CN103214989B - Intelligent dimming PVB (Polyvinyl Butyral) film and preparation method of intelligent dimming PVB laminated glass - Google Patents

Intelligent dimming PVB (Polyvinyl Butyral) film and preparation method of intelligent dimming PVB laminated glass Download PDF

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CN103214989B
CN103214989B CN201310157436.7A CN201310157436A CN103214989B CN 103214989 B CN103214989 B CN 103214989B CN 201310157436 A CN201310157436 A CN 201310157436A CN 103214989 B CN103214989 B CN 103214989B
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pvb
intelligent dimming
glass
preparation
film
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CN103214989A (en
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徐刚
肖秀娣
史继富
熊斌
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Guangzhou Institute of Energy Conversion of CAS
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Guangzhou Institute of Energy Conversion of CAS
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Abstract

The invention discloses preparation methods of an intelligent dimming PVB (Polyvinyl Butyral) film and intelligent dimming PVB laminated glass. The preparation method of the intelligent dimming PVB film comprises the following steps of: dispersing a dopant-containing vanadium dioxide nanopowder dispersing solution of which a high-temperature phase or low-temperature phase has a phase change function into adhesive PVB resin, stirring to form a PVB sizing agent, and then preparing the PVB film with an intelligent dimming property by adopting a coating or extrusion molding method; and the preparation method of the intelligent dimming PVB laminated glass comprises the following step of: putting the intelligent dimming PVB film prepared by using the preparation method between two layers of glass by adopting a hot-pressing molding process to obtain the intelligent dimming PVB laminated glass. The PVB film with the intelligent dimming property can be molded on glass without any adhesive and extra process and is formed in one step, therefore, the preparation process is greatly simplified, and furthermore the cost of the intelligent glass is reduced; and meanwhile, the stability and service life of an intelligent dimming layer are greatly improved. The laminated glass can be widely applied to building energy conservation, car window heat insulation and other aspects.

