CN105273610A - Preparation method of nano-silica and tin antimony oxide-modified water-based nano transparent insulating paint - Google Patents
Preparation method of nano-silica and tin antimony oxide-modified water-based nano transparent insulating paint Download PDFInfo
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- CN105273610A CN105273610A CN201510739356.1A CN201510739356A CN105273610A CN 105273610 A CN105273610 A CN 105273610A CN 201510739356 A CN201510739356 A CN 201510739356A CN 105273610 A CN105273610 A CN 105273610A
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Abstract
The invention relates to a preparation method of nano-silica and antimony-doped tin oxide-modified water-based nano transparent insulating paint, which belongs to the technical field of high polymer materials. According to the preparation method, antimony-doped tin oxide nano powder and nano-silica liquid are modified to prepare transparent nano modified powder, and then the nano modified powder is used to modify urethane acrylate prepolymer, so as to prepare the transparent insulating paint. The preparation method has the beneficial effects that the nano-silica and antimony-doped tin oxide-modified water-based nano transparent insulating paint has small powder particle size and good insulating effect, the indoor and outdoor temperature difference is 8 to 9 DEG C, and additionally, the adhesion of the paint is increased by doping silicon, thereby increasing the adhesive force.
Description
Technical field
The present invention relates to a kind of preparation method of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope, belong to technical field of polymer materials.
Background technology
Nano transparent insulating coating is a kind of ceramic-like heat-insulation thermal-insulation water-based paint, adopts up-to-date composite ceramics heat-insulating technique and nanometer titanic oxide material, and design is used for reflecting luminous energy and radiant heat energy.The environmental protection composition of its uniqueness of nano transparent insulating coating---nano ATO liquid, titanium dioxide can remove the peculiar smell in surrounding environment, degradation of formaldehyde and other objectionable impuritiess.Nano transparent insulating coating is a kind of new coating, meets requirement and the characteristic of environmental protection coating material.
Transparent heat insulating dope in existing technology is all generally be prepared from by the mode that heat insulation nano material and different macromolecule film former (such as aqueous polyurethane, water polyacrylic acid) carry out physical blending.These co-mixing systems exist that nanoparticle dispersion is poor, poor stability and the problem of very easily reuniting, and cause the effect of heat insulation of coating poor, and the moulding property of water-based paint and poor adhesive force, in use energy consumption is high, is not suitable for industrialized production.
Summary of the invention
The technical problem that the present invention mainly solves: poor for nanoparticle dispersion in transparent heat insulating dope of the prior art, poor stability is very easily reunited, cause the effect of heat insulation of coating poor, provide a kind of preparation method of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope, the present invention is mainly prepared into transparent nano modified powder by antimony-doped tin oxide nano-powder and nano silicon liquid modifying, again by nano modification powder modification polyurethane acrylate prepolymer, prepare transparent heat insulating dope, nano-silicon dioxide modified antimony-doped tin oxide water nano transparent heat insulating dope diameter of particle prepared by the present invention is little, good heat-insulation effect, indoor/outdoor temperature-difference 8 ~ 9 DEG C, doped silicon makes the adhesion property of coating improve simultaneously, thus sticking power improves.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention:
