CN109424306A - Can ultraviolet blocking-up photochromic building window preparation method and application - Google Patents

Can ultraviolet blocking-up photochromic building window preparation method and application Download PDF

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Publication number
CN109424306A
CN109424306A CN201710902702.2A CN201710902702A CN109424306A CN 109424306 A CN109424306 A CN 109424306A CN 201710902702 A CN201710902702 A CN 201710902702A CN 109424306 A CN109424306 A CN 109424306A
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Prior art keywords
photochromic
building window
variety
ultraviolet blocking
building
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CN201710902702.2A
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CN109424306B (en
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吴长征
杨波
谢毅
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University of Science and Technology of China USTC
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University of Science and Technology of China USTC
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    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B9/00—Screening or protective devices for wall or similar openings, with or without operating or securing mechanisms; Closures of similar construction
    • E06B9/24—Screens or other constructions affording protection against light, especially against sunshine; Similar screens for privacy or appearance; Slat blinds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B11/00—Oxides or oxyacids of halogens; Salts thereof
    • C01B11/22—Oxygen compounds of iodine
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • G—PHYSICS
    • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F3/00—Labels, tag tickets, or similar identification or indication means; Seals; Postage or like stamps
    • G09F3/02—Forms or constructions
    • G09F3/0291—Labels or tickets undergoing a change under particular conditions, e.g. heat, radiation, passage of time
    • G09F3/0294—Labels or tickets undergoing a change under particular conditions, e.g. heat, radiation, passage of time where the change is not permanent, e.g. labels only readable under a special light, temperature indicating labels and the like
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60J—WINDOWS, WINDSCREENS, NON-FIXED ROOFS, DOORS, OR SIMILAR DEVICES FOR VEHICLES; REMOVABLE EXTERNAL PROTECTIVE COVERINGS SPECIALLY ADAPTED FOR VEHICLES
    • B60J1/00—Windows; Windscreens; Accessories therefor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B11/00—Oxides or oxyacids of halogens; Salts thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B11/00—Oxides or oxyacids of halogens; Salts thereof
    • C01B11/20—Oxygen compounds of bromine
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G15/00—Compounds of gallium, indium or thallium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G29/00—Compounds of bismuth
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G29/00—Compounds of bismuth
    • C01G29/006—Compounds containing, besides bismuth, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G30/00—Compounds of antimony
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/006—Compounds containing, besides vanadium, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/001—General methods for coating; Devices therefor
    • C03C17/002—General methods for coating; Devices therefor for flat glass, e.g. float glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
    • C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/16—Halogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
    • E06B3/30—Coverings, e.g. protecting against weather, for decorative purposes
    • G—PHYSICS
    • G02—OPTICS
    • G02C—SPECTACLES; SUNGLASSES OR GOGGLES INSOFAR AS THEY HAVE THE SAME FEATURES AS SPECTACLES; CONTACT LENSES
    • G02C7/00—Optical parts
    • G02C7/10—Filters, e.g. for facilitating adaptation of the eyes to the dark; Sunglasses
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/17—Nanostrips, nanoribbons or nanobelts, i.e. solid nanofibres with two significantly differing dimensions between 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/29—Mixtures
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/90—Other aspects of coatings
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/118—Deposition methods from solutions or suspensions by roller-coating
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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    • C08J2369/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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    • C08K2201/00—Specific properties of additives
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    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B9/00—Screening or protective devices for wall or similar openings, with or without operating or securing mechanisms; Closures of similar construction
    • E06B9/24—Screens or other constructions affording protection against light, especially against sunshine; Similar screens for privacy or appearance; Slat blinds
    • E06B2009/2405—Areas of differing opacity for light transmission control

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Abstract

The present invention relates to can ultraviolet blocking-up the preparation method of photochromic building window and products thereof and application, be M the method includes preparing general formulaaObXcCan ultraviolet blocking-up photochromic nano material, wherein M, O and X and a, b and c are as defined herein, and using the photochromic nano material by forming in common building object window surface one layer of photochromic material film of adherency, or after the photochromic nano material is mixed with building window material to prepare photochromic building window.Photochromic building window prepared by the present invention can block 80% or more ultraviolet light, especially can be changed to transparent dead color in strong illumination, reduce transmitance；It can restore colorless and transparent state again in no strong illumination.Method of the invention has the characteristics that process flow is simple, low in cost, yield is big, is suitable for industrial production, there is preferable practical prospect.

Description

Can ultraviolet blocking-up photochromic building window preparation method and application
Technical field
The present invention relates to intelligent color-changing Material Fields, and in particular to it is a kind of can ultraviolet blocking-up photochromic building window Preparation method, photochromic building window and its application.
Background technique
It is photochromic to refer to that under the light radiation of certain wavelength and intensity certain change occurs for certain compound-materials Reaction is learned, causes compound structure to change, compound colors is caused to change, remove illumination or again through another wavelength and intensity Light irradiation after, color is restored or occurs new variation.From the fifties in last century, Hirshberg et al. is reported about light Mutagens color was applied to after a possibility that optical recording stores, and the performance of various novel photochromic materials and its application are The research of system is widely used in building window glass, light-sensitive sunglasses eyeglass, vehicles glass pane, information storage material, decoration The fields such as material, photosensitive material.
