CN105567106A - Efficient-thermal-insulation transparent polymer glue film and preparation method and application thereof - Google Patents

Efficient-thermal-insulation transparent polymer glue film and preparation method and application thereof Download PDF

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CN105567106A
CN105567106A CN201610066238.3A CN201610066238A CN105567106A CN 105567106 A CN105567106 A CN 105567106A CN 201610066238 A CN201610066238 A CN 201610066238A CN 105567106 A CN105567106 A CN 105567106A
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heat insulation
preparation
glued membrane
high heat
polymkeric substance
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CN105567106B (en
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朱秀玲
陈盈盈
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Dalian University of Technology
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Dalian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/1077—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing polyurethane
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/10779—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing polyester
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/10788—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing ethylene vinylacetate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
    • C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
    • C08F255/026—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethylene-vinylester copolymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
    • C08F261/12—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated acetals or ketals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/02—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonates or saturated polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/304—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/412—Transparent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2419/00—Buildings or parts thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2419/00—Buildings or parts thereof
    • B32B2419/06—Roofs, roof membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2607/00—Walls, panels
    • C—CHEMISTRY; METALLURGY
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    • C09J2451/00—Presence of graft polymer

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Joining Of Glass To Other Materials (AREA)

Abstract

The invention discloses an efficient-thermal-insulation transparent polymer glue film and a preparation method and application thereof. According to the preparation method, orderly microporous oxide nano particles and a vinyl resin monomer are added into a glue film resin solution, the mixture is initiated by an initiator for in-situ polymerization, and then the efficient-thermal-insulation high-transparent polymer laminated glass glue film is prepared. By the utilization of the preparation method of the efficient-thermal-insulation transparent polymer laminated glass glue film, laminated glass prepared from the glue film is good in thermal insulation, and the light transmittance reaches 92%. The preparation method of the polymer glue film is simple and convenient to implement, and the polymer glue film has important application value when applied to thermal-insulation materials for green building envelopes (such as a building curtain wall, a window, a wall, a floor and a roof) or sunlight rooms or other thermal-insulation devices.

