CN103122155B - 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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- CN103122155B CN103122155B CN201110367313.7A CN201110367313A CN103122155B CN 103122155 B CN103122155 B CN 103122155B CN 201110367313 A CN201110367313 A CN 201110367313A CN 103122155 B CN103122155 B CN 103122155B
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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 a kind of preparation method of high-performance window film insulation medium.
Background technology
The window film insulation medium of producing both at home and abroad at present, nano-powder and the nano pulps such as component ATO or ITO that main employing is single or other nano ceramics microballon, when but these nano materials are just used alone, these single insulation medium, to spectrophotometric data, always there is a lot of defect, the W03 of single-component, ATO, ITO nano material respectively possesses some good points and deficiency, respective feature is, ATO near 780nm-1300nm is better than ITO nano material to the rejection rate of IR for wavelength, ATO is best to the rejection rate of IR near 1100nm, wavelength WO3 near 780nm-1000nm compares ATO to the rejection rate of IR, ITO nano material is all good, WO3 is best to the rejection rate of IR near 900nm.But wavelength is better than the transmitance of ATO, WO3 visible ray at the visible region ITO of 380nm-780nm, ITO to the barrier region of IR near 780nm-1600nm.(the Different Effects graphic representation of WO3, ATO, ITO nano material to optical property sees attached list one).Therefore, what be used alone in the insulation medium such as WO3, ATO, ITO is a certain, all well can not adjust the impact on optical index, therefore, research and probe, scientific and reasonable combination utilizes the advantage of various insulation medium, can develop a kind ofly can meet near infrared region the high-performance window film insulation medium that high transparent can realize 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 one can improve window film insulation performance, can improve again the preparation method of high-performance window film insulation medium of the high transparency of the properties of transparency of fenestrated membrane, high heat insulation rate.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 high-performance window film insulation medium provided by the invention, comprises following processing step::
The blue nanometer WO that primary particle size is not more than 40nm is taken respectively by weight 1: 1: 1
3powder, primary particle size are not more than blue Nanometer ITO Powder three kinds of nano-powders that the blue nano ATO powder of 10nm and primary particle size are not more than 20nm, mix;
Take 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 respectively, join in the dispersion bucket of planet wet ball-milling rapid dispersion machine, the diameter adding nano-powder mixture 3 times amount is again the zirconium ball of 0.2-0.3mm, be under the condition of 11000-13000 rev/min at rotating speed, continuous high speed dispersion 14-18 hour, obtained high-performance window film insulation medium.
Preferably, in the preparation method of the above-mentioned high-performance window film insulation medium of the present invention, the solution mixed according to volume ratio 1: 1 of aqueous dispersant diethanolamine and trolamine; The JU-110 modified poly ester wetting dispersing agent that Ju Te Science and Technology Ltd. of oiliness dispersion agent Shenzhen produces and the solution that the BYK2008 that German Bick chemical company produces mixes according to weight ratio 1: 1.
Preferably, in the preparation method of the above-mentioned high-performance window film insulation medium 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 Nanometer ITO Powder that the blue nano ATO powder of 10nm and primary particle size be not more than 20nm and all adopts usual method to be prepared from.For example, the blue nano ATO powder that primary particle size is not more than 10nm can adopt method preparation disclosed in Chinese patent CN101597022A; The blue Nanometer ITO Powder that primary particle size is not more than 20nm can adopt method preparation disclosed in 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. in high speed sand milling dispersion machine, pour wolframic acid into, purity be 99.9 In (OH)
3powder and mixed solvent, this mixed solvent is the mixed solution of the first alcohol and water of weight ratio 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; With N, N-dimethylethanolamine, the pH value in system is adjusted to 5-5.5; Be under the condition of 12000-14000 rev/min at rotating speed, high speed sand milling dispersion 4-6 hour;
2. the material that 1. step obtains pours AL into
2o
3in crucible, put into after drying baker is dried and take out, in drying course, being after drying 5-7 hour under the condition of 85-95 DEG C in temperature, is dry 4-8 hour again under the condition of 160-200 DEG C in temperature.