The research of photochromic material focuses primarily upon two major classes, i.e. organic photochromic material and inorganic photochromic material Material.But organic photochromic material there are thermal stability it is poor, easy to aging, weatherability is weak the problems such as, limit its and practical answer With.Inorganic photochromic material is better than the good characteristic of organic photochromic material with its many and is concerned.So far, The research of inorganic photochromic material focuses primarily upon transition elements oxide of mutually (such as MoO3、TiO2、Nb2O5、WO3、Ta2Os、BeO Deng), metal halide (such as CuCl2、CdCl2, AgX etc.), polyoxometallate and rare earth compounding etc..Although some materials body System's relative maturity, but there is the problems such as such as higher cost of raw material and complicated processing technology, it is big to limit it Scale commercial application.Meanwhile existing many photochromic materials can only reduce the transmitance of light, and cannot block in sunlight To the maximum ultraviolet light of body effect.
With the continuous acceleration of economic fast development and urbanization process, high buildings and large mansions are rised sheer from level ground, for building Daylighting, energy conservation and living environment comfort level put forward new requirements.Photochromic window comes into being.
CN103032018A discloses a kind of compound glass preparation that silver bromide and copper oxide are smeared on simple glass Intelligent photochromic window.CN106218172A discloses one kind by wear-resisting anti-scratch polyester layer, first transparent base film, light-induced variable The photochromic fenestrated membrane that chromoresin layer, second transparent base film, ultraviolet-resistant pressure-sensitive adhesive layer and transparent release film are constituted.However, These buildings discoloration window generally requires complicated multilayered structure, and reaction mechanism process is complicated, and technology of preparing is more severe It carves.
In summary it can be seen, with the development of intelligent main trend, people for photochromic building window demand not It is disconnected to rise.That there are the costs of raw material is higher for existing photochromic building window, technology is complicated etc. is unable to satisfy industrial life The requirement for producing economy, hinders extensive development of the photochromic building window in business application.Meanwhile it is inexpensive new The photochromic building window of type is still less.Therefore, it is badly in need of exploitation with technology is simple, the cost of raw material is cheap, resistance to Time property is relatively strong, simultaneously can with ultraviolet blocking-up can large-scale commercial applications application photochromic building window.
Summary of the invention
In order to solve the above problem, the present invention provides following technical schemes:
On the one hand, the present invention provide it is a kind of prepare can ultraviolet blocking-up photochromic building window method, including Following steps:
(1) general formula is MaObXcCan ultraviolet blocking-up photochromic nano material preparation:
By containing M cation source compounds, polyalcohol, surfactant and the first solvent mixture add under stiring Heat obtains the first solution of heat；
Anion source compound containing X is mixed with the second solvent, obtains the second solution；
The first solution that second solution is injected the heat obtains reaction mixture to react；With
The reaction mixture cool down, separate, wash and/or dry, the photochromic nano material is obtained,
Wherein, M indicate selected from one of tin, indium, antimony and bismuth it is a variety of or its be selected from titanium, barium, nickel, vanadium, zinc and copper One of or a variety of combinations；O indicates oxygen atom；X indicates to be selected from and the formula MaObXcIn (MaOb) primitive being capable of shape At one of the tungstate radicle primitive of compound, molybdate primitive, vanadic acid foundation member, fluorine, chlorine, bromine and iodine it is a variety of or its with Selected from one of sulphur, carbon, phosphorus and boron or a variety of combinations, and in the formula MaObXcIn, each molar ratio for forming primitive A: b: c is (1~50): (1~50): 1；
(2) can ultraviolet blocking-up photochromic building window preparation
Photochromic nano material obtained in step (1) is dispersed in third solvent, uniform colloidal solution is obtained, Then the colloidal solution is coated uniformly on a surface of polymeric substrate film to form photochromatic layer, then in institute It states armor coated material in photochromatic layer and thus obtains photochromic building window pad pasting to form protective layer, finally will The photochromic building window pad pasting is pasted on the surface of routine building object glass pane, so that it is photochromic to obtain adhesive film type Building window, or
Photochromic nano material obtained in step (1) is being had with the building window material for being used to prepare building window Or without uniformly mixing in the presence of third solvent, obtain blend；Then by the blend molding, photochromic building is obtained Object window blank；Finally obtained photochromic building window blank is cut, grinding and buffing processing, to obtain one The photochromic building window of body formula.
In a preferred embodiment, the photochromic material formula MaObXcIn, each molar ratio a for forming primitive: B: c is (1~20): (1~30): 1.
In a preferred embodiment, the polyalcohol is selected from oleyl alcohol, glycerine, pentaerythrite, xylitol, mannitol With one of sorbierite or a variety of；
The surfactant is selected from neopelex, cetyl trimethylammonium bromide, ethylenediamine tetra-acetic acid In disodium, polyvinylpyrrolidone, lauroyl glutamate, sodium stearyl sulfate and sodium sulfate of polyethenoxy ether of fatty alcohol It is one or more；
First solvent and second solvent are independently from each other C1-6Alkanol, deionized water, oleyl amine, hexamethylene With one of oleic acid or a variety of.
In a preferred embodiment, the third solvent is selected from water, ethyl alcohol, ethyl acetate, toluene, acetone, second two One of amine, three ethyl alcohol and acetonitrile are a variety of.
In a preferred embodiment, the material of the polymeric substrate film or the protective layer material independently selected from Colombia's resin, polyurethane, polyvinyl resin, acrylic resin, acrylic resin, polycarbonate, poly-methyl methacrylate Ester, Kynoar, polytetrafluoroethylene (PTFE), polyvinyl butyral, polyvinyl butyral, polyethylene terephthalate and One of dimethyl silicone polymer is a variety of.
