CN102559025A - Preparation method for high-performance transparent glass heat-insulating coating - Google Patents

Preparation method for high-performance transparent glass heat-insulating coating Download PDF

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Publication number
CN102559025A
CN102559025A CN2011103673122A CN201110367312A CN102559025A CN 102559025 A CN102559025 A CN 102559025A CN 2011103673122 A CN2011103673122 A CN 2011103673122A CN 201110367312 A CN201110367312 A CN 201110367312A CN 102559025 A CN102559025 A CN 102559025A
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performance
transparent glass
heat
preparation
insulating coating
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CN2011103673122A
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CN102559025B (en
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李佳怡
李学成
郑爱玉
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Shanghai Shanghai Industrial Co., Ltd.
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SHANGHAI HUZHENG NANO-TECH Co Ltd
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Abstract

The invention discloses a preparation method for a high-performance transparent glass heat-insulating coating, comprising the following steps of: preparing a novel high-performance transparent mixed nano-slurry mixed and dispersed by blue WO3 (tungsten trioxide), ATO (antimony tin oxide) and ITO (indium tin oxide) at first, and then mixing, stirring and filtering by transparent polyurethane resin to obtain the transparent glass heat-insulating coating with high heat-insulating performance. The high-performance transparent glass heat-insulating coating prepared by the method disclosed by the invention has super-strong transparency, heat insulation and ultraviolet-preventing performance, and especially has very high heat-insulating performance in a near-infrared area ranging from 780 to 900 nm; and the high-performance transparent glass heat-insulating coating can be widely applied to production for high-performance heat-insulating glass and high-performance heat-insulating window membrane, as well as has very important social and economic values.