(1) by antimony-doped tin oxide nano-powder and nano silicon liquid, by solid-liquid mass ratio 1:20, with the speed magnetic agitation 10 ~ 15min of 1200 ~ 1500r/min at temperature 20 ~ 30 DEG C, form nanometer mixed slurry, to be mixed mix after, mixed slurry is placed in the ultrasonic disperse instrument of 200 ~ 300W, ultrasonic disperse process 1 ~ 2h;
(2) mixed slurry after ultrasonic disperse is placed in the thermostat water bath of 25 ~ 30 DEG C, and by mixed slurry and vinyltriethoxysilane by volume 2:1 mix, carry out magnetic agitation 1 ~ 2h, to its modifying surface process, to be mixed complete after, continue to be heated to 45 ~ 50 DEG C to it, after secondary temperature elevation magnetic agitation 1 ~ 2h, stop heating and making it naturally cool to 20 ~ 30 DEG C, take out and be placed in separating centrifuge, centrifugal 10 ~ 15min under rotating speed 3000 ~ 5000r/min, collect lower sediment and pass through absolute ethanol washing 3 ~ 5 times, be placed on dry 10 ~ 12h in 80 ~ 90 DEG C of baking ovens, take out and it is milled and sieve, obtained 80 ~ 120 object modified Nano powder are for subsequent use,
(3) polyester polyol is chosen and isophorone diisocyanate is placed in 80 ~ 90 DEG C of baking ovens, dry 5 ~ 6h, count by weight subsequently, choose the glycol ether of the dried polyester polyol of 30 ~ 55 parts, the dried isophorone diisocyanate of 30 ~ 45 parts, the dibutyl tin laurate of 5 ~ 10 parts, the dimethylol propionic acid of 3 ~ 6 parts and 7 ~ 9 parts respectively, be uniformly mixed under 1200 ~ 1500r/min rotating speed, form polyurethane acrylate prepolymer mixed solution;
(4) the polyurethane acrylate prepolymer mixed solution of above-mentioned preparation is placed in 70 ~ 80 DEG C of water-baths and carries out reacting by heating, after question response 1 ~ 2h, by polyurethane acrylate prepolymer mixed solution and Propylene glycol monoacrylate mass ratio 20:1, Propylene glycol monoacrylate is slowly dropped in polyurethane acrylate prepolymer mixed solution, rate of addition is 2mL/min, after being added dropwise to complete, be 600 ~ 800mpas by acetone regulator solution viscosity, when stopping subsequently heating and making it naturally cool to 50 ~ 55 DEG C, its pH is regulated to be 7.0 by triethylamine, be prepared into polyurethane acrylate prepolymer,
(5) count by weight, choose the isophorone of 10 ~ 35 parts of above-mentioned obtained polyurethane acrylate prepolymers, the modified Nano powder that 50 ~ 60 parts of steps (2) are obtained, the diphenylethan of 5 ~ 10 parts, the sodium polyacrylate of 5 ~ 10 parts, the polyether silicone oil of 2 ~ 6 parts and 3 ~ 4 parts, compound 3 ~ 4h is stirred under 3000 ~ 4000rpm rotating speed, desolvation, make its standing and defoaming subsequently, obtain a kind of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope.
Application of the present invention: the constructional method a kind of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope of above-mentioned preparation being adopted spraying, is sprayed at transparent glass surface, and control thickness 5 ~ 15 μm, spray area is now about 15m
2/ kg, the ambient cure time is 40 ~ 48h, the nano transparent heat-insulating glass after spraying, and with the glass ratio not spraying nano transparent insulating coating, effect of heat insulation improves 5 ~ 7 DEG C, and transmittance improves 5 ~ 10%.
The invention has the beneficial effects as follows:
(1) fine paint powders particle diameter is little, good heat-insulation effect, indoor/outdoor temperature-difference 8 ~ 9 DEG C;
(2) doped silicon makes the adhesion property of coating improve, thus sticking power improves;
(3) preparation process is simple, and cost is low.