In a preferred embodiment, the method for coating the colloidal solution and/or the protective layer material is selected From one of silk-screen printing, spraying, spin coating, dip coated, lifting film, round brush, calendering and curtain coating or a variety of.
In a preferred embodiment, the building window material is selected from tempered glass, Colombia's resin, poly- ammonia Ester, polyvinyl resin, acrylic resin, acrylic resin, polycarbonate, polymethyl methacrylate, Kynoar, poly- four One of vinyl fluoride, polyvinyl butyral, polyethylene terephthalate and dimethyl silicone polymer are a variety of.
In a preferred embodiment, it is selected from for the method for the blend molding and prolongs molded method, compression moulding One of method, extrinsion pressing, injection moulding, casting moulding and blow molding method are a variety of；Preferably, the building Object window blank with a thickness of 5 μm~20mm；Preferably, edge shape of the building window blank after cutting is selected from straight line One of type, fold-line-shaped, waveform and arc line shaped are a variety of；Preferably, the building window blank is after grinding and buffing Finish reach mirror surface grade.
On the other hand, the present invention provides by the above method prepare can ultraviolet blocking-up photochromic building Window, the photochromic building window can block 80% or more ultraviolet light, and can become transparent in strong illumination Dead color can restore colorless and transparent state in no strong illumination to reduce transmitance.
On the other hand, the present invention provides it is above-mentioned can ultraviolet blocking-up photochromic building window application, it is described Photochromic building window be used for make can ultraviolet blocking-up building window.
The present invention provides can the photochromic material of ultraviolet blocking-up and the preparation method of photochromic building window.This The photochromic building window of invention preparation can block 80% or more ultraviolet light, especially can be changed to transparent in strong illumination Dead color reduces transmitance；It can restore colorless and transparent state again in no strong illumination.In addition, of the invention blocking is ultraviolet The photochromic building window of line is suitable for production building window etc..
Detailed description of the invention
Fig. 1 be the adhesive film type that is prepared according to one embodiment of the invention can ultraviolet blocking-up photochromic building window Structural schematic diagram；
Fig. 2 be according to one embodiment of the invention prepare can ultraviolet blocking-up photochromic building window in difference Light transmittance curve figure when state；
Fig. 3 be the adhesive film type that is prepared according to another embodiment of the invention can ultraviolet blocking-up photochromic building The structural schematic diagram of window；
Fig. 4 be the integral type that is prepared according to another embodiment of the invention can ultraviolet blocking-up photochromic building The structural schematic diagram of window.
Specific embodiment
The present invention relates to the use of general formula is MaObXcCan the photochromic nano material of ultraviolet blocking-up can be blocked to prepare The photochromic building window of ultraviolet light, wherein M indicate selected from one of tin, indium, antimony and bismuth it is a variety of or its be selected from One of titanium, barium, nickel, vanadium, zinc and copper or a variety of combinations；O indicates oxygen atom；X indicates to be selected from and the formula MaObXcIn (MaOb) primitive is capable of forming in tungstate radicle primitive, molybdate primitive, vanadic acid foundation member, fluorine, chlorine, bromine and the iodine of compound It is one or more or its with selected from one of sulphur, carbon, phosphorus and boron or a variety of combinations, the photochromic material general formula MaObXcIn, each molar ratio a: b: c for forming primitive is (1~50): (1~50): 1, preferably (1~20): (1~30): 1.
In the method for the invention, firstly, preparing general formula is MaObXcCan ultraviolet blocking-up photochromic nano material Material, comprising the following steps:
By containing M cation source compounds, polyalcohol, surfactant and the first solvent mixture add under stiring Heat obtains the first solution of heat；
Anion source compound containing X is mixed with the second solvent, obtains the second solution；
The first solution that second solution is injected the heat obtains reaction mixture to react；
The reaction mixture cool down, separate, wash and/or dry, obtain it is described can ultraviolet blocking-up light Mutagens color nano material.
As used in this article, statement " M indicate selected from one of tin, indium, antimony and bismuth it is a variety of or its with selected from titanium, One of barium, nickel, vanadium, zinc and copper or a variety of combinations " means that M can be only one of tin, indium, antimony and bismuth or a variety of, Simultaneously M may be one of tin, indium, antimony and bismuth or it is a variety of be selected from one of titanium, barium, nickel, vanadium, zinc and copper or a variety of Cationic source combination.In the case where M is that the cationic source combines, mole coefficient a is to own in cationic source combination The sum of molal quantity of atom.
As used in this article, " X indicates to be selected from and the formula M for statementaObXcIn (MaOb) primitive is capable of forming chemical combination One of tungstate radicle primitive, molybdate primitive, vanadic acid foundation member, fluorine, chlorine, bromine and iodine of object or it is a variety of or its with selected from sulphur, One of carbon, phosphorus and boron or a variety of combinations " mean X can be only tungstate radicle primitive, molybdate primitive, vanadic acid foundation member, One of fluorine, chlorine, bromine and iodine are a variety of, at the same X may be tungstate radicle primitive, molybdate primitive, vanadic acid foundation member, fluorine, One of chlorine, bromine and iodine a variety of are combined with selected from one of sulphur, carbon, phosphorus and boron or a variety of anion sources.Here, Shen It asks someone it is noted that these primitives are separate single in the case where X is tungstate radicle primitive, molybdate primitive, vanadic acid foundation member Member or atomic group, and the metallic atom and O atom for including in these primitives all belong to the X in general formula, and cannot return respectively Belong to the formula MaObXcIn M and O.In the case where X is that the anion source combines, mole coefficient c is the anion source The sum of the molal quantity of all primitives in combination.