Description

The preparation method of high-performance insulating mold coating of transparent glass
Technical field
The present invention relates to a kind of preparation method of high-performance insulating mold coating of transparent glass.
Background technology
The insulating mold coating of transparent glass of producing at present both at home and abroad has a variety of forms, and water-based is arranged, and the insulating mold coating of transparent glass of solvent borne is also arranged; But the heat insulation medium that is to use all is to be unable to do without ATO nano pulp and ITO nano pulp, and is similar, just adds on the amount of ATO, ITO nano pulp variant; Used resin system is different; Therefore, though the formula combination of which type of glass heat-insulating coating, under the situation that limits paint coatings thickness; To the influence of optical property, all can not have greatly improved.This is because coating uses the characteristic of nano heat-insulating medium A TO, ITO material itself to determine.If just adopting single ATO, ITO is heat insulation medium; Or just the nano pulp of ATO, ITO blending dispersion gained; The glass heat-insulating coating of being done requires to limit visible light transmissivity greater than 70%, under the thicknesses of layers 3um situation; Rejection rate to IR can not be greater than 70% near 900nm at light wave, the use defect problem of some nano material that Here it is.Therefore, research is explored can satisfy the high-performance glass thermal insulating coating that high transparent can be realized high heat-proof quality again near infrared region, has the very urgent market requirement.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of high-performance glass thermal insulating coating of high transparent, the high thermal insulation that can improve the glass heat-proof performance.Preparing method of the present invention is simple, low production cost, helps scale operation.
In order to solve the problems of the technologies described above, the preparation method of high-performance insulating mold coating of transparent glass provided by the invention comprises following process step:
Take by weighing primary particle size by weight 1: 1: 1 respectively and be not more than the blue nanometer WO of 40nm 3Powder, primary particle size are not more than the blue nano ATO powder of 10nm and three kinds of nano-powders of blue nano-ITO powder that primary particle size is not more than 20nm and put into the quick dispersion machine of planet; Add an amount of water-based/oil-based solvent and water-based/oiliness dispersion agent; Adding an amount of diameter again is the zirconium ball of 0.2-0.4mm; Be that continuous high speed disperseed 14-18 hour, made the nanometer mixed slurry under 11000-13000 rev/min the condition at rotating speed;
Take by weighing the water-based/oil-based solvent of the nanometer mixed slurry of 20-50 weight part, the water-based of 50-80 weight part/oiliness transparent polyurethane resin and 0-30 weight part, add in the container, stir, cross 200 purpose filter screens, make the high-performance insulating mold coating of transparent glass.
Preferably, among the preparation method of the above-mentioned high-performance insulating mold coating of transparent glass of the present invention, aqueous dispersant is separated into N, and N-dimethylethanolamine, oiliness dispersion agent are HSDB 338.
Preferably, among the preparation method of the above-mentioned high-performance insulating mold coating of transparent glass of the present invention, aqueous solvent is a deionized water, and oil-based solvent is a N-BUTYL ACETATE.
Among the present invention, primary particle size is not more than the blue nano ATO powder of 10nm and blue nano-ITO powder that primary particle size is not more than 20nm all adopts usual method to be prepared from.For example, the primary particle size blue nano ATO powder that is not more than 10nm can adopt the preparation of Chinese patent CN101597022A disclosed method; The blue nano-ITO powder that primary particle size is not more than 20nm can adopt the preparation of Chinese patent CN1775693A disclosed method.
Among the present invention, primary particle size is not more than the blue nanometer WO of 40nm 3The preparation of powder comprises the steps:
1. in high speed sand milling dispersion machine, pour wolframic acid, purity into and be 99.9 In (OH) 3Powder and mixed solvent, this mixed solvent are the mixed solution of 1: 1 first alcohol and water of weight ratio, wolframic acid, In (OH) 3The consumption of powder and mixed solvent is respectively: wolframic acid 40-60 weight part, In (OH) 3Powder 2-8 weight part, mixed solvent 40-55 weight part; Use N, the N-dimethylethanolamine transfers to 5-5.5 to the pH value in the system; Be that the high speed sand milling disperseed 4-6 hour under 12000-14000 rev/min the condition at rotating speed;
2. the material that 1. obtains of step is poured AL into 2O 3In the crucible, putting into drying baker oven dry back and take out, in the drying course, is oven dry after 5-7 hour under 85-95 ℃ the condition in temperature, in temperature is to dry 4-8 hour under 160-200 ℃ the condition again.
