropping process, in bottle, material carries out polyreaction at 100 DEG C ~ 110 DEG C, 3h dropwises, and dropwises rear insulation 1 hour.
Insulation terminates the mixture 50g continuing to drip solvent and initiator in backward reaction flask, wherein solvent is toluene 48g (accounting for the 9.6wt% reacting the total amount that feeds intake), initiator is benzoyl peroxide 2g (accounting for the 0.4wt% reacting the total amount that feeds intake), temperature in reaction flask is kept to drip at 100 ~ 110 DEG C, 1h drips off, cooling discharge after soaking time 3h at 110 ~ 120 DEG C, the acrylate modified hydroxy-terminated polybutadienes resin 500g of obtained low infrared emissivity, gained resin solid content is 40wt%, saves backup.
(preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of embodiment 4, low infrared emissivity)
The preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of the low infrared emissivity of the present embodiment is as follows:
In four mouthfuls of reaction flasks of 500mL that agitator, thermometer, dropping funnel and condenser are housed; add solvent butyl acetate 180g (accounting for the 36wt% reacting the total amount that feeds intake) and hydroxy-terminated polybutadienes 30g (accounting for the 6wt% reacting the total amount that feeds intake); under nitrogen atmosphere protection; start agitator, heating makes material in reaction flask be warming up to 120 DEG C.
Open dropping funnel, start the mixed solution 270g of acrylate monomer at the uniform velocity addition funnel and/or methacrylate monomer and initiator, mixed solution in the present embodiment in dropping funnel comprises methyl methacrylate 150g, butyl methacrylate 50g, butyl acrylate 66g (amounts to 266g, account for the 53.2wt% reacting the total amount that feeds intake) and initiator benzoyl peroxide 4g (accounting for the 0.8wt% reacting the total amount that feeds intake), in dropping process, in bottle, material carries out polyreaction at 120 DEG C ~ 130 DEG C, 5h dropwises, and dropwises rear insulation 1 hour.
Insulation terminates the mixture 20g continuing to drip solvent and initiator in backward reaction flask, wherein, solvent is toluene 18g (accounting for the 3.6wt% reacting the total amount that feeds intake), initiator is benzoyl peroxide 2g (accounting for the 0.4wt% reacting the total amount that feeds intake), temperature in reaction flask is kept to drip at 120 ~ 130 DEG C, 0.5h drips off, at 120 ~ 130 DEG C, 3h is incubated after dripping off, cooling discharge, the acrylate modified hydroxy-terminated polybutadienes resin 500g of obtained low infrared emissivity, gained resin solid content is 60wt%, saves backup.
(preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of embodiment 5, low infrared emissivity)
The preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of the low infrared emissivity of the present embodiment is as follows:
In four mouthfuls of reaction flasks of 500mL that agitator, thermometer, dropping funnel and condenser are housed; add toluene solvant 250g (accounting for the 50wt% reacting the total amount that feeds intake) and hydroxy-terminated polybutadienes 40g (accounting for the 8wt% reacting the total amount that feeds intake); under nitrogen atmosphere protection; start agitator, heating makes material in reaction flask be warming up to 90 DEG C.
Open dropping funnel, start the mixed solution 160g of acrylate monomer at the uniform velocity addition funnel and/or methacrylate monomer and initiator, mixed solution in the present embodiment in dropping funnel comprises methyl methacrylate 79g, butyl methacrylate 79g and (amounts to 158g, account for the 31.6wt% reacting the total amount that feeds intake), initiator is Diisopropyl azodicarboxylate 2g (accounting for the 0.4wt% reacting the total amount that feeds intake), in dropping process, in bottle, material carries out reactive polymeric at 90 ~ 100 DEG C, 4h dropwises, and dropwises rear insulation 1 hour.
Insulation terminates the mixture 50g (comprising solvent and initiator) continuing to drip solvent and initiator in backward reaction flask, wherein solvent is toluene 49g (accounting for the 9.8wt% reacting the total amount that feeds intake), initiator is benzoyl peroxide 1g (accounting for the 0.2wt% reacting the total amount that feeds intake), temperature in reaction flask is kept to drip at 90 ~ 100 DEG C, 1h drips off, after dripping off at 100 ~ 110 DEG C cooling discharge after soaking time 3h, the acrylate modified hydroxy-terminated polybutadienes resin 500g of obtained low infrared emissivity, gained resin solid content is 40wt%, save backup.