The cation source compounds containing M are preferably stannide, bismuthide, antimonide and indium compound, more preferably on State the trivalent compound, 4 valence compounds or 5 valence compounds of metal, the soluble trivalent compound of more preferably above-mentioned metal, 4 Valence compound or 5 valence compounds, specifically can be, for example, tin/bismuth/antimony/indium chloride, tin/bismuth/antimony/indium acetate, tin/bismuth/ Antimony/indium nitrate, tin/bismuth/antimony/indium citrate etc..
The polyalcohol is not particularly limited in the present invention, preferably pentaerythrite, neopentyl glycol, cinnamyl alcohol, three hydroxyl first One of base ethane, glycerine, xylitol, oleyl alcohol, mannitol and sorbierite are a variety of, more preferably oleyl alcohol, glycerine, season Penta tetrol, xylitol, mannitol and sorbierite one or more, most preferably oleyl alcohol, glycerine, xylitol and mannitol It is one or more.
Surfactant of the present invention is not particularly limited, preferably lignosulfonates, neopelex, ten Six alkyl trimethyl ammonium bromides, heavy alkylbenzene sulfonate, alkylsulfonate, disodium ethylene diamine tetraacetate, polyvinylpyrrolidone, Lauroyl glutamate, sodium stearyl sulfate and sodium sulfate of polyethenoxy ether of fatty alcohol, more preferably dodecyl benzene sulfonic acid Sodium, cetyl trimethylammonium bromide, disodium ethylene diamine tetraacetate, polyvinylpyrrolidone, lauroyl glutamate, octadecane One or more, the most preferably cetyl trimethylammonium bromide, second of base sodium sulphate and sodium sulfate of polyethenoxy ether of fatty alcohol Edetate disodium, polyvinylpyrrolidone and neopelex it is one or more.
The additional amount of Surfactant of the present invention is not particularly limited, the surfactant and the M cationic source The mass ratio of compound is preferably (1~2000): 20, more preferably (1~1000): 20, more preferably (1~500): 20, most Preferably (1~150): 20.
First and second organic solvent can be independently selected from alcohols, pentane, deionized water, acetone, oleyl amine, ten One of eight alkene, hexamethylene and oleic acid are a variety of, more preferably alcohols, deionized water, oleyl amine, oleic acid, hexamethylene and 18 One of alkene is a variety of, most preferably one of alcohols, deionized water, oleyl amine, oleic acid and octadecylene or a variety of.
The mass ratio of first solvent and the M cation source compounds is preferably (1~2000): 10, more preferably (1~1800): 10, most preferably (1~1200): 10.
The yin source compound preferably includes the tungstates, molybdate or potassium vanadate of sodium, potassium and ammonium；Chlorination tricresyl phosphate Sodium；Vanadium chloride；Sodium, potassium, manganese, barium, copper, magnesium and ammonium one of halide such as potassium fluoride, potassium chloride etc. or a variety of, more preferably For potassium tungstate, potassium molybdate, potassium vanadate, sodium tungstate, sodium molybdate, sodium vanadate, ammonium tungstate, ammonium molybdate, ammonium vanadate, chlorination tricresyl phosphate Sodium, vanadium chloride, potassium fluoride, potassium chloride, potassium bromide, potassium iodide, sodium fluoride, sodium chloride, sodium bromide, sodium iodide, ammonium fluoride, chlorination One of ammonium, ammonium bromide and ammonium iodide are a variety of, most preferably potassium tungstate, potassium molybdate, potassium vanadate, sodium tungstate, sodium molybdate, vanadium Sour sodium, sodium tungstate, sodium molybdate, ammonium vanadate, Efficacious Disinfeitant, vanadium chloride, potassium chloride, potassium bromide, potassium iodide, sodium chloride, bromine Change one of sodium, sodium iodide, ammonium chloride, ammonium bromide and ammonium iodide or a variety of.
The mass ratio of second solvent and the negative source compound is preferably (1~1500): 10, more preferably (1~ 1300): 10, most preferably (1~1000): 10.
For the progress for guaranteeing reaction, the heating temperature of first solution is preferably 30~500 DEG C, more preferably 30~ 300 DEG C, most preferably 80~200 DEG C.
The time of first solution of the second solution injection heat is preferably 1s~12h, more preferably 1s~6h, most preferably For 1s~2h.The time of the cooling is preferably 1~180min, more preferably 1~60min, most preferably 1~30min.
The temperature of the cooling is preferably -50~50 DEG C, more preferably -20~20 DEG C, most preferably -10~10 DEG C.
Dry temperature is not particularly limited in the present invention, preferably -50~150 DEG C, more preferably -50~120 DEG C, most Preferably -50~60 DEG C.
The dry time is not particularly limited in the present invention, preferably 1~72h, more preferably 1~60h, and most preferably 8 ~for 24 hours.
Secondly, using it is above-mentioned can ultraviolet blocking-up photochromic nano material come prepare can ultraviolet blocking-up light-induced variable Color building window, comprising:
Photochromic nano material obtained as above is dispersed in third solvent, obtains uniform colloidal solution, then The colloidal solution is coated uniformly on a surface of polymeric substrate film to form photochromatic layer, then in the light On mutagens chromatograph thus armor coated material obtains photochromic building window pad pasting to form protective layer, finally will be described Photochromic building window pad pasting is pasted on the surface of routine building object glass pane, to obtain the photochromic building of adhesive film type Object window, or
Photochromic nano material obtained as above is being had or do not had with the building window material for being used to prepare building window It is uniformly mixed in the presence of third solvent, obtains blend；Then by the blend molding, photochromic building window is obtained Blank；Finally obtained photochromic building window blank is cut, grinding and buffing processing, to obtain integral type Photochromic building window.