3. the material that 2. step obtains first is processed into meal with pulverizer, then is machined to ultrafine powder with air dispersion; The heat insulation WO of blue-tinted transparent of this ultrafine powder obtained below primary particle size 40nm after dropping into retort furnace calcining
3nano-powder, wherein, calcining temperature is 600-650 DEG C, and calcination time is 5-7 hour, is filled with nitrogen protection in calcination process, and nitrogen charge is 15-25m
3/ min.
Embodiment subsequently will prove, the high-performance window film insulation medium that the inventive method obtains is that wavelength is in 380nm-900nm region, during paint film 3um, IR rejection rate is greater than 90%, and visible light transmissivity VLT is greater than 80%, has the superpower transparency, 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 is built improving, the energy-saving efficiency of automobile has great importance.
Accompanying drawing explanation
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, set forth the present invention further.These embodiments are interpreted as only being not used in for illustration of the present invention limiting the scope of the 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 equivalence changes and modification fall into the scope of the claims in the present invention equally.
Embodiment 1.0 (prepares the blue WO that primary particle size is not more than 40nm
3powder)
Getting 1. 50 weight part content successively is respectively the wolframic acid (H of 99.9%
2wO
4); Get the indium hydroxide In (OH) that 2. 5 weight part content are 99.9%
3powder; Get the mixed solvent of 3. 45 parts by weight Methanol and deionized water 1: 1,1. 2. 3. pouring in ready high speed sand milling dispersion machine successively, rotating speed is transferred to 12000 revs/min, after spending 30 minutes, with the pH value of N, N mono-colloid mixture in dimethylethanolamine adjustment high speed sand milling dispersion machine, after pH value controls to 5, start high speed dispersion, continuous dispersion is after 4 hours, then the colloid mixture taken out in high speed sand milling dispersion machine pours Al into
2o
3crucible, put into drying baker again to dry, temperature is transferred to 85 degree dries 5 hours, again temperature increase 160 degree 4 hours, after cooling, put into retort furnace calcining again, temperature controls at 600 degree, connects nitrogen in retort furnace, nitrogen flow adjusts to 15 cubic meters per minute, opens retort furnace lid and take out powder and first can obtain by air dispersion machine super-fine processing the heat insulation WO of blue-tinted transparent that primary particle size is less than 40 nanometers again with pulverizer roughing after controlling to 5 hours heat-up time after naturally cooling
3nano-powder.
Embodiment 1.1 (preparation water-based high-performance insulation medium)
Take the blue WO that the obtained primary particle size of 1. embodiment 1.0 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, the solution 40g that diethanolamine and trolamine mix by 1: 1 volume ratio;
1. 2. 3. 4. 5. pouring into successively, diameter is housed is in the dispersion bucket of planet wet type rapid dispersion machine of 0.2mm zirconium ball, adjustment of rotational speed to 11000 revs/min, dispersion bung is opened in continuous dispersion after 14 hours, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, the water-based high-performance insulation medium that solid content is 48% can be obtained.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build adjusts to 3um during coating, records result with spectral instrument as follows: IR rejection rate 91%; VLT transmitance 86%.WO in this insulation medium
3, ATO and ITO to optical property influence curve as shown in Figure 1.
Embodiment 1.2 (preparation oiliness high-performance insulation medium)
Take the blue WO that the obtained primary particle size of 1. embodiment 1.0 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. oleaginous system dispersion agent, the solution 40g that JU-110 and BYK2008 mixes according to weight ratio 1: 1.
1. 2. 3. 4. 5. pouring into successively, diameter is housed is in the dispersion bucket of planet wet type rapid dispersion machine of 0.3mm zirconium ball, adjustment of rotational speed to 12000 revs/min, dispersion bung is opened in continuous dispersion after 16 hours, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, the oiliness high-performance insulation medium that solid content is 48% can be obtained.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build adjusts to 3um during coating, records result with spectral instrument as follows: IR rejection rate 90%; VLT transmitance 87%.WO in this insulation medium
3, ATO and ITO to optical property influence curve and Fig. 1 similar.