Embodiment
First by antimony-doped tin oxide nano-powder and nano silicon liquid, by solid-liquid mass ratio 1:20, with the speed magnetic agitation 10 ~ 15min of 1200 ~ 1500r/min at temperature 20 ~ 30 DEG C, form nanometer mixed slurry, to be mixed mix after, mixed slurry is placed in the ultrasonic disperse instrument of 200 ~ 300W, ultrasonic disperse process 1 ~ 2h, again the mixed slurry after ultrasonic disperse is placed in the thermostat water bath of 25 ~ 30 DEG C, and by mixed slurry and vinyltriethoxysilane by volume 2:1 mix, carry out magnetic agitation 1 ~ 2h, to its modifying surface process, to be mixed complete after, continue to be heated to 45 ~ 50 DEG C to it, after secondary temperature elevation magnetic agitation 1 ~ 2h, stop heating and making it naturally cool to 20 ~ 30 DEG C, take out and be placed in separating centrifuge, centrifugal 10 ~ 15min under rotating speed 3000 ~ 5000r/min, collect lower sediment and pass through absolute ethanol washing 3 ~ 5 times, be placed on dry 10 ~ 12h in 80 ~ 90 DEG C of baking ovens, take out and it is milled and sieve, obtained 80 ~ 120 object modified Nano powder are for subsequent use, choose polyester polyol and isophorone diisocyanate is placed in 80 ~ 90 DEG C of baking ovens, dry 5 ~ 6h, count by weight subsequently, choose the glycol ether of the dried polyester polyol of 30 ~ 55 parts, the dried isophorone diisocyanate of 30 ~ 45 parts, the dibutyl tin laurate of 5 ~ 10 parts, the dimethylol propionic acid of 3 ~ 6 parts and 7 ~ 9 parts respectively, be uniformly mixed under 1200 ~ 1500r/min rotating speed, form polyurethane acrylate prepolymer mixed solution, then the polyurethane acrylate prepolymer mixed solution of above-mentioned preparation is placed in 70 ~ 80 DEG C of water-baths and carries out reacting by heating, after question response 1 ~ 2h, by polyurethane acrylate prepolymer mixed solution and Propylene glycol monoacrylate mass ratio 20:1, Propylene glycol monoacrylate is slowly dropped in polyurethane acrylate prepolymer mixed solution, rate of addition is 2mL/min, after being added dropwise to complete, be 600 ~ 800mpas by acetone regulator solution viscosity, when stopping subsequently heating and making it naturally cool to 50 ~ 55 DEG C, its pH is regulated to be 7.0 by triethylamine, be prepared into polyurethane acrylate prepolymer, finally count by weight, choose the isophorone of 10 ~ 35 parts of above-mentioned obtained polyurethane acrylate prepolymers, 50 ~ 60 parts of obtained modified Nano powder, the diphenylethan of 5 ~ 10 parts, the sodium polyacrylate of 5 ~ 10 parts, the polyether silicone oil of 2 ~ 6 parts and 3 ~ 4 parts, compound 3 ~ 4h is stirred under 3000 ~ 4000rpm rotating speed, desolvation, make its standing and defoaming subsequently, be prepared into obtain a kind of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope.
Example 1
First by antimony-doped tin oxide nano-powder and nano silicon liquid, by solid-liquid mass ratio 1:20, with the speed magnetic agitation 15min of 1500r/min at temperature 30 DEG C, form nanometer mixed slurry, to be mixed mix after, mixed slurry is placed in the ultrasonic disperse instrument of 300W, ultrasonic disperse process 2h, again the mixed slurry after ultrasonic disperse is placed in the thermostat water bath of 30 DEG C, and by mixed slurry and vinyltriethoxysilane by volume 2:1 mix, carry out magnetic agitation 2h, to its modifying surface process, to be mixed complete after, continue to be heated to 50 DEG C to it, after secondary temperature elevation magnetic agitation 2h, stop heating and making it naturally cool to 30 DEG C, take out and be placed in separating centrifuge, centrifugal 15min under rotating speed 5000r/min, collect lower sediment and pass through absolute ethanol washing 5 times, be placed on dry 12h in 90 DEG C of baking ovens, take out and it is milled and sieve, obtained 120 object modified Nano powder are for subsequent use, choose polyester polyol and isophorone diisocyanate is placed in 90 DEG C of baking ovens, dry 6h, count by weight subsequently, choose the glycol ether of the dried polyester polyol of 55 parts, the dried isophorone diisocyanate of 30 parts, the dibutyl tin laurate of 5 parts, the dimethylol propionic acid of 3 parts and 7 parts respectively, be uniformly mixed under 1200r/min rotating speed, form polyurethane acrylate prepolymer mixed solution, then the polyurethane acrylate prepolymer mixed solution of above-mentioned preparation is placed in 80 DEG C of water-baths and carries out reacting by heating, after question response 2h, by polyurethane acrylate prepolymer mixed solution and Propylene glycol monoacrylate mass ratio 20:1, Propylene glycol monoacrylate is slowly dropped in polyurethane acrylate prepolymer mixed solution, rate of addition is 2mL/min, after being added dropwise to complete, be 800mpas by acetone regulator solution viscosity, when stopping subsequently heating and making it naturally cool to 55 DEG C, regulate its pH to be 7.0 by triethylamine, be prepared into polyurethane acrylate prepolymer, finally count by weight, choose the isophorone of 35 parts of above-mentioned obtained polyurethane acrylate prepolymers, 50 parts of modified Nano powder, the diphenylethan of 5 parts, the sodium polyacrylate of 5 parts, the polyether silicone oil of 2 parts and 3 parts, compound 4h is stirred under 4000rpm rotating speed, desolvation, make its standing and defoaming subsequently, be prepared into obtain a kind of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope.A kind of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope of above-mentioned preparation is adopted the constructional method of spraying, be sprayed at transparent glass surface, control thickness 15 μm, spray area is now about 15m
2/ kg, the ambient cure time is 48h, the nano transparent heat-insulating glass after spraying, and with the glass ratio not spraying nano transparent insulating coating, effect of heat insulation improves 7 DEG C, and transmittance improves 10%.