It is noted that in the present invention, term " building window " and " building window glass " may be used interchangeably, and They not only refer to the building window manufactured with common glass material, but also refer to the material with similar light transmission function Such as building window made of resin etc..
More specifically, preparing for the photochromic building window of adhesive film type is as follows:
A) resulting photochromic nano material is dispersed in third solvent, obtains uniform colloidal solution；
B) colloidal solution is coated on the surface of polymeric substrate film, to form photochromatic layer, structure is Photochromatic layer/polymeric substrate film；
C) in the photochromatic layer thus armor coated material obtains photochromic building to form protective layer The photochromic building window pad pasting is finally pasted on the surface of routine building object glass pane, to obtain by window pad pasting The photochromic building window of adhesive film type.
In the present invention, the material of the polymeric substrate film and the protective layer material are preferably independently selected from brother's human relations Than subresin, polyurethane, polyvinyl resin, acrylic resin, acrylic resin, polycarbonate, polymethyl methacrylate, gather One in vinylidene, polytetrafluoroethylene (PTFE), polyvinyl butyral, polyethylene terephthalate and dimethyl silicone polymer Kind is a variety of, more preferably independently selected from polyurethane, unsaturated polyester (UP), acrylic resin, polycarbonate, polymethylacrylic acid Methyl esters, Kynoar, polytetrafluoroethylene (PTFE), polyvinyl butyral, polyethylene terephthalate and polydimethylsiloxanes One of alkane is a variety of, most preferably independently selected from polyurethane, unsaturated polyester (UP), acrylic resin, polycarbonate, poly- first One of base methyl acrylate, Kynoar, polytetrafluoroethylene (PTFE) and polyethylene terephthalate are a variety of.
In the present invention, the method for coating the colloidal solution and/or the protective layer material is preferably screen printing One of brush, spraying, spin coating, dip coated, lifting film, round brush, calendering and curtain coating are a variety of, more preferably screen printing One of brush, spraying, dip coated, lifting film, round brush, calendering and curtain coating are a variety of, most preferably silk-screen printing, spray One of painting, dip coated, calendering and curtain coating are a variety of.
In the present invention, it is preferred to after forming the photochromatic layer and after forming the protective layer all into Row drying.Dry mode and temperature is not particularly limited in the present invention, can such as dry for room temperature, heating, drying or air-dried, Drying temperature is preferably 5~500 DEG C, more preferably 25~300 DEG C, most preferably 25~250 DEG C.In addition, the present invention is to drying Time be not particularly limited, preferably 1~72h, more preferably 1~36h, most preferably 2~12h.
The thickness of the photochromatic layer of formation is not particularly limited in the present invention, and preferably 1~500 μm, more preferably 1~ 300 μm, more preferably 10~200 μm.
The thickness of the protective layer of formation is not particularly limited in the present invention, preferably 1~500 μm, more preferably 1~300 μ M, more preferably 10~200 μm.
The present invention pastes the mode on building window for will be formed by building window pad pasting and is not particularly limited, this Field technical staff can be pasted by conventional means such as adhesive to be realized.
More specifically, in the present invention, preparing for the photochromic building window of integral type is as follows:
A resulting photochromic nano material is mixed in mixer with building window material), is obtained uniform Blend；
B) by resulting blend molding, photochromic building window blank is obtained；
C) resulting photochromic building window blank is cut, grinding and buffing processing, obtains the integral type Photochromic building window.
In the present invention, building window material be preferably tempered glass, Colombia's resin, polyurethane, polyvinyl resin, Acrylic resin, acrylic resin, polycarbonate, polymethyl methacrylate, Kynoar, polytetrafluoroethylene (PTFE), polyethylene One of butyral, polyethylene terephthalate and dimethyl silicone polymer are a variety of, more preferably tempered glass, Polyurethane, unsaturated polyester (UP), acrylic resin, polycarbonate, polymethyl methacrylate, Kynoar, polytetrafluoroethylene (PTFE), One of polyvinyl butyral, polyethylene terephthalate and dimethyl silicone polymer are a variety of, most preferably steel Change glass, polyurethane, unsaturated polyester (UP), acrylic resin, polycarbonate, polymethyl methacrylate, Kynoar, poly- four One of vinyl fluoride and polyethylene terephthalate are a variety of.
In the present invention, depend on whether using third solvent, Gu the form of the blend can for solid/blend, One of solid-liquid blend, liquid liquid blend are a variety of.
In the present invention, third solvent be preferably water, ethyl alcohol, ethyl acetate, toluene, acetone, ethylenediamine, triethanolamine and One of acetonitrile is a variety of, more preferably deionized water, dehydrated alcohol, ethyl acetate, toluene, ethylenediamine, triethanolamine and One of acetonitrile is a variety of, most preferably in deionized water, dehydrated alcohol, ethyl acetate, toluene, ethylenediamine and triethanolamine It is one or more.
In the present invention, preferably prolong molded method for the method for the blend molding, compression moulding method, be squeezed into One of type method, injection moulding, casting moulding and blow molding method are a variety of, more preferably prolong molded method, compacting One of the method for forming, extrinsion pressing, casting moulding and blow molding method are a variety of, most preferably prolong molded method, pressure One of the method for forming, extrinsion pressing and casting moulding processed are a variety of.