Description

The preparation method of a kind of intelligent dimming PVB film and intelligent dimming PVB doubling glass
Technical field:
The present invention relates to energy-saving building technology field, be specifically related to a kind of intelligent dimming PVB film and intelligent dimming PVB doubling glass.
Background technology:
Current polyvinyl butyral acetal (PVB) is under catalyst action, through the synthetic resins that butyraldehyde-n and the PVA aqueous solution carry out condensation reaction and obtain, have transparent, fast light, water-fast, film forming and erosion-resisting characteristics, good adhesiveproperties is had to glass, metal, timber, pottery, leather, fiber and other material, be the tackiness agent that glass is best in the world, therefore its main application is as intermediate adhesion thin film layer in laminated safety glass manufactures.At present, the PVB of about 89% is for the production of building and the shatter proof glass of automobile industry.
Under the background that power supply is increasingly severe, energy-saving and cost-reducing is the target that the people of the world struggles jointly.Building energy consumption accounts for 30% of whole society's total energy consumption, and wherein topmost is exactly heating and air-conditioning, accounts for 20%.Go along with sb. to guard him greatly in parts in four of building, accounted for more than 50% of whole building and heating and air-conditioning power consumption by door and window dispersed heat.Western developed country carries out the research work of Energy Saving Windows from the sixties in 20th century, as heat-reflecting glass, and Low-E glass etc.The energy-conservation of Building Trade in China is mainly reflected on window design and illuminating energy-saving, less to the use of Energy Saving Windows.
Vanadium dioxide is a kind of transition metal oxide with phase-change characteristic.Can there is phase in version at 68 degree in vanadium dioxide monocrystal material, change the quadratic metal state high temperature from the monocline semiconductor form of low temperature into, and the transformation of M phase (low-temperature phase) to R phase (high-temperature-phase) namely occurs.While phase structure changes, the optics of vanadium dioxide material, electricity, the physicalies such as magnetics are also undergone mutation.In optics, vanadium dioxide by the transformation of the infrared transparent state of low temperature to the infrared external reflection state of high temperature, thus can reach the object of reflected infrared and sunlight due to the transformation of structure.The phase transition temperature of vanadium dioxide can be regulated by the content of doping agent, from-20 degree to 68 degree.Therefore, the film prepared with vanadium dioxide can realize Intelligent adjustment sunlight and ultrared object, and at energy-saving coating, optical memory material, there is purposes widely the aspects such as lasing safety.
The method that at present conventional preparation contains vanadium dioxide coating mainly contains magnetron sputtering method, chemical Vapor deposition process, sol-gel method etc., and these methods all also exist the high and complex process of apparatus expensive, cost, and film forming area is little, is not suitable for the limitations such as batch production.Patent CN102399072A, CN102120615A, CN102464354A, CN102336528A refer to the method film after hypovanadic oxide powder dispersion, but because the dispersion system used in these methods does not all have good cohesiveness on matrix, can only apply on specific matrix, significantly limit its use range.Even if the coating be coated on flexible parent metal still needs to apply could use after one deck installs glue, not only increase the complicacy of rete technique, and add film cost.
Summary of the invention:
The object of this invention is to provide a kind of preparation method of intelligent dimming PVB film.
Another object of the present invention is to provide a kind of preparation method of intelligent dimming PVB doubling glass.
The present invention is achieved by the following technical programs:
A kind of intelligent dimming PVB(polyvinyl butyral acetal) preparation method of film, R phase (high-temperature-phase) or M phase (low-temperature phase) are had the vanadium dioxide (VO containing doping agent of phase transition function 2) nano-powder dispersion liquid is distributed to has in close-burning PVB resin, stir and form PVB slurry, then by apply or the method for extrusion moulding prepares the pvb film with intelligent dimming performance; Described coating refers to apply on pvb film the PVB slurry that one deck contains vanadium dioxide nano powder; Described extrusion moulding is that the PVB slurry containing vanadium oxide is extruded the intelligent dimming pvb film that rear curtain coating is drawn into different size; Described doping agent is selected from least one in tungsten, molybdenum, niobium, tantalum, zirconium, fluorine element, and the content of doping agent is VO 2the 0-5% of molar content; In described PVB slurry, the content of vanadium dioxide is 1-100g/L, and more preferably scope is 10-75g/L.
Described VO 2the particle diameter of nano-powder is preferably 20-500nm.
Described VO 2nano-powder dispersion liquid, VO 2massfraction in dispersion agent is 0.5-20%, described dispersion agent is organic solvent, is selected from least one in methyl alcohol, ethanol, Virahol, butanols, benzene,toluene,xylene, methyl acetate, ethyl acetate, propyl acetate, butylacetate, hexyl acetate, acetone, espeleton, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, acetonitrile, pyridine, methylene dichloride, chlorobenzene, dichlorobenzene, ether or sherwood oil.
A preparation method for intelligent dimming PVB doubling glass, inserts between layer glass by the intelligent dimming PVB film prepared by preceding method by hot-forming, forms the PVB doubling glass with intelligent dimming performance.