Example 2
First by antimony-doped tin oxide nano-powder and nano silicon liquid, by solid-liquid mass ratio 1:20, with the speed magnetic agitation 10min of 1200r/min at temperature 20 DEG C, form nanometer mixed slurry, to be mixed mix after, mixed slurry is placed in the ultrasonic disperse instrument of 200W, ultrasonic disperse process 1h, again the mixed slurry after ultrasonic disperse is placed in the thermostat water bath of 25 DEG C, and by mixed slurry and vinyltriethoxysilane by volume 2:1 mix, carry out magnetic agitation 1h, to its modifying surface process, to be mixed complete after, continue to be heated to 45 DEG C to it, after secondary temperature elevation magnetic agitation 1h, stop heating and making it naturally cool to 20 DEG C, take out and be placed in separating centrifuge, centrifugal 10min under rotating speed 3000r/min, collect lower sediment and pass through absolute ethanol washing 3 times, be placed on dry 10h in 80 DEG C of baking ovens, take out and it is milled and sieve, obtained 80 object modified Nano powder are for subsequent use, choose polyester polyol and isophorone diisocyanate is placed in 80 DEG C of baking ovens, dry 5h, count by weight subsequently, choose the glycol ether of the dried polyester polyol of 30 parts, the dried isophorone diisocyanate of 45 parts, the dibutyl tin laurate of 10 parts, the dimethylol propionic acid of 6 parts and 9 parts respectively, be uniformly mixed under 1200r/min rotating speed, form polyurethane acrylate prepolymer mixed solution, then the polyurethane acrylate prepolymer mixed solution of above-mentioned preparation is placed in 70 DEG C of water-baths and carries out reacting by heating, after question response 1h, by polyurethane acrylate prepolymer mixed solution and Propylene glycol monoacrylate mass ratio 20:1, Propylene glycol monoacrylate is slowly dropped in polyurethane acrylate prepolymer mixed solution, rate of addition is 2mL/min, after being added dropwise to complete, be 600mpas by acetone regulator solution viscosity, when stopping subsequently heating and making it naturally cool to 50 DEG C, regulate its pH to be 7.0 by triethylamine, be prepared into polyurethane acrylate prepolymer, finally count by weight, choose the isophorone of 10 parts of above-mentioned obtained polyurethane acrylate prepolymers, 60 parts of modified Nano powder, the diphenylethan of 10 parts, the sodium polyacrylate of 10 parts, the polyether silicone oil of 6 parts and 4 parts, compound 3h is stirred under 3000pm rotating speed, desolvation, make its standing and defoaming subsequently, be prepared into obtain a kind of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope.A kind of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope of above-mentioned preparation is adopted the constructional method of spraying, be sprayed at transparent glass surface, control thickness 5 μm, spray area is now about 15m
2/ kg, the ambient cure time is 40h, the nano transparent heat-insulating glass after spraying, and with the glass ratio not spraying nano transparent insulating coating, effect of heat insulation improves 5 DEG C, and transmittance improves 5%.