The thickness of building window blank after molding is not particularly limited in the present invention, preferably 5 μm~20mm, more preferably 5 μm~10mm, most preferably 5 μm~5mm.
Preferably, sample after molding can be cut into edge shape and be selected from linear type, fold-line-shaped, waveform and arc line type One of or it is a variety of.
Photochromic building window surface quality after the grinding and buffing can reach mirror surface grade.
The photochromic material and photochromic building window, can block 80% or more ultraviolet light；In intense light irradiation It can be changed to transparent dead color when penetrating, reduce transmitance；It can restore colorless and transparent state again in no strong illumination.
It is of the invention it is above-mentioned can the photochromic building window of ultraviolet blocking-up can be used for making can ultraviolet blocking-up Photochromic building window, such as the window of residence building, office building, industrial premises.
Embodiment
In order to further illustrate the present invention, with reference to embodiments to a kind of inorganic photochromic material provided by the invention And preparation method thereof be described in detail, but it is to be understood that these embodiments are under the premise of the technical scheme of the present invention Implemented, the detailed implementation method and specific operation process are given, only for further illustrate feature of the invention and Advantage, rather than limiting to the claimed invention, protection scope of the present invention are also not necessarily limited to following embodiments.Meanwhile In the case where no in addition explanation, various source chemicals involved in present specification and equipment are purchased from market simultaneously Directly use.
Embodiment 1:BiBaO2The preparation of Br nano material and the photochromic building window of adhesive film type
Weighing the addition of 0.5g bismuth nitrate and filling the volume of 30mL deionized water is to use magnetic stirring apparatus in the three-necked bottle of 50mL Stirring 5 minutes；It weighs 1g mannitol and above-mentioned mixed liquor is added, electricity consumption heating mantle heats are to 100 DEG C；Weigh the addition of 0.6g barium acetate Above-mentioned mixed liquor continues heating stirring 10 minutes；It weighs 1g disodium ethylene diamine tetraacetate and is added to above-mentioned mixed liquor, continue to heat Stirring 30 minutes obtains the first solution until transparence is presented in solution；
Weighing the addition of 0.45g sodium bromide and filling the volume of 10mL deionized water is in the beaker of 25mL, with equipped with electric heating The magnetic stirrer of set 15 minutes obtains the second solution until transparence is presented in solution；
Second solution syringe is injected into the first solution, three heated in above-mentioned magnetic stirrer, electric heating cover After reacting 240s in neck bottle, reaction system is cooled to room temperature in ice bath；
Washing 3~5 times with dehydrated alcohol and deionized water circular centrifugal after the reaction was completed, (supercentrifuge is purchased from middle section Good Scientific Instruments Corporation, centrifugal speed 14000rpm, centrifugation time 5 minutes every time)；Finally, the freezing by sample at -50 DEG C is done It is dry in dry case (purchased from Shanghai than bright instrument manufacturing Co., Ltd).
Resulting sample is identified and tested and analyzed, determines that resulting sample is BiBaO of uniform size2Br nanometers Piece.
Weigh the BiBaO of preparation described in 1g2The spiral shell for filling that the volume of 10mL dehydrated alcohol is 25mL is added in Br nano material In mouthful bottle, with the thermostatic ultrasonic machine (instrument model: PS-40A10L) of the 240W of power at 25 DEG C ultrasound 30min, dispersed Uniform lotion；
Above-mentioned emulsion is sprayed on to the poly terephthalic acid second two purchased from market using electric paint spray gun (model: FUJ-89) Alcohol ester (PET) basement membrane surface spontaneously dries 30min, obtains one layer of photochromatic layer when room temperature is 20 DEG C；Then, it utilizes Electric paint spray gun (model: FUJ-89) sprays a strata ethylene glycol terephthalate conduct on above-mentioned photochromic film surface PET protective layer, the dry 60min in 250 DEG C of thermostatic drying chambers, obtain can ultraviolet blocking-up photochromic film pad pasting.It will The pad pasting pastes on common building object window, and the adhesive film type for obtaining structure as shown in Figure 1 (i.e. laminate structures) can block purple The photochromic building window of outside line.
Using deep ultraviolet-Visible-to-Near InfaRed spectrophotometer (model: DUV 1) to obtained skin covering of the surface laminar Photochromic translucent glass carries out light transmission rate detection, obtains the optical transmission spectra figure of Fig. 2.As can be seen from Figure 2: utilizing this The skin covering of the surface laminar photochromic translucent glass of the inorganic photochromic nano material preparation of invention is in reset condition, photochromic The light of ultraviolet band can be filtered out under state and recovery state；It, can be visible with filtration fraction meanwhile under photochromic state Light reduces the transmitance of light, weakens luminous intensity.
Embodiment 2:Sb4O5Cl2The preparation of nano material and the preparation of the photochromic building window of adhesive film type
Weighing the addition of 0.8g antimony chloride and filling the volume of 30mL deionized water is to use magnetic stirring apparatus in the three-necked bottle of 50mL Stirring 5 minutes；It weighs 0.5g xylitol and above-mentioned mixed liquor is added, electricity consumption heating mantle heats are to 150 DEG C；Weigh 1g polyethylene pyrrole Lip river Alkanone is added to above-mentioned mixed liquor, continues heating stirring 15 minutes, until transparence is presented in solution, obtains the first solution；
Weighing the addition of 0.2g sodium chloride and filling the volume of 3mL oleic acid is in the beaker of 10mL, with the magnetic for being furnished with electric heating cover Power blender stirs 25 minutes, until transparence is presented in solution, obtains the second solution；
Second solution syringe is injected into the first solution, three heated in above-mentioned magnetic stirrer, electric heating cover After reacting 80s in neck bottle, reaction system is cooled to room temperature in ice bath；
Washing 3~5 times with dehydrated alcohol and hexamethylene circular centrifugal after the reaction was completed, (supercentrifuge is purchased from good in middle section Scientific Instruments Corporation, centrifugal speed 14000rpm, centrifugation time 5 minutes every time)；Finally, the freeze-drying by sample at -50 DEG C It is dry in case (purchased from Shanghai than bright instrument manufacturing Co., Ltd).
