CN103122155A - Preparation method of high-performance window film insulation medium - Google Patents
Preparation method of high-performance window film insulation medium Download PDFInfo
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- CN103122155A CN103122155A CN2011103673137A CN201110367313A CN103122155A CN 103122155 A CN103122155 A CN 103122155A CN 2011103673137 A CN2011103673137 A CN 2011103673137A CN 201110367313 A CN201110367313 A CN 201110367313A CN 103122155 A CN103122155 A CN 103122155A
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Abstract
The invention discloses a preparation method of high-performance window film insulation medium. The preparation method includes: firstly, selecting blue WO3, ATO and ITO nano-powders according to corresponding conditions, using a planet wet ball-milling disperser and a scientific and reasonable combining-scattering comparison method, and optimally selecting factors such as selection proportion and solid content of different insulation media, selection on mill ball size, control on rotation speed and continuous dispersion time. Therefore, optimal transmittance of visible light, optimal insulation, optimal ultraviolet proofing and optimal performance of high-performance insulation medium are achieved. The high-performance window film insulation medium prepared by the preparation method is high in transparency, thermal insulation and ultraviolet proofing, has high insulation in the near-infrared area of 780nm-900nm, is widely applied to production of high-performance insulation glass and high-performance insulation window films, and has very important social and economic values.
Description
Technical field
The present invention relates to the preparation method of the heat insulation medium of a kind of high-performance fenestrated membrane.
Background technology
the heat insulation medium of fenestrated membrane of producing both at home and abroad at present, single component ATO or ITO or other nano-powder and the nano pulps such as nano ceramics microballon of main employing, when but these nano materials are just used separately, the heat insulation medium that these are single, to spectrophotometric data, always there are a lot of defectives, the W03 of single-component, ATO, the ITO nano material respectively possesses some good points and is not enough, characteristics separately are, near ATO 780nm-1300nm is better than ITO nano material to the rejection rate of IR for wavelength, near ATO rejection rate to IR 1100nm is best, near wavelength WO3 780nm-1000nm compares ATO to the rejection rate of IR, the ITO nano material is all good, near WO3 rejection rate to IR 900nm is best.But wavelength is better than the transmitance of ATO, WO3 visible light at the visible region of 380nm-780nm ITO, ITO to the barrier region of IR near 780nm-1600nm.(WO3, ATO, ITO nano material see attached list one to the Different Effects graphic representation of optical property).Therefore, use separately a certain in the heat insulation media such as WO3, ATO, ITO, all can not well adjust the impact on optical index, therefore, research and probe, scientific and reasonable combination utilizes the advantage of various heat insulation media, can develop a kind ofly can satisfy near infrared region the heat insulation medium of high-performance fenestrated membrane that high transparent can be realized again high heat-proof quality, has the very urgent market requirement.
Summary of the invention
Technical problem to be solved by this invention is to provide and a kind ofly can improves the fenestrated membrane heat-proof quality, can improve again the preparation method of the heat insulation medium of high-performance fenestrated membrane of high transparent, high heat insulation rate of the properties of transparency of fenestrated membrane.Preparation method of the present invention is simple, low production cost, is conducive to scale operation.
In order to solve the problems of the technologies described above, the preparation method of the heat insulation medium of high-performance fenestrated membrane provided by the invention comprises following processing step::
Took respectively the blue nanometer WO that primary particle size is not more than 40nm by weight 1: 1: 1
3Powder, primary particle size are not more than the blue nano ATO powder of 10nm and three kinds of nano-powders of blue Nanometer ITO Powder that primary particle size is not more than 20nm, mix;
Take respectively nano-powder mixture 30-50 weight part, water-based/oil-based solvent 40-60 weight part and water-based/oiliness dispersion agent 0.3-5 weight part, join in the dispersion bucket of planet wet ball-milling rapid dispersion machine, the diameter that adds again 3 times of amounts of nano-powder mixture is the zirconium ball of 0.2-0.3mm, be under the condition of 11000-13000 rev/min at rotating speed, continuous high speed disperseed 14-18 hour, made the heat insulation medium of high-performance fenestrated membrane.
Preferably, in the preparation method of the heat insulation medium of the above-mentioned high-performance fenestrated membrane of the present invention, the aqueous dispersant solution according to volume ratio mixing in 1: 1 of diethanolamine and trolamine; The solution that the BYK2008 that the JU-110 modified poly ester wetting dispersing agent that the oiliness dispersion agent is produced with the poly-special Science and Technology Ltd. in Shenzhen and German Bick chemical company produce mixes according to weight ratio at 1: 1.
Preferably, in the preparation method of the heat insulation medium of the above-mentioned high-performance fenestrated membrane of the present invention, aqueous solvent is deionized water, and oil-based solvent is N-BUTYL ACETATE.