Embodiment 2.1 (preparation water-based high-performance insulation medium)
Take the blue WO that the obtained primary particle size of 1. embodiment 1.0 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, the solution 30g that diethanolamine and trolamine mix by 1: 1 volume ratio
1. 2. 3. 4. 5. pouring into successively, diameter is housed is in the dispersion bucket of planet wet type rapid dispersion machine of 0.3mm zirconium ball, adjustment of rotational speed to 12000 revs/min, dispersion bung is opened in continuous dispersion after 16 hours, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, the water-based high-performance insulation medium that solid content is 45% can be obtained.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build adjusts to 3um during coating, records result with spectral instrument as follows: IR rejection rate 93%; VLT transmitance 86%.WO in this insulation medium
3, ATO and ITO to optical property influence curve and Fig. 1 similar.
Embodiment 2.2 (preparation oiliness high-performance insulation medium)
Take the blue WO that the obtained primary particle size of 1. embodiment 1.0 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. oleaginous system dispersion agent, the solution 30g that JU-110 and BYK2008 mixes according to weight ratio 1: 1.
1. 2. 3. 4. 5. pouring into successively, diameter is housed is in the dispersion bucket of planet wet type rapid dispersion machine of 0.3mm zirconium ball, adjustment of rotational speed to 13000 revs/min, dispersion bung is opened in continuous dispersion after 18 hours, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, the oiliness high-performance insulation medium that solid content is 45% can be obtained.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build adjusts to 3um during coating, records result with spectral instrument as follows: IR rejection rate 92%; VLT transmitance 86%.WO in this insulation medium
3, ATO and ITO to optical property influence curve and Fig. 1 similar.
Embodiment 3.1 (preparation water-based high-performance insulation medium)
Take the blue WO that the obtained primary particle size of 1. embodiment 1.0 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, the solution 20g that diethanolamine and trolamine mix by 1: 1 volume ratio
1. 2. 3. 4. 5. pouring into successively, diameter is housed is in the dispersion bucket of planet wet type rapid dispersion machine of 0.3mm zirconium ball, adjustment of rotational speed to 12000 revs/min, dispersion bung is opened in continuous dispersion after 16 hours, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, the high-performance insulation medium that solid content is 42% can be obtained.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build adjusts to 3um during coating, records result with spectral instrument as follows: IR rejection rate 94%; VLT transmitance 85%.WO in this insulation medium
3, ATO and ITO to optical property influence curve and Fig. 1 similar.
Embodiment 3.2 (preparation oiliness high-performance insulation medium)
Take the blue WO that the obtained primary particle size of 1. embodiment 1.0 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. oleaginous system dispersion agent, the solution 20g that JU-110 and BYK2008 mixes according to weight ratio 1: 1.
1. 2. 3. 4. 5. pouring into successively, diameter is housed is in the dispersion bucket of planet wet type rapid dispersion machine of 0.2mm zirconium ball, adjustment of rotational speed to 12500 revs/min, dispersion bung is opened in continuous dispersion after 17 hours, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, the oiliness high-performance insulation medium that solid content is 42% can be obtained.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build adjusts to 3um during coating, records result with spectral instrument as follows: IR rejection rate 93%; VLT transmitance 85%.WO in this insulation medium
3, ATO and ITO to optical property influence curve and Fig. 1 similar.
Embodiment 4.1 (preparation water-based high-performance insulation medium)
Take the blue WO that the obtained primary particle size of 1. embodiment 1.0 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, the solution 10g that diethanolamine and trolamine mix by 1: 1 volume ratio
1. 2. 3. 4. 5. pouring into successively, diameter is housed is in the dispersion bucket of planet wet type rapid dispersion machine of 0.2mm zirconium ball, adjustment of rotational speed to 11500 revs/min, dispersion bung is opened in continuous dispersion after 15 hours, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, the water-based high-performance insulation medium that solid content is 39% can be obtained.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build adjusts to 3um during coating, records result with spectral instrument as follows: IR rejection rate 94%; VLT transmitance 85%.WO in this insulation medium
3, ATO and ITO to optical property influence curve and Fig. 1 similar.