Example 3
First by antimony-doped tin oxide nano-powder and nano silicon liquid, by solid-liquid mass ratio 1:20, with the speed magnetic agitation 12min of 1300r/min at temperature 25 DEG C, form nanometer mixed slurry, to be mixed mix after, mixed slurry is placed in the ultrasonic disperse instrument of 250W, ultrasonic disperse process 1h, again the mixed slurry after ultrasonic disperse is placed in the thermostat water bath of 27 DEG C, and by mixed slurry and vinyltriethoxysilane by volume 2:1 mix, carry out magnetic agitation 1h, to its modifying surface process, to be mixed complete after, continue to be heated to 47 DEG C to it, after secondary temperature elevation magnetic agitation 1h, stop heating and making it naturally cool to 25 DEG C, take out and be placed in separating centrifuge, centrifugal 12min under rotating speed 4000r/min, collect lower sediment and pass through absolute ethanol washing 4 times, be placed on dry 11h in 85 DEG C of baking ovens, take out and it is milled and sieve, obtained 100 object modified Nano powder are for subsequent use, choose polyester polyol and isophorone diisocyanate is placed in 85 DEG C of baking ovens, dry 5h, count by weight subsequently, choose the glycol ether of the dried polyester polyol of 40 parts, the dried isophorone diisocyanate of 40 parts, the dibutyl tin laurate of 7 parts, the dimethylol propionic acid of 4 parts and 9 parts respectively, be uniformly mixed under 1400r/min rotating speed, form polyurethane acrylate prepolymer mixed solution, then the polyurethane acrylate prepolymer mixed solution of above-mentioned preparation is placed in 75 DEG C of water-baths and carries out reacting by heating, after question response 1h, by polyurethane acrylate prepolymer mixed solution and Propylene glycol monoacrylate mass ratio 20:1, Propylene glycol monoacrylate is slowly dropped in polyurethane acrylate prepolymer mixed solution, rate of addition is 2mL/min, after being added dropwise to complete, be 700mpas by acetone regulator solution viscosity, when stopping subsequently heating and making it naturally cool to 52 DEG C, regulate its pH to be 7.0 by triethylamine, be prepared into polyurethane acrylate prepolymer, finally count by weight, choose the isophorone of 20 parts of above-mentioned obtained polyurethane acrylate prepolymers, 60 parts of modified Nano powder, the diphenylethan of 5 parts, the sodium polyacrylate of 5 parts, the polyether silicone oil of 6 parts and 4 parts, compound 3h is stirred under 3500rpm rotating speed, desolvation, make its standing and defoaming subsequently, be prepared into obtain a kind of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope.A kind of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope of above-mentioned preparation is adopted the constructional method of spraying, be sprayed at transparent glass surface, control thickness 10 μm, spray area is now about 15m
2/ kg, the ambient cure time is 42h, the nano transparent heat-insulating glass after spraying, and with the glass ratio not spraying nano transparent insulating coating, effect of heat insulation improves 6 DEG C, and transmittance improves 7%.