3. the material that 2. obtains of step is processed into meal with kibbler earlier, is processed into ultrafine powder with the air-flow dispersion machine again; This ultrafine powder makes the blue transparent heat-insulated WO below the primary particle size 40nm after dropping into the retort furnace calcining 3Nano-powder, wherein, calcining temperature is 600-650 ℃, and calcination time is 5-7 hour, charges into nitrogen protection in the calcination process, and the nitrogen amount of charging into is 15-25m 3/ min.
Embodiment subsequently will prove, the high-performance insulating mold coating of transparent glass that the inventive method makes, and wavelength is in the 380nm-900nm zone; During coating rete 3um, the IR rejection rate is greater than 90%, and visible light transmissivity VLT is greater than 75%; Have high heat-proof quality and high transparent, can be widely used in building, vehicle glass sun-proof energy-conservation; Improve people's life, improve energy-saving efficiency and have great importance.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.These embodiment are interpreted as only being used to the present invention is described and are not used in restriction protection scope of the present invention.After the content of having read the present invention's record, those skilled in the art can do various changes or modification to the present invention, and these equivalences change and modify and fall into claim of the present invention institute restricted portion equally.
(the preparation primary particle size is not more than the blue nanometer WO of 40nm to embodiment 1.1 3Powder)
Get 1. 50 weight part content successively respectively and be 99.9% wolframic acid (H 2WO 4); Get 2. 5 weight part content and be 99.9% indium hydroxide In (OH) 3Powder; Get 3. 45 weight part methyl alcohol and 1: 1 mixed solvent of deionized water, 1. 2. 3. pouring into successively in the ready prepd high speed sand milling dispersion machine, rotating speed is transferred to 12000 rev/mins; After spending 30 minutes; Use N, the pH value of colloid mixture begins high speed dispersion after pH value controls to 5 in the N one dimethylethanolamine adjustment high speed sand milling dispersion machine; Disperse after 4 hours continuously, the colloid mixture that takes out again in the high speed sand milling dispersion machine is poured Al into 2O 3Crucible is put into the drying baker oven dry again, and temperature is transferred to 85 degree oven dry 5 hours; Increase 160 degree 4 hours to temperature again; After cooling off, put into the retort furnace calcining again, temperature is controlled at 600 degree, connects nitrogen in the retort furnace; Nitrogen flow is adjusted to 15 cubic meters per minute, controls to heat-up time to open the retort furnace lid after 5 hours behind the naturally cooling and take out powder and can obtain the blue transparent heat-insulated WO of primary particle size less than 40 nanometers with air-flow dispersion machine super-fine processing again with kibbler roughing earlier 3Nano-powder.
Embodiment 1.2
☆ prepares the heat insulation medium of water-based high-performance (mixing nano pulp A component to call in the following text)
Take by weighing primary particle size that 1. embodiment 1.1 makes and be not more than the blue nanometer WO of 40nm 3Powder 1300g;
Take by weighing 2. primary particle size and be not more than the blue nano ATO powder 1300g of 10nm;
Take by weighing 3. primary particle size and be not more than the blue nano-ITO powder 1300g of 20nm;
Take by weighing 4. deionized water 4900g;
Take by weighing 5. water-based system dispersion agent N, N-dimethylethanolamine 200g.
Be equipped with in the dispersion bucket of the quick dispersion machine of planet that diameter is a 0.3mm zirconium ball 1. 2. 3. 4. 5. pouring into successively; Adjust to 12000 rev/mins to rotating speed; Disperseing continuously to open after 16 hours disperses bung; Take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, the acquisition solid content is 49% mixing nano pulp A component.
★ prepares the heat insulation medium of N-BUTYL ACETATE class oiliness high-performance (mixing nano pulp B component to call in the following text)
Take by weighing primary particle size that 1. embodiment 1.1 makes and be not more than the blue nanometer WO of 40nm 3Powder 1300g;
Take by weighing 2. primary particle size and be not more than the blue nano ATO powder 1300g of 10nm;
Take by weighing 3. primary particle size and be not more than the blue nano-ITO powder 1300g of 20nm;
Take by weighing 4. solvent butyl acetate 4900g;
Take by weighing 5. oiliness system dispersion agent HSDB 338 200g.
Be equipped with in the dispersion bucket of the quick dispersion machine of planet that diameter is a 0.3mm zirconium ball 1. 2. 3. 4. 5. pouring into successively; Adjust to 12000 rev/mins to rotating speed; Disperseing continuously to open after 16 hours disperses bung; Take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, the acquisition solid content is 49% mixing nano pulp B component.
Embodiment 2 (preparation water-based high-performance glass thermal insulating coating)
Take by weighing the mixing nano pulp A component 20g of embodiment 1.2 preparations;
Take by weighing aqueous transparent urethane resin 80g;
Pour in the container with the aqueous transparent urethane resin and stirred 20 minutes mixing nano pulp A component,, promptly get water-based high-performance glass thermal insulating coating with the filtration of 200 order filter cloths.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build was adjusted to 3um during coating, it was following to record the result with spectral instrument: IR rejection rate 91%; UV rejection rate 80%; VLT transmitance 76%.