Embodiment 4.2 (preparation oiliness high-performance insulation medium)
Take the blue WO that the obtained primary particle size of 1. embodiment 1.0 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. oleaginous system dispersion agent, the solution 10g that JU-110 and BYK2008 mixes according to weight ratio 1: 1.
1. 2. 3. 4. 5. pouring into successively, diameter is housed is in the dispersion bucket of planet wet type rapid dispersion machine of 0.25mm zirconium ball, adjustment of rotational speed to 13000 revs/min, dispersion bung is opened in continuous dispersion after 18 hours, take out the nano pulp of colloid mixture, after filtering with 200 order filter cloths, the oiliness high-performance insulation medium that solid content is 39% can be obtained.
Optical performance test: be brushed to the thick glass surface of 5mm with spreading rod, when build adjusts to 3um during coating, records result with spectral instrument as follows: IR rejection rate 93%; VLT transmitance 85%.WO in this insulation medium
3, ATO and ITO to optical property influence curve and Fig. 1 similar.
Claims (1)
1. a preparation method for high-performance window film insulation medium, is characterized in that, comprises following processing step:
1:1:1 takes the blue nanometer WO that primary particle size is not more than 40nm respectively by weight
3powder, primary particle size are not more than blue Nanometer ITO Powder three kinds of nano-powders that the blue nano ATO powder of 10nm and primary particle size are not more than 20nm, mix;
Take nano-powder mixture 30-50 weight part, water-based or oil-based solvent 40-60 weight part and water-based or oiliness dispersion agent 0.3-5 weight part respectively, join in the dispersion bucket of planet wet ball-milling rapid dispersion machine, the diameter adding nano-powder mixture 2.5-3 times amount is again the zirconium ball of 0.2-0.3mm, be under the condition of 11000-13000 rev/min at rotating speed, continuous high speed dispersion 14-18 hour, obtained high-performance window film insulation medium; Wherein:
Aforementioned aqueous dispersant is the solution of diethanolamine and trolamine 1:1 mixing by volume; Oiliness dispersion agent is the solution that the JU-110 modified poly ester wetting dispersing agent of Ju Te Science and Technology Ltd. of Shenzhen production and the BYK2008 of German Bick chemical company production mix according to weight ratio 1:1;
Aqueous solvent is deionized water, and oil-based solvent is N-BUTYL ACETATE.
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| CN103283532B (en) * | 2013-06-17 | 2014-11-19 | 湖北天瑞博能科技有限公司 | Nanometer self-assembly thermal insulation agricultural film |
| CN106146881B (en) * | 2015-03-23 | 2018-06-22 | 上海沪正纳米科技有限公司 | The preparation method of the hot phase transformation nano material of the high thermal insulation of high transparency |
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| CN101603619A (en) * | 2008-06-11 | 2009-12-16 | 财团法人工业技术研究院 | Transparent heat-insulating multilayered structure |
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| WO2008043373A1 (en) * | 2006-10-09 | 2008-04-17 | Advanced Glass Ceramics Establishment | Heat insulating composite and methods of manufacturing thereof |
| KR101611627B1 (en) * | 2007-11-05 | 2016-04-11 | 바스프 에스이 | Heat shielding additives |
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| CN101054455A (en) * | 2007-04-27 | 2007-10-17 | 南京工业大学 | Nano semi-conductor metal oxide paste composition and preparing process thereof |
| CN101603619A (en) * | 2008-06-11 | 2009-12-16 | 财团法人工业技术研究院 | Transparent heat-insulating multilayered structure |
| CN101899249A (en) * | 2009-05-25 | 2010-12-01 | 上海复甲新型材料科技有限公司 | Transparent thermal insulation anti-ultraviolet coating and preparation method thereof |
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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. |