(application examples)
Should the Performance Detection of use-case to the obtained acrylate modified hydroxy-terminated polybutadienes resin of embodiment 1 to embodiment 4 as follows:
(1) detection method
1. the preparation of paint film
By the general preparation method's preparation of GB1727-92 paint film, solidifying agent is the aliphatic isocyanates N-3390 solidifying agent of Beyer Co., Ltd, dilute with dimethylbenzene, the acrylate modified hydroxy-terminated polybutadienes portions of resin N-3390 solidifying agent of consumption low infrared emissivity: dimethylbenzene=5: 1: 3, spray to the tinplate of the 50mm × 120mm through polishing, film thickness is less than 0.2mm.Dry 48h under fixed temperature and humidity condition.
2. the detection of emittance
By GJB 5023.2-2003 material and coating reflectivity and emittance testing method part 2: emittance regulation detects.The ET-10 portable infrared spectral emissions instrument of peace continent science and technology is adopted to measure, wavelength region 8-12 μm.
3. paint film appearance: range estimation.
4. resin viscosity detection method
Detect by the mensuration regulation of GB/T2794-1995 tackiness agent viscosity.
5. resin solid content detection method
Detect by the mensuration regulation of GB/T1725-2007 colored paint, varnish and plastics non-volatile content.
6. gloss of film detection method
By GB/T9754-2007 paint and varnish not 20 °, 60 ° and 85 ° specular glosss of the colored paint paint film of containing metal pigment measuring method regulation detect.
7. paint film aberration
Measuring method second section by GB/T11186.2-1989 film color: the measuring method that color measuring specifies detects;
8. QUV is aging
Be exposed to by the artificial weathering of GB/T 23987-2009 paint and varnish coating the measuring method that fluorescent UV and water specifies to detect, fluorescent tube used is I type, exposes the exposure of employing method A-containing condensation.
Detected result is in table 1
The detected result of the resin of table 1 embodiment 1 to embodiment 4
Acrylate modified hydroxy-terminated polybutadienes resin of the present invention is obtained by hydroxy-terminated polybutadienes and acrylic ester copolymer, hydroxy-terminated polybutadienes in resin has Linear Double bond structure, and infrared transparent is good, and gloss is low, reflectivity is low, is desirable stealth material; Hydroxy-terminated polybutadienes by with acrylic ester copolymer modification, improve the weathering resistance of resin, can be used for the occasions such as outdoor; Because the strong primary hydroxyl of reactive behavior is contained at hydroxy-terminated polybutadienes molecule two ends, can with cured with isocyanates, after being made into polyurethane coating, the weathering resistance of the paint film that institute's application obtains, water tolerance, the more general polyurethane coating of salt fog resistance strengthen further, and the infrared stealth coating of preparation is better long-lasting; The polybutadiene configuration good toughness of long-chain in acrylate modified hydroxy-terminated polybutadienes resin of the present invention, mechanical property are superior, are desirable infrared stealth tackiness agents.
The acrylate modified hydroxy-terminated polybutadienes resinous luster of low infrared emissivity of the present invention is low, good weatherability, can be used for the infrared stealth coating preparing two component, for the application in the places such as military equipment, machinery, engineering and barracks, plays stealthy object.
Claims (10)
1. the acrylate modified hydroxy-terminated polybutadienes resin of a low infrared emissivity, it is characterized in that: by hydroxy-terminated polybutadienes and acrylate monomer and/or methacrylate monomer by free-radical polymerized acquisition, in free radicals copolymerization reaction, each raw material dosage is as follows: hydroxy-terminated polybutadienes 5wt% ~ 15wt%, acrylate monomer and/or methacrylate monomer 25wt% ~ 55wt%, solvent 35wt% ~ 65wt%, initiator 0.5wt% ~ 2wt%, the acrylate modified hydroxy-terminated polybutadienes resin solid content of the low infrared emissivity of gained is 40 ~ 60wt%.
2. the acrylate modified hydroxy-terminated polybutadienes resin of low infrared emissivity according to claim 1, is characterized in that: described hydroxy-terminated polybutadienes is the homopolymer of divinyl, and number-average molecular weight is 2000 ~ 3000; On average there is two or more hydroxyl at each macromole two ends.