Described glass is simple glass, toughened glass or semi-tempered glass.
The PVB film with intelligent dimming performance of the present invention can take shape on glass without any need for binding agent and extra technique, once shaped, greatly simplify preparation technology, and then reduce the cost of intelligent glass, simultaneously because intelligent dimming layer is between layer glass, decrease the possibility of oxidation due to air and artificial destruction, the stability of intelligent dimming layer and life-span are improved greatly.This doubling glass can be widely used in building energy conservation, the aspects such as vehicle window heat-insulation.
Accompanying drawing illustrates:
Fig. 1 is traditional intelligence light modulation film and intelligent light modulation film of the present invention contrast schematic diagram;
Wherein, (1), traditional intelligence glass structure of adjusting luminance; (2), intelligent dimming pad pasting glass structure; (3), intelligent dimming glass structure of the present invention; A, glass; B, light modulation rete; C, tack coat; D, protective film; E glass.
Embodiment:
Below further illustrate of the present invention, instead of limitation of the present invention.
Embodiment 1
(1) the unadulterated hypovanadic oxide powder of 0.5g is got; VO 2the particle diameter of particle is 100nm;
(2) prepare with ethanol the vanadium dioxide dispersion liquid that massfraction is 0.5%;
(3) dispersion liquid of vanadium dioxide is added in a certain amount of PVB resin, after stirring, form the PVB slurry that vanadium dioxide content is 1g/L;
(4) PVB slurry is extruded rear curtain coating to draw, obtains intelligent dimming PVB film,
(5) intelligent dimming PVB film is clipped between two panels simple glass, namely obtains intelligent dimming PVB doubling glass by hot-forming.
Embodiment 2
(1) getting 0.5g tungsten molar content is the hypovanadic oxide powder of 0.5%; VO 2the particle diameter of particle is 20nm;
(2) prepare with acetone the vanadium dioxide dispersion liquid that mass percentage concentration is 1%;
(3) VO 2dispersion liquid add in PVB resin, form VO after stirring 2content is the PVB slurry of 10g/L;
(4) PVB slurry is extruded rear curtain coating to draw, obtains intelligent dimming PVB film,
(5) intelligent dimming PVB film is clipped between two panels toughened glass, namely obtains intelligent dimming PVB doubling glass by hot-forming.
Embodiment 3
(1) getting 0.5g tungsten molar content is the hypovanadic oxide powder of 1%; VO 2the particle diameter of particle is 50nm;
(2) prepare with dimethylbenzene the vanadium dioxide dispersion liquid that massfraction is 2%;
(3) VO 2dispersion liquid add in PVB resin, form VO after stirring 2content is the PVB slurry of 15g/L;
(4) PVB slurry is extruded rear curtain coating to draw, obtains intelligent dimming PVB film,
(5) intelligent dimming PVB film is clipped between two panels simple glass, namely obtains intelligent dimming PVB doubling glass by hot-forming.
Embodiment 4
(1) getting 0.5g molybdenum molar content is the hypovanadic oxide powder of 2%; VO 2the particle diameter of particle is 300nm;
(2) prepare by ethyl acetate the vanadium dioxide dispersion liquid that massfraction is 5%;
(3) VO 2dispersion liquid add in PVB resin, form VO after stirring 2content is the PVB slurry of 50g/L;
(4) PVB slurry is extruded rear curtain coating to draw, obtains intelligent dimming PVB film,
(5) intelligent dimming PVB film is clipped between the glass of two panels half tempered, namely obtains intelligent dimming PVB doubling glass by hot-forming.
Embodiment 5
(1) getting 0.5g fluorine molar content is the hypovanadic oxide powder of 3%; VO 2the particle diameter of particle is 150nm;
(2) spent glycol monomethyl ether preparation massfraction is the vanadium dioxide dispersion liquid of 15%;
(3) VO 2dispersion liquid add in PVB resin, form VO after stirring 2content is the PVB slurry of 60g/L;
(4) PVB slurry is extruded rear curtain coating to draw, obtains intelligent dimming PVB film,
(5) intelligent dimming PVB film is clipped between two panels simple glass, namely obtains intelligent dimming PVB doubling glass by hot-forming.
Embodiment 6
(1) getting 0.5g zirconium molar content is the hypovanadic oxide powder of 5%; VO 2the particle diameter of particle is 500nm;
(2) prepare with sherwood oil the vanadium dioxide dispersion liquid that massfraction is 20%;
(3) VO 2dispersion liquid add in PVB resin, form VO after stirring 2content is the PVB slurry of 75g/L;
(4) by PVB slurry blade coating in not containing VO 2pvb film on, form intelligent dimming pvb film;
(5) intelligent dimming PVB film is clipped between two panels simple glass, namely obtains intelligent dimming PVB doubling glass by hot-forming.
Embodiment 7
(1) getting 0.5g niobium molar content is the hypovanadic oxide powder of 0.5%; VO 2the particle diameter of particle is 100nm;
(2) prepare with sherwood oil the vanadium dioxide dispersion liquid that massfraction is 20%;
(3) VO 2dispersion liquid add in PVB resin, form VO after stirring 2content is the PVB slurry of 100g/L;
(4) by PVB slurry blade coating in not containing on the pvb film of VO2, form intelligent dimming pvb film;
(5) intelligent dimming PVB film is clipped between two panels simple glass, namely obtains intelligent dimming PVB doubling glass by hot-forming.
Embodiment 8
(1) getting 0.5g tantalum molar content is the hypovanadic oxide powder of 0.5%; VO 2the particle diameter of particle is 80nm;
(2) prepare by ethyl acetate the vanadium dioxide dispersion liquid that massfraction is 5%;
(3) VO 2dispersion liquid add in PVB resin, form VO after stirring 2content is the PVB slurry of 20g/L;
(4) PVB slurry is extruded rear curtain coating to draw, obtains intelligent dimming PVB film,
(5) intelligent dimming PVB film is clipped between the glass of two panels half tempered, namely obtains intelligent dimming PVB doubling glass by hot-forming.