Identification identical with above-described embodiment 1 and detection and analysis are carried out to resulting sample, determine that resulting sample is ruler Very little uniform Sb4O5Cl2CdS quantum dots.
Weigh the Sb of preparation described in 1g4O5Cl2Nano material (i.e. photochromic material) and 10g polycarbonate (i.e. macromolecule Polymer), being added to and filling the volume of 50mL toluene is in the beaker of 100mL, with the magnetic equipped with heating device for being purchased from market Power blender is heated to 85 DEG C and stirs 45min, until transparence is presented in solution, obtains finely dispersed lotion；By above-mentioned emulsion With the cast film machine purchased from market in polyethylene terephthalate (PET) basilar memebrane (i.e. PET base film) for being purchased from market Transparent thin film layer (i.e. the blended layer of photochromic material and high molecular polymer) is made on surface, utilizes the cutting for being purchased from market Machine row cutting, obtain can ultraviolet blocking-up photochromic film pad pasting.The pad pasting is pasted on common building object window, is obtained To the photochromic building window of adhesive film type of structure as shown in Figure 3 (that is, laminate structures).
To the progress of resulting adhesive film type photochromic building window and the same detection in above-described embodiment 1, obtain similar As a result, the adhesive film type photochromic translucent glass prepared using inorganic photochromic nano material of the invention in original shape The light of ultraviolet band can be filtered out under state, photochromic state and recovery state；It, can be with meanwhile under photochromic state Filtration fraction visible light reduces the transmitance of light, weakens luminous intensity.
Embodiment 3:Bi2O3WO3The preparation of the photochromic building window of preparation integral type of nano material
Weighing the addition of 0.5g bismuth nitrate and filling the volume of 30mL deionized water is to use magnetic stirring apparatus in the three-necked bottle of 50mL Stirring 5 minutes；It weighs 0.5g mannitol and above-mentioned mixed liquor is added, electricity consumption heating mantle heats are to 90 DEG C；Weigh 0.8g cetyl Trimethylammonium bromide is added to above-mentioned mixed liquor, continues heating stirring 30 minutes, until transparence is presented in solution, it is molten to obtain first Liquid；
Weighing the addition of 0.2g sodium tungstate and filling the volume of 5mL deionized water is in the beaker of 10mL, with equipped with electric heating cover Magnetic stirrer 15 minutes, until solution present transparence, obtain the second solution；
Second solution syringe is injected into the first solution, three heated in above-mentioned magnetic stirrer, electric heating cover After reacting 240s in neck bottle, reaction system is cooled to room temperature in ice bath；
Washing 3~5 times with dehydrated alcohol and deionized water circular centrifugal after the reaction was completed, (supercentrifuge is purchased from middle section Good Scientific Instruments Corporation, centrifugal speed 14000rpm, centrifugation time 5 minutes every time)；Finally, the constant temperature by sample at 60 DEG C is done It is dry in dry case.
Identification identical with above-described embodiment 1 and detection and analysis are carried out to resulting sample, determine that resulting sample is ruler Very little uniform Bi2O3WO3Nano particle.
Weigh the Bi of preparation described in 0.5g2O3WO3Nano material and 10g polytetrafluoroethylene (PTFE) are added to ball mill (instrument type Number: in DECO-PBM-V-0.4L), ball milling 1h obtains uniformly mixed mixed powder；Above-mentioned mixed uniformly powder is purchased Suppressed from the calender in market, obtain integral type can ultraviolet blocking-up photochromic building window blank, using being purchased from market Cutting machine cutting processing, the integral type of structure (i.e. integral structure) as shown in Figure 4 are carried out to obtained building window blank Photochromic building window.
To the progress of resulting integral type photochromic building window and the same detection in above-described embodiment 1, obtain similar As a result, the incorporation formula photochromic translucent glass prepared using inorganic photochromic nano material of the invention in original shape The light of ultraviolet band can be filtered out under state, photochromic state and recovery state；It, can be with meanwhile under photochromic state Filtration fraction visible light reduces the transmitance of light, weakens luminous intensity.
Other embodiments
With the program similar with above-described embodiment 1,2 or 3, the present invention can also prepare Bi5O7I nano material, InOI nanometer Material, Bi9V2O18Cl nano material, Bi9O18P2Cl nano material, Sb8O11Br2 nano material, SnO2MoO3Nano material etc. is received Rice material, and adhesive film type and/or integral type can be prepared with the program in embodiment 1 and 3 respectively using these nano materials Can ultraviolet blocking-up photochromic building window.Moreover, being carried out and above-described embodiment 1 to resulting photochromic building window In same detection, obtain similar result.
As can be seen from the above embodiments, photochromic building window prepared by the present invention can block 80% or more it is ultraviolet Line especially can be changed to transparent dead color in strong illumination, reduce transmitance；It can restore again in no strong illumination colorless and transparent State.Meanwhile the present invention has the characteristics that process flow is simple, low in cost, yield is big, is suitable for industrial production, has preferably Practical prospect.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.