Claims (1)
1. a preparation method for nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope, is characterized in that concrete preparation process is:
(1) by antimony-doped tin oxide nano-powder and nano silicon liquid, by solid-liquid mass ratio 1:20, with the speed magnetic agitation 10 ~ 15min of 1200 ~ 1500r/min at temperature 20 ~ 30 DEG C, form nanometer mixed slurry, to be mixed mix after, mixed slurry is placed in the ultrasonic disperse instrument of 200 ~ 300W, ultrasonic disperse process 1 ~ 2h;
(2) mixed slurry after ultrasonic disperse is placed in the thermostat water bath of 25 ~ 30 DEG C, and by mixed slurry and vinyltriethoxysilane by volume 2:1 mix, carry out magnetic agitation 1 ~ 2h, to its modifying surface process, to be mixed complete after, continue to be heated to 45 ~ 50 DEG C to it, after secondary temperature elevation magnetic agitation 1 ~ 2h, stop heating and making it naturally cool to 20 ~ 30 DEG C, take out and be placed in separating centrifuge, centrifugal 10 ~ 15min under rotating speed 3000 ~ 5000r/min, collect lower sediment and pass through absolute ethanol washing 3 ~ 5 times, be placed on dry 10 ~ 12h in 80 ~ 90 DEG C of baking ovens, take out and it is milled and sieve, obtained 80 ~ 120 object modified Nano powder are for subsequent use,
(3) polyester polyol is chosen and isophorone diisocyanate is placed in 80 ~ 90 DEG C of baking ovens, dry 5 ~ 6h, count by weight subsequently, choose the glycol ether of the dried polyester polyol of 30 ~ 55 parts, the dried isophorone diisocyanate of 30 ~ 45 parts, the dibutyl tin laurate of 5 ~ 10 parts, the dimethylol propionic acid of 3 ~ 6 parts and 7 ~ 9 parts respectively, be uniformly mixed under 1200 ~ 1500r/min rotating speed, form polyurethane acrylate prepolymer mixed solution;
(4) the polyurethane acrylate prepolymer mixed solution of above-mentioned preparation is placed in 70 ~ 80 DEG C of water-baths and carries out reacting by heating, after question response 1 ~ 2h, by polyurethane acrylate prepolymer mixed solution and Propylene glycol monoacrylate mass ratio 20:1, Propylene glycol monoacrylate is slowly dropped in polyurethane acrylate prepolymer mixed solution, rate of addition is 2mL/min, after being added dropwise to complete, be 600 ~ 800mpas by acetone regulator solution viscosity, when stopping subsequently heating and making it naturally cool to 50 ~ 55 DEG C, its pH is regulated to be 7.0 by triethylamine, be prepared into polyurethane acrylate prepolymer,
(5) count by weight, choose the isophorone of 10 ~ 35 parts of above-mentioned obtained polyurethane acrylate prepolymers, the modified Nano powder that 50 ~ 60 parts of steps (2) are obtained, the diphenylethan of 5 ~ 10 parts, the sodium polyacrylate of 5 ~ 10 parts, the polyether silicone oil of 2 ~ 6 parts and 3 ~ 4 parts, compound 3 ~ 4h is stirred under 3000 ~ 4000rpm rotating speed, desolvation, make its standing and defoaming subsequently, obtain a kind of nano-silicon dioxide modified tin-antiomony oxide water nano transparent heat insulating dope.
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| CN201510739356.1A CN105273610A (en) | 2015-11-04 | 2015-11-04 | Preparation method of nano-silica and tin antimony oxide-modified water-based nano transparent insulating paint |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106189365A (en) * | 2016-07-15 | 2016-12-07 | 深圳大学 | Modified Fxmnysn(1 x y)o2nano-powder and the preparation method of modified aqueous polyurethane emulsion |
| CN106366903A (en) * | 2016-10-09 | 2017-02-01 | 常州亚环环保科技有限公司 | Preparation method of high-leveling-property transparent glass heat insulation coating |
| CN112694814A (en) * | 2020-12-23 | 2021-04-23 | 深圳市深赛尔股份有限公司 | Water-based paint for color steel plate and preparation method thereof |
-
2015
- 2015-11-04 CN CN201510739356.1A patent/CN105273610A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106189365A (en) * | 2016-07-15 | 2016-12-07 | 深圳大学 | Modified Fxmnysn(1 x y)o2nano-powder and the preparation method of modified aqueous polyurethane emulsion |
| CN106189365B (en) * | 2016-07-15 | 2018-06-22 | 深圳大学 | Modified FxMnySn(1-x-y)O2The preparation method of nano-powder and modified aqueous polyurethane emulsion |
| CN106366903A (en) * | 2016-10-09 | 2017-02-01 | 常州亚环环保科技有限公司 | Preparation method of high-leveling-property transparent glass heat insulation coating |
| CN112694814A (en) * | 2020-12-23 | 2021-04-23 | 深圳市深赛尔股份有限公司 | Water-based paint for color steel plate and preparation method thereof |
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Application publication date: 20160127 |