Claims (3)

1. the preparation method of an intelligent dimming PVB film, it is characterized in that, high-temperature-phase or low-temperature phase are had being distributed to containing the vanadium dioxide nano powder dispersion liquid of doping agent of phase transition function to be had in close-burning PVB resin, stir and form PVB slurry, then prepare the pvb film with intelligent dimming performance by the method for coating or extrusion moulding, described doping agent is selected from least one in tungsten, molybdenum, niobium, tantalum, zirconium, fluorine element, and the content of doping agent is the 0-5% of vanadium dioxide molar content, in described PVB slurry, the content of vanadium dioxide is 10-75g/L, the particle diameter of described vanadium dioxide nano powder is 20-500nm, described vanadium dioxide nano powder dispersion liquid, the massfraction of vanadium dioxide in dispersion agent is 0.5-20%, described dispersion agent is selected from methyl alcohol, ethanol, Virahol, butanols, benzene, toluene, dimethylbenzene, methyl acetate, ethyl acetate, propyl acetate, butylacetate, hexyl acetate, acetone, espeleton, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, acetonitrile, pyridine, methylene dichloride, chlorobenzene, dichlorobenzene, at least one in ether or sherwood oil.
2. a preparation method for intelligent dimming PVB doubling glass, is characterized in that, the intelligent dimming PVB film prepared is inserted between layer glass by hot-forming by the method described in aforementioned claim.
3. the preparation method of intelligent dimming PVB doubling glass according to claim 2, is characterized in that, described glass is simple glass, toughened glass or semi-tempered glass.
CN201310157436.7A 2013-04-28 2013-04-28 Intelligent dimming PVB (Polyvinyl Butyral) film and preparation method of intelligent dimming PVB laminated glass Active CN103214989B (en)

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CN106543910B (en) * 2015-09-23 2019-07-02 上海沪正纳米科技有限公司 A kind of intelligent temperature control PVB glue film and preparation method thereof
CN105086859B (en) * 2015-09-24 2017-06-30 佛山市明事达智能材料有限公司 A kind of infrared ray regulation heat-insulated EVA adhesive film of intelligence and preparation method thereof
CN106527035A (en) * 2016-10-18 2017-03-22 孙绪刚 Transparent ultraviolet-prevention projection screen based on PVB film, and preparation method therefor
CN106675115A (en) * 2016-11-28 2017-05-17 江南大学 Preparation method of high-transmittance thermochromatic intelligent recoating

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CN102674713A (en) * 2012-05-07 2012-09-19 信义超薄玻璃(东莞)有限公司 Thermochromic laminated glass and manufacturing method thereof

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