3. the acrylate modified hydroxy-terminated polybutadienes resin of low infrared emissivity according to claim 1, is characterized in that: described acrylate monomer is one or more the composition in vinylformic acid, ethyl propenoate, butyl acrylate, Isooctyl acrylate monomer, glycidyl acrylate, isobornyl acrylate; Methacrylate monomer is one or more the composition in methyl methacrylate, butyl methacrylate, Propenoic acid, 2-methyl, isobutyl ester, isobornyl methacrylate.
4. the acrylate modified hydroxy-terminated polybutadienes resin of low infrared emissivity according to claim 3, is characterized in that: also comprise modified monomer, and modified monomer is tertiary carbonic acid glycidyl ester, tertiary ethylene carbonate or vinylbenzene; The mixture of modified monomer and acrylate monomer and/or methacrylate monomer and hydroxy-terminated polybutadienes react, and modified monomer and acrylate monomer and/or methacrylate monomer consumption account for the 25wt% ~ 55wt% reacting total consumption.
5. the acrylate modified hydroxy-terminated polybutadienes resin of low infrared emissivity according to claim 1, is characterized in that: described solvent is one or more the composition in varsol, ketones solvent, esters solvent, ether solvent, solvent of ether ester type.
6. the acrylate modified hydroxy-terminated polybutadienes resin of low infrared emissivity according to claim 1, it is characterized in that: described initiator is Diisopropyl azodicarboxylate, benzoyl peroxide, one or more the composition in peroxidized t-butyl perbenzoate or ditertiary butyl peroxide.
7. the preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of a low infrared emissivity as claimed in claim 1, it is characterized in that step is as follows: in reaction flask, add the part in hydroxy-terminated polybutadienes and solvent, stir, heating makes material in reaction flask be warming up to 80 DEG C ~ 130 DEG C; Then drip acrylate monomer and/or methacrylate monomer and the mixture of the part in initiator, dropwise in 3 ~ 5h, dropwising rear first time is incubated 1h; Insulation terminates the rear mixture continuing to drip residual solvent and residue initiator, and dropwise in 0.5 ~ 1h, cooling discharge be again incubated 2 ~ 3h at 80 DEG C ~ 130 DEG C after, obtains product.
8. the preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of low infrared emissivity according to claim 7, is characterized in that: the amount of the initiator that first time drips in reaction flask is for the second time to 1.8 ~ 2.5 times of dripping quantity in reaction flask.
9. the preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of low infrared emissivity according to claim 7, is characterized in that: the amount of the solvent that first time drips in reaction flask is for the second time to 4 ~ 11 times of dripping quantity in reaction flask.
10. the preparation method of the acrylate modified hydroxy-terminated polybutadienes resin of low infrared emissivity according to claim 7, it is characterized in that: after heating makes material in reaction flask be warming up to 80 DEG C ~ 130 DEG C, drip the mixture of the part in modified monomer and/or acrylate monomer and/or methacrylate monomer and initiator, dropwise in 3 ~ 5h;
Described modified monomer is tertiary carbonic acid glycidyl ester, tertiary ethylene carbonate or vinylbenzene;
Described acrylate monomer is one or more the composition in vinylformic acid, ethyl propenoate, butyl acrylate, Isooctyl acrylate monomer, glycidyl acrylate, isobornyl acrylate; Methacrylate monomer is one or more the composition in methyl methacrylate, butyl methacrylate, Propenoic acid, 2-methyl, isobutyl ester, isobornyl methacrylate.
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| CN113088153A (en) * | 2019-12-23 | 2021-07-09 | 万华化学集团股份有限公司 | Chlorinated polypropylene/acrylate hybrid aqueous dispersion and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113088153A (en) * | 2019-12-23 | 2021-07-09 | 万华化学集团股份有限公司 | Chlorinated polypropylene/acrylate hybrid aqueous dispersion and preparation method and application thereof |
| CN113088153B (en) * | 2019-12-23 | 2022-07-12 | 万华化学集团股份有限公司 | Chlorinated polypropylene/acrylate hybrid aqueous dispersion as well as preparation method and application thereof |
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