In the present invention, primary particle size is not more than the blue nano ATO powder of 10nm and blue Nanometer 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 disclosed method preparation of Chinese patent CN101597022A; The blue Nanometer ITO Powder that primary particle size is not more than 20nm can adopt the disclosed method preparation of Chinese patent CN1775693A.
In the present invention, primary particle size is not more than the blue nanometer WO of 40nm
3The preparation of powder comprises the steps:
1. pour wolframic acid, purity into and be 99.9 In (OH) in high speed sand milling dispersion machine
3Powder and mixed solvent, this mixed solvent are the mixed solution of the weight ratio first alcohol and water of 1: 1, 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 system; Be under the condition of 12000-14000 rev/min at rotating speed, the high speed sand milling disperseed 4-6 hour;
2. the material that 1. obtains of step is poured AL into
2O
3In crucible, taking out after putting into drying baker oven dry, in drying course, is oven dry after 5-7 hour under the condition of 85-95 ℃ in temperature, in temperature is to dry 4-8 hour under the condition of 160-200 ℃ again.
3. the material that 2. obtains of step first is processed into meal with pulverizer, then is processed into ultrafine powder with the air-flow dispersion machine; This ultrafine powder makes the following blue transparent heat-insulated WO of 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, is filled with nitrogen protection in calcination process, and the nitrogen amount of being filled with is 15-25m
3/ min.
Embodiment subsequently will prove, the heat insulation medium of high-performance fenestrated membrane that the inventive method makes is that wavelength is in the 380nm-900nm zone, during coating rete 3um, the IR rejection rate is greater than 90%, and visible light transmissivity VLT has the superpower transparency greater than 80%, thermal insulation, the characteristic of antiultraviolet can be widely used in and produce high performance building sunshade thermal insulation fenestrated membrane and high-performance glass energy-saving heat-insulating coating, and this invention has great importance to the energy-saving efficiency that improves building, automobile.
Description of drawings
Fig. 1 is WO
3, ATO and ITO be to optical property influence curve figure.
Embodiment
Below in conjunction with the drawings and specific embodiments, further set forth the present invention.These embodiment are interpreted as only being used for explanation the present invention 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 make various changes or modifications the present invention, and these equivalences change and modification falls into claim limited range of the present invention equally.
(the preparation primary particle size is not more than the blue WO of 40nm to embodiment 1.0
3Powder)
Get respectively successively 1. 50 weight part content 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 the deionized water mixed solvent of 1: 1,1. 2. 3. pouring into successively in ready high speed sand milling dispersion machine, rotating speed is transferred to 12000 rev/mins, after spending 30 minutes, use N, N one dimethylethanolamine is adjusted the pH value of colloid mixture in high speed sand milling dispersion machine, and pH value controls to 5 rear beginning high speed dispersion, disperse after 4 hours continuously, then the colloid mixture that takes out in high speed sand milling dispersion machine is poured Al into
2O
3Crucible, put into again the drying baker oven dry, temperature is transferred to 85 degree oven dry 5 hours, again temperature is increased 160 degree 4 hours, put into the retort furnace calcining after cooling, temperature is controlled at 600 degree again, connects nitrogen in 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 after naturally cooling and take out powder and first can obtain primary particle size less than the blue transparent heat-insulated WO of 40 nanometers with air-flow dispersion machine super-fine processing again with pulverizer roughing
3Nano-powder.
Embodiment 1.1 (the heat insulation medium of preparation water-based high-performance)
Take the blue WO that primary particle size that 1. embodiment 1.0 makes is not more than 40nm
3Powder 160g;
Take the blue ATO powder 160g that 2. primary particle size is not more than 10nm;
Take the blue ITO powder 160g that 3. primary particle size is not more than 20nm;
Take 4. deionized water 480g;
Take 5. water-based system dispersion agent, diethanolamine and trolamine are by the solution 40g of volume ratio mixing in 1: 1;
Be equipped with in the dispersion bucket of planet wet type rapid dispersion machine that diameter is 0.2mm zirconium ball 1. 2. 3. 4. 5. pouring into successively, adjustment of rotational speed to 11000 rev/min, disperseing continuously to open after 14 hours disperses bung, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, can obtain solid content and be 48% the heat insulation medium of water-based high-performance.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when during coating, build is adjusted to 3um, record result with spectral instrument as follows: IR rejection rate 91%; VLT transmitance 86%.WO in this heat insulation medium
3, ATO and ITO to the optical property influence curve as shown in Figure 1.
Embodiment 1.2 (the heat insulation medium of preparation oiliness high-performance)
Take the blue WO that primary particle size that 1. embodiment 1.0 makes is not more than 40nm
3Powder 160g;
Take the blue ATO powder 160g that 2. primary particle size is not more than 10nm;
Take the blue ITO powder 160g that 3. primary particle size is not more than 20nm;
Take 4. N-BUTYL ACETATE 480g;
Take 5. oiliness system dispersion agent, the solution 40g that JU-110 and BYK2008 mix according to weight ratio at 1: 1.