Embodiment 3 (preparation oiliness high-performance glass thermal insulating coating)
Take by weighing the mixing nano pulp B component 20g of preparation among the embodiment 1.2;
Take by weighing oiliness transparent polyurethane resin 60g;
Take by weighing oil-based solvent N-BUTYL ACETATE 20g;
Pour into successively in the container and stirred 20 minutes mixing nano pulp B component, oiliness transparent polyurethane resin and oil-based solvent N-BUTYL ACETATE,, promptly get oiliness high-performance glass thermal insulating coating with the filtration of 200 order filter cloths.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build was adjusted to 3um during coating, it was following to record the result with spectral instrument: IR rejection rate 90%; UV rejection rate 79%; VLT transmitance 77%.
Embodiment 4 (preparation water-based high-performance glass thermal insulating coating)
Get the mixing nano pulp A component 30g of preparation among the embodiment 1.2;
Take by weighing aqueous transparent urethane resin 70g;
Pour in the container with the aqueous transparent urethane resin and stirred 20 minutes mixing nano pulp A component,, promptly get water-based high-performance glass thermal insulating coating of the present invention with the filtration of 200 order filter cloths.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build was adjusted to 3um during coating, it was following to record the result with spectral instrument: IR rejection rate 93%; UV rejection rate 82%; VLT transmitance 76%.
Embodiment 5 (preparation oiliness high-performance glass thermal insulating coating)
Take by weighing the prepared mixing nano pulp B component 30g of the foregoing description 1.2;
Take by weighing oiliness transparent polyurethane resin 50g;
Take by weighing oil-based solvent N-BUTYL ACETATE 20g;
Pour into successively in the container and stirred 20 minutes mixing nano pulp B component, oiliness transparent polyurethane resin and oil-based solvent N-BUTYL ACETATE,, promptly get oiliness high-performance glass thermal insulating coating with the filtration of 200 order filter cloths.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build was adjusted to 3um during coating, it was following to record the result with spectral instrument: IR rejection rate 92%; UV rejection rate 80%; VLT transmitance 76%.
Embodiment 6 (preparation water-based high-performance glass thermal insulating coating)
Take by weighing the mixing nano pulp A component 40g of the foregoing description 1.2 preparations;
Take by weighing aqueous transparent urethane resin 60g;
Pour in the container with the aqueous transparent urethane resin and stirred 20 minutes mixing nano pulp A component,, promptly get water-based high-performance glass thermal insulating coating of the present invention with the filtration of 200 order filter cloths.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build was adjusted to 3um during coating, it was following to record the result with spectral instrument: IR rejection rate 94%; UV rejection rate 83%; VLT transmitance 75%.
Embodiment 7 (preparation oiliness high-performance glass thermal insulating coating)
Take by weighing the prepared mixing nano pulp B component 40g of the foregoing description 1.2;
Take by weighing oiliness transparent polyurethane resin 50g;
Take by weighing oil-based solvent N-BUTYL ACETATE 10g;
Pour into successively in the container and stirred 20 minutes mixing nano pulp B component, oiliness transparent polyurethane resin and oil-based solvent N-BUTYL ACETATE,, promptly get oiliness high-performance glass thermal insulating coating with the filtration of 200 order filter cloths.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build was adjusted to 3um during coating, it was following to record the result with spectral instrument: IR rejection rate 93%; UV rejection rate 81%; VLT transmitance 75%.
Embodiment 8 (preparation water-based high-performance glass thermal insulating coating)
Take by weighing the mixing nano pulp A component 40g of the foregoing description 1.2 preparations;
Take by weighing aqueous transparent urethane resin 60g;
Pour in the container with the aqueous transparent urethane resin and stirred 20 minutes mixing nano pulp A component,, promptly get water-based high-performance glass thermal insulating coating with the filtration of 200 order filter cloths.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build was adjusted to 3um during coating, it was following to record the result with spectral instrument: IR rejection rate 94%; UV rejection rate 83%; VLT transmitance 75%.
Embodiment 9 (preparation oiliness high-performance glass thermal insulating coating)
Take by weighing the prepared mixing nano pulp B component 40g of the foregoing description 1.2;
Take by weighing oiliness transparent polyurethane resin 50g;
Take by weighing oil-based solvent N-BUTYL ACETATE 10g;
Pour into successively in the container and stirred 20 minutes mixing nano pulp B component, oiliness transparent polyurethane resin and oil-based solvent N-BUTYL ACETATE,, promptly get oiliness high-performance glass thermal insulating coating with the filtration of 200 order filter cloths.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build was adjusted to 3um during coating, it was following to record the result with spectral instrument: IR rejection rate 93%; UV rejection rate 81%; VLT transmitance 75%.