Claims (10)

1. it is a kind of prepare can ultraviolet blocking-up photochromic building window method, comprising the following steps:
(1) general formula is MaObXcCan ultraviolet blocking-up photochromic nano material preparation:
By containing M cation source compounds, polyalcohol, surfactant and the first solvent mixture heat under stiring, obtain To the first solution of heat；
Anion source compound containing X is mixed with the second solvent, obtains the second solution；
The first solution that second solution is injected the heat obtains reaction mixture to react；With
The reaction mixture cool down, separate, wash and/or dry, the photochromic nano material is obtained,
Wherein, M indicate selected from one of tin, indium, antimony and bismuth it is a variety of or its in titanium, barium, nickel, vanadium, zinc and copper One or more combinations；O indicates oxygen atom；X indicates to be selected from and the formula MaObXcIn (MaOb) being capable of forming of primitive Close object one of tungstate radicle primitive, molybdate primitive, vanadic acid foundation member, fluorine, chlorine, bromine and iodine it is a variety of or its be selected from One of sulphur, carbon, phosphorus and boron or a variety of combinations, and in the formula MaObXcIn, each molar ratio a: b for forming primitive: C is (1~50): (1~50): 1；
(2) can ultraviolet blocking-up photochromic building window preparation
Photochromic nano material obtained in step (1) is dispersed in third solvent, obtains uniform colloidal solution, then The colloidal solution is coated uniformly on a surface of polymeric substrate film to form photochromatic layer, then in the light On mutagens chromatograph thus armor coated material obtains photochromic building window pad pasting to form protective layer, finally will be described Photochromic building window pad pasting is pasted on the surface of routine building object glass pane, to obtain the photochromic building of adhesive film type Object window, or
Photochromic nano material obtained in step (1) is being had or do not had with the building window material for being used to prepare building window It is uniformly mixed in the presence of third solvent, obtains blend；Then by the blend molding, photochromic building window is obtained Blank；Finally obtained photochromic building window blank is cut, grinding and buffing processing, to obtain integral type Photochromic building window.
2. preparation according to claim 1 can ultraviolet blocking-up photochromic building window method, which is characterized in that The photochromic material formula MaObXcIn, each molar ratio a: b: c for forming primitive is (1~20): (1~30): 1.
3. preparation according to claim 1 can ultraviolet blocking-up photochromic building window method, which is characterized in that
The polyalcohol is selected from one of oleyl alcohol, glycerine, pentaerythrite, xylitol, mannitol and sorbierite or a variety of；
The surfactant be selected from neopelex, cetyl trimethylammonium bromide, disodium ethylene diamine tetraacetate, One of polyvinylpyrrolidone, lauroyl glutamate, sodium stearyl sulfate and sodium sulfate of polyethenoxy ether of fatty alcohol Or it is a variety of；
First solvent and second solvent are independently from each other C1-6Alkanol, deionized water, oleyl amine, hexamethylene and oil One of acid is a variety of.
4. preparation according to claim 1 can ultraviolet blocking-up photochromic building window method, which is characterized in that The third solvent is selected from one of water, ethyl alcohol, ethyl acetate, toluene, acetone, ethylenediamine, three ethyl alcohol and acetonitrile or a variety of.
5. preparation according to claim 1 can ultraviolet blocking-up photochromic building window method, which is characterized in that The material of the polymeric substrate film or the protective layer material are independently selected from Colombia's resin, polyurethane, polyethylene tree Rouge, acrylic resin, acrylic resin, polycarbonate, polymethyl methacrylate, Kynoar, polytetrafluoroethylene (PTFE), poly- second One of enol butyral, polyvinyl butyral, polyethylene terephthalate and dimethyl silicone polymer are a variety of.
6. preparation according to claim 1 can ultraviolet blocking-up photochromic building window method, which is characterized in that For coat the colloidal solution and/or the protective layer material method be selected from silk-screen printing, spraying, spin coating, dip coated, Lift one of film, round brush, calendering and curtain coating or a variety of.
7. preparation according to claim 1 can ultraviolet blocking-up photochromic building window method, which is characterized in that The building window material is selected from tempered glass, Colombia's resin, polyurethane, polyvinyl resin, acrylic resin, acrylic acid Resin, polymethyl methacrylate, Kynoar, polytetrafluoroethylene (PTFE), polyvinyl butyral, gathers to benzene two polycarbonate One of formic acid glycol ester and dimethyl silicone polymer are a variety of.
8. preparation according to claim 1 can ultraviolet blocking-up photochromic building window method, which is characterized in that Method for the blend molding, which is selected from, prolongs molded method, compression moulding method, extrinsion pressing, injection moulding, casting One of the method for forming and blow molding method are a variety of；Preferably, the building window blank with a thickness of 5 μm~20mm；It is excellent Selection of land, edge shape of the building window blank after cutting are in linear type, fold-line-shaped, waveform and arc line shaped It is one or more；Preferably, finish of the building window blank after grinding and buffing reaches mirror surface grade.
9. by method according to any one of claims 1 to 8 prepare can ultraviolet blocking-up photochromic building window, The photochromic building window can block 80% or more ultraviolet light, and can become transparent dead color in strong illumination To reduce transmitance, and colorless and transparent state can be restored in no strong illumination.
10. it is according to claim 9 can ultraviolet blocking-up photochromic building window application, it is described photochromic to build Build object window for make can ultraviolet blocking-up building window.
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