Be equipped with in the dispersion bucket of planet wet type rapid dispersion machine that diameter is 0.3mm zirconium ball 1. 2. 3. 4. 5. pouring into successively, adjustment of rotational speed to 12000 rev/min, disperseing continuously to open after 16 hours disperses bung, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, can obtain solid content and be 48% the heat insulation medium of oiliness high-performance.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when during coating, build is adjusted to 3um, record result with spectral instrument as follows: IR rejection rate 90%; VLT transmitance 87%.WO in this heat insulation medium
3, ATO and ITO similar to optical property influence curve and Fig. 1.
Embodiment 2.1 (the heat insulation medium of preparation water-based high-performance)
Take the blue WO that primary particle size that 1. embodiment 1.0 makes is not more than 40nm
3Powder 150g;
Take the blue ATO powder 150g that 2. primary particle size is not more than 10nm;
Take the blue ITO powder 150g that 3. primary particle size is not more than 20nm;
Take 4. deionized water 520g;
Take 5. water-based system dispersion agent, diethanolamine and trolamine are by the solution 30g of volume ratio mixing in 1: 1
Be equipped with in the dispersion bucket of planet wet type rapid dispersion machine that diameter is 0.3mm zirconium ball 1. 2. 3. 4. 5. pouring into successively, adjustment of rotational speed to 12000 rev/min, disperseing continuously to open after 16 hours disperses bung, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, can obtain solid content and be 45% the heat insulation medium of water-based high-performance.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when during coating, build is adjusted to 3um, record result with spectral instrument as follows: IR rejection rate 93%; VLT transmitance 86%.WO in this heat insulation medium
3, ATO and ITO similar to optical property influence curve and Fig. 1.
Embodiment 2.2 (the heat insulation medium of preparation oiliness high-performance)
Take the blue WO that primary particle size that 1. embodiment 1.0 makes is not more than 40nm
3Powder 150g;
Take the blue ATO powder 150g that 2. primary particle size is not more than 10nm;
Take the blue ITO powder 150g that 3. primary particle size is not more than 20nm;
Take 4. N-BUTYL ACETATE 520g;
Take 5. oiliness system dispersion agent, the solution 30g that JU-110 and BYK2008 mix according to weight ratio at 1: 1.
Be equipped with in the dispersion bucket of planet wet type rapid dispersion machine that diameter is 0.3mm zirconium ball 1. 2. 3. 4. 5. pouring into successively, adjustment of rotational speed to 13000 rev/min, disperseing continuously to open after 18 hours disperses bung, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, can obtain solid content and be 45% the heat insulation medium of oiliness high-performance.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when during coating, build is adjusted to 3um, record result with spectral instrument as follows: IR rejection rate 92%; VLT transmitance 86%.WO in this heat insulation medium
3, ATO and ITO similar to optical property influence curve and Fig. 1.
Embodiment 3.1 (the heat insulation medium of preparation water-based high-performance)
Take the blue WO that primary particle size that 1. embodiment 1.0 makes is not more than 40nm
3Powder 140g;
Take the blue ATO powder 140g that 2. primary particle size is not more than 10nm;
Take the blue ITO powder 140g that 3. primary particle size is not more than 20nm;
Take 4. deionized water 560g;
Take 5. water-based system dispersion agent, diethanolamine and trolamine are by the solution 20g of volume ratio mixing in 1: 1
Be equipped with in the dispersion bucket of planet wet type rapid dispersion machine that diameter is 0.3mm zirconium ball 1. 2. 3. 4. 5. pouring into successively, adjustment of rotational speed to 12000 rev/min, disperseing continuously to open after 16 hours disperses bung, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, can obtain solid content and be 42% the heat insulation medium of high-performance.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when during coating, build is adjusted to 3um, record result with spectral instrument as follows: IR rejection rate 94%; VLT transmitance 85%.WO in this heat insulation medium
3, ATO and ITO similar to optical property influence curve and Fig. 1.
Embodiment 3.2 (the heat insulation medium of preparation oiliness high-performance)
Take the blue WO that primary particle size that 1. embodiment 1.0 makes is not more than 40nm
3Powder 140g;
Take the blue ATO powder 140g that 2. primary particle size is not more than 10nm;
Take the blue ITO powder 140g that 3. primary particle size is not more than 20nm;
Take 4. N-BUTYL ACETATE 560g;
Take 5. oiliness system dispersion agent, the solution 20g that JU-110 and BYK2008 mix according to weight ratio at 1: 1.