Claims (3)

1. the preparation method of a high-performance insulating mold coating of transparent glass is characterized in that, comprises following process step:
Take by weighing primary particle size by weight 1: 1: 1 respectively and be not more than the blue nanometer WO of 40nm 3Powder, primary particle size are not more than the blue nano ATO powder of 10nm and three kinds of nano-powders of blue nano-ITO powder that primary particle size is not more than 20nm and put into the quick dispersion machine of planet; Add an amount of water-based/oil-based solvent and water-based/oiliness dispersion agent; Adding an amount of diameter again is the zirconium ball of 0.2-0.4mm; Be that continuous high speed disperseed 14-18 hour, made the nanometer mixed slurry under 11000-13000 rev/min the condition at rotating speed;
Take by weighing the water-based/oil-based solvent of the nanometer mixed slurry of 20-50 weight part, the water-based of 50-80 weight part/oiliness transparent polyurethane resin and 0-30 weight part, add in the container, stir, cross 200 purpose filter screens, make the high-performance insulating mold coating of transparent glass.
2. the preparation method of high-performance insulating mold coating of transparent glass according to claim 1 is characterized in that aqueous dispersant is separated into N, and N-dimethylethanolamine, oiliness dispersion agent are HSDB 338.
3. the preparation method of high-performance insulating mold coating of transparent glass according to claim 1 is characterized in that, aqueous solvent is a deionized water, and oil-based solvent is a N-BUTYL ACETATE.
CN 201110367312 2011-11-18 2011-11-18 Preparation method for high-performance transparent glass heat-insulating coating Active CN102559025B (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732144A (en) * 2012-07-16 2012-10-17 惠州市彩田化工实业有限公司 Aqueous UV (Ultraviolet) photo-curing full-shielding nano transparent heat-insulating coating
CN102732108A (en) * 2012-07-16 2012-10-17 惠州市彩田化工实业有限公司 Aqueous self-cleaning transparent heat-insulated nano-dope capable of fully shielding infrared ray and ultraviolet ray
CN102732138A (en) * 2012-07-16 2012-10-17 惠州市彩田化工实业有限公司 Alkyd resin nanometer transparent heat-insulating coating capable of shielding infrared and ultraviolet full-wave bands
CN102746781A (en) * 2012-07-16 2012-10-24 惠州市彩田化工实业有限公司 Full-shielded infrared and ultraviolet polyurethane nanometer transparent heat insulating coating
CN104861762A (en) * 2015-05-26 2015-08-26 湖南省华京粉体材料有限公司 Transparent glass thermal insulation material and application thereof
CN106079764A (en) * 2016-06-24 2016-11-09 海安浩驰科技有限公司 Fenestrated membrane and processing technology thereof
CN106146894A (en) * 2015-03-23 2016-11-23 李佳怡 A kind of preparation method of the high transparent hot phase-change material of high thermal insulation
CN106497200A (en) * 2016-11-09 2017-03-15 深圳市兆新能源股份有限公司 Heat-insulating slurry and preparation method thereof and water-borne heat-insulating glass coating and preparation method thereof
CN109216548A (en) * 2018-10-22 2019-01-15 东莞理工学院 A kind of perovskite solar battery scrapes coating preparation method
CN112029402A (en) * 2020-09-11 2020-12-04 湖南尚鑫新材料科技有限公司 Heat insulation coating composition
CN112029431A (en) * 2020-09-11 2020-12-04 湖南尚鑫新材料科技有限公司 Heat-insulating explosion-proof film for automobile front windshield glass