Be equipped with in the dispersion bucket of planet wet type rapid dispersion machine that diameter is 0.2mm zirconium ball 1. 2. 3. 4. 5. pouring into successively, adjustment of rotational speed to 12500 rev/min, disperseing continuously to open after 17 hours disperses bung, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, can obtain solid content and be 42% the heat insulation medium of oiliness high-performance.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when during coating, build is adjusted to 3um, record result with spectral instrument as follows: IR rejection rate 93%; VLT transmitance 85%.WO in this heat insulation medium
3, ATO and ITO similar to optical property influence curve and Fig. 1.
Embodiment 4.1 (the heat insulation medium of preparation water-based high-performance)
Take the blue WO that primary particle size that 1. embodiment 1.0 makes is not more than 40nm
3Powder 130g;
Take the blue ATO powder 130g that 2. primary particle size is not more than 10nm;
Take the blue ITO powder 130g that 3. primary particle size is not more than 20nm;
Take 4. deionized water 600g;
Take 5. water-based system dispersion agent, diethanolamine and trolamine are by the solution 10g of volume ratio mixing in 1: 1
Be equipped with in the dispersion bucket of planet wet type rapid dispersion machine that diameter is 0.2mm zirconium ball 1. 2. 3. 4. 5. pouring into successively, adjustment of rotational speed to 11500 rev/min, disperseing continuously to open after 15 hours disperses bung, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, can obtain solid content and be 39% the heat insulation medium of water-based high-performance.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when during coating, build is adjusted to 3um, record result with spectral instrument as follows: IR rejection rate 94%; VLT transmitance 85%.WO in this heat insulation medium
3, ATO and ITO similar to optical property influence curve and Fig. 1.
Embodiment 4.2 (the heat insulation medium of preparation oiliness high-performance)
Take the blue WO that primary particle size that 1. embodiment 1.0 makes is not more than 40nm
3Powder 130g;
Take the blue ATO powder 130g that 2. primary particle size is not more than 10nm;
Take the blue ITO powder 130g that 3. primary particle size is not more than 20nm;
Take 4. N-BUTYL ACETATE 600g;
Take 5. oiliness system dispersion agent, the solution 10g that JU-110 and BYK2008 mix according to weight ratio at 1: 1.
Be equipped with in the dispersion bucket of planet wet type rapid dispersion machine that diameter is 0.25mm zirconium ball 1. 2. 3. 4. 5. pouring into successively, adjustment of rotational speed to 13000 rev/min, disperseing continuously to open after 18 hours disperses bung, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, can obtain solid content and be 39% the heat insulation medium of oiliness high-performance.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when during coating, build is adjusted to 3um, record result with spectral instrument as follows: IR rejection rate 93%; VLT transmitance 85%.WO in this heat insulation medium
3, ATO and ITO similar to optical property influence curve and Fig. 1.
Claims (3)
1. the preparation method of the heat insulation medium of high-performance fenestrated membrane, is characterized in that, comprises following processing step:
Took respectively the blue nanometer WO that primary particle size is not more than 40nm by weight 1: 1: 1
3Powder, primary particle size are not more than the blue nano ATO powder of 10nm and three kinds of nano-powders of blue Nanometer ITO Powder that primary particle size is not more than 20nm, mix;
Take respectively nano-powder mixture 30-50 weight part, water-based/oil-based solvent 40-60 weight part and water-based/oiliness dispersion agent 0.3-5 weight part, join in the dispersion bucket of planet wet ball-milling rapid dispersion machine, the diameter that adds again nano-powder mixture 2.5-3 doubly to measure is the zirconium ball of 0.2-0.3mm, be under the condition of 11000-13000 rev/min at rotating speed, continuous high speed disperseed 14-18 hour, made the heat insulation medium of high-performance fenestrated membrane.
2. the preparation method of the heat insulation medium of high-performance fenestrated membrane according to claim 1, is characterized in that, aqueous dispersant is the solution that diethanolamine and trolamine mixed in 1: 1 by volume; The oiliness dispersion agent is the solution that BYK2008 that the JU-110 modified poly ester wetting dispersing agent produced of the poly-special Science and Technology Ltd. in Shenzhen and German Bick chemical company produce mixes according to weight ratio at 1: 1.
3. the preparation method of the heat insulation medium of high-performance fenestrated membrane according to claim 1, is characterized in that, aqueous solvent is deionized water, and oil-based solvent is N-BUTYL ACETATE.
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| CN106146881A (en) * | 2015-03-23 | 2016-11-23 | 上海沪正纳米科技有限公司 | The preparation method of high transparent high thermal insulation hot phase transformation nano material |
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Effective date of registration: 20191211 Address after: 201404 Shanghai, Fengxian District layered Road, No. 5, building 585 Patentee after: Shanghai Shanghai Industrial Co., Ltd. Address before: 201204 Shanghai city Pudong New Area Lianxi Road No. 1151 Patentee before: Shanghai Huzheng Nano-Tech Co., Ltd. |