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WO2010092991A1 (en) * 2009-02-13 2010-08-19 旭硝子株式会社 Coating composition for the formation of hydrophilic film
CN101993657A (en) * 2009-08-14 2011-03-30 北京建筑技术发展有限责任公司 Intelligent nano transparent insulating glass coating

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CN1997712A (en) * 2004-08-13 2007-07-11 李海旭 Composition for functional coatings, film formed therefrom and method for forming the composition and the film
WO2010092991A1 (en) * 2009-02-13 2010-08-19 旭硝子株式会社 Coating composition for the formation of hydrophilic film
CN101993657A (en) * 2009-08-14 2011-03-30 北京建筑技术发展有限责任公司 Intelligent nano transparent insulating glass coating

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732144B (en) * 2012-07-16 2016-05-25 惠州市彩田化工实业有限公司 A kind of water-based ultraviolet (UV) curable full-shield nano transparent insulating coating
CN102732108B (en) * 2012-07-16 2015-04-08 惠州市彩田化工实业有限公司 Aqueous self-cleaning transparent heat-insulated nano-dope capable of fully shielding infrared ray and ultraviolet ray
CN102732144A (en) * 2012-07-16 2012-10-17 惠州市彩田化工实业有限公司 Aqueous UV (Ultraviolet) photo-curing full-shielding nano transparent heat-insulating coating
CN102746781A (en) * 2012-07-16 2012-10-24 惠州市彩田化工实业有限公司 Full-shielded infrared and ultraviolet polyurethane nanometer transparent heat insulating coating
CN102732138B (en) * 2012-07-16 2016-01-27 惠州市彩田化工实业有限公司 One shields the infrared and full wave Synolac nano transparent insulating coating of ultraviolet
CN102746781B (en) * 2012-07-16 2015-04-22 惠州市彩田化工实业有限公司 Full-shielded infrared and ultraviolet polyurethane nanometer transparent heat insulating coating
CN102732108A (en) * 2012-07-16 2012-10-17 惠州市彩田化工实业有限公司 Aqueous self-cleaning transparent heat-insulated nano-dope capable of fully shielding infrared ray and ultraviolet ray
CN102732138A (en) * 2012-07-16 2012-10-17 惠州市彩田化工实业有限公司 Alkyd resin nanometer transparent heat-insulating coating capable of shielding infrared and ultraviolet full-wave bands
CN106146894A (en) * 2015-03-23 2016-11-23 李佳怡 A kind of preparation method of the high transparent hot phase-change material of high thermal insulation
CN106146894B (en) * 2015-03-23 2018-07-10 李佳怡 A kind of preparation method of the hot phase-change material of the high thermal insulation of high transparency
CN104861762A (en) * 2015-05-26 2015-08-26 湖南省华京粉体材料有限公司 Transparent glass thermal insulation material and application thereof
CN104861762B (en) * 2015-05-26 2017-07-25 湖南省华京粉体材料有限公司 A kind of clear glass heat-barrier material and its application
CN106079764A (en) * 2016-06-24 2016-11-09 海安浩驰科技有限公司 Fenestrated membrane and processing technology thereof
CN106497200A (en) * 2016-11-09 2017-03-15 深圳市兆新能源股份有限公司 Heat-insulating slurry and preparation method thereof and water-borne heat-insulating glass coating and preparation method thereof
CN109216548A (en) * 2018-10-22 2019-01-15 东莞理工学院 A kind of perovskite solar battery scrapes coating preparation method
CN112029402A (en) * 2020-09-11 2020-12-04 湖南尚鑫新材料科技有限公司 Heat insulation coating composition
CN112029431A (en) * 2020-09-11 2020-12-04 湖南尚鑫新材料科技有限公司 Heat-insulating explosion-proof film for automobile front windshield glass

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