Description

A kind of high heat insulation transparent polymkeric substance glued membrane and its preparation method and application
Technical field
The present invention relates to a kind of high heat insulation transparent polymkeric substance glued membrane and its preparation method and application, belong to technical field of polymer materials.
Background technology
China's building energy consumption accounts for about 25% of national total energy consumption, belong to high energy consumption industry, building energy consumption comprises architectural exterior-protecting construction energy consumption (window, body of wall, floor, roofing), lighting energy consumption, ventilation energy consumptions etc., wherein architectural exterior-protecting construction energy consumption is main energy consuming part.So the heat-proof quality improving architectural exterior-protecting construction is an effective way of save energy.
The Chinese government proposes the target of building energy conservation 65%, for reaching target, widely using transparent doubling glass at present, can effectively intercept extraneous IR or ultraviolet in building, keep buildings cool in summer and warm in winter, significantly promote building energy conservation efficiency.Doubling shatter proof glass is widely used in building and automobile industry with excellent properties such as its safety, sound insulation, heat insulation, uvioresistants.With regard to doubling glass, when glass material is certain, the effect of heat insulation of doubling glass depends on the heat-proof quality of intermediate coat material, so carrying out heat insulation modification to middle mould material is the key preparing heat insulation type doubling glass.Glued membrane in doubling glass, main use polyvinyl butyral acetal (PVB), ionic polymer intermediate coat (SGP), the multiple polymers such as ethylene-vinyl acetate copolymer (EVA), polyethylene terephthalate (PET) or urethane (PU), as doubling glued membrane body material, are widely used in doubling glass film, shield glass film, functional greenhouse film, packing film and the field such as hot melt adhesive, cable and wire.Sunlight primary waves strong point in visible ray, infrared and ultraviolet, wherein infrared proportion 45%, visible ray 50%, ultraviolet 5%.When not affecting ordinary ray, visible ray must be retained and intercept infrared and ultraviolet.Because infrared proportion is much larger than ultraviolet, so lagging material mainly intercepts ultrared passing.The thermal conductivity of simple glass is about 1.0W/ (m.K), the thermal conductivity that can be used as the polymeric film material of intermediate coat base material is more much lower than simple glass, inorganic nano-particle carries out modification to polymkeric substance glued membrane, effectively can prepare the lower adhesive film material of thermal conductivity.The glass clamp glued membrane of common heat insulation modifier modification, with glass cementation strength degradation, the transparency reduces; Common nanometer particle-modified glass clamp glued membrane, the transparency is better, and thermal insulation improves limited.
Summary of the invention
The thermal insulation that the present invention is directed to domestic and international doubling glass cement film is poor, the problem that transmittance is not high, provides a kind of economy, the transparent heat-insulated glued membrane of easy-operating preparation and preparation method thereof.Obtained by the present invention, polymkeric substance glued membrane transparency is high, heat-proof quality is excellent, satisfactory mechanical property, is applicable to the energy-conservation place heat-insulating heat-preserving materials such as building curtain wall, window, roof, or other heat-proof device lagging material.
As follows in order to solve the problems of the technologies described above the technical solution adopted in the present invention:
A preparation method for high heat insulation transparent polymkeric substance glued membrane, by orderly microporous oxide nanoparticle dispersion in a solvent, adds Vinylite monomer, glued membrane resin, initiator; Carry out in-situ polymerization 0.5-30h in 30 DEG C ~ 100 DEG C under being caused by initiator, except desolventizing, dry and obtain high heat insulation transparent polymkeric substance glued membrane;
Wherein, glued membrane resin, Vinylite monomer, initiator, the in order mass ratio of microporous oxide nanoparticle, solvent are 100:1 ~ 50:0.05 ~ 5:0.01 ~ 30:100 ~ 500;
The main component of described orderly microporous oxide nanoparticle is one or more in the oxide compound of indium, tin, silicon, aluminium or antimony.
Further, in technique scheme, described orderly microporous oxide nanoparticle is as follows by template synthesis: template is soluble in water, adds presoma under alkaline condition, at 20-100 DEG C of reaction 0.2-10h; Reaction terminates rear filtration, washing, ultrasonic disperse in dehydrated alcohol, acidolysis; Centrifugal, washing, vacuum-drying, namely obtains orderly microporous oxide nanoparticle; The mass ratio of template, presoma, water is: 100:300-5000:10 3~ 10 6.
Described presoma, comprises tin halide and antimony chloride, potassium antimonate, the NaSb (OH) such as the metal-salt of the indiums such as indium hydroxide, indium chloride, indium nitrate, positive quanmethyl silicate, tetraethyl orthosilicate, vinyl silicate, aluminium hydroxide, water glass, tindichloride, tin tetrachloride 6deng one or more.
Further, in technique scheme, described glued membrane resin is selected from polyvinyl butyral acetal, the one in ethylene-vinyl acetate copolymer, polyethylene terephthalate or urethane.
Further, in technique scheme, described template is one or more in anionic templates agent, positively charged ion template and neutral template, comprises 4-propyl bromide, sarcosyl, sodium laurylsulfonate, disodium ethylene diamine tetraacetate, polyoxyethylene glycol, polypropylene glycol, cetyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, polymethylmethacrylate, dimethyl tetradecyl amine.
Further, in technique scheme, described Vinylite monomer is in one in vinyl ether, vinyl acetate, vinylbenzene, vinyl toluene, methyl methacrylate, butyl methacrylate, ethyl propenoate, 2-methyl methacrylate and ethyl 2-methacrylate, isobornylene acrylate and propylene glycol diacrylate, 1,4 butanediol diacrylate or several.
Further, in technique scheme, described initiator is azo-initiator, peroxide initiator and oxidation-reduction initiator, comprise Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), ammonium persulphate, Potassium Persulphate, benzoyl peroxide, methylethyl ketone peroxide, dicumyl peroxide etc., the present invention selects wherein one or more mixture.
Further, in technique scheme, described solvent is one or more mixtures in acetone, ethyl acetate, chlorobenzene, benzene, toluene, chloroform or ethanol.
The invention provides the high heat insulation transparent polymkeric substance glued membrane that a kind of above-mentioned preparation method obtains.
Described high heat insulation transparent polymkeric substance glued membrane, when thickness is 0.4mm, the heat insulation temperature difference reaches 8-10 DEG C.
The invention provides the laminated glass of a kind of above-mentioned high heat insulation transparent polymer latex film preparation, described laminated glass visible light transmissivity is 85 ~ 92%.Heat-proof quality is good.
Adopt transparent heat-insulated doubling glass cement film prepared by method provided by the invention through experiment test, its heat-proof quality is obviously improved, and transparency is high, good mechanical property, high comprehensive performance.
Accompanying drawing explanation
Fig. 1 is hot box schematic diagram;
Fig. 2 is the particle diameter test curve figure of laser particle instrument to orderly microporous oxide nanoparticle prepared by embodiment 3;
Fig. 3 is the light transmittance curve figure of polymkeric substance glued membrane prepared by embodiment 7.
Embodiment
Specific embodiment of the invention scheme is described below in detail.Being necessary to point out embodiment only for doing further supplementary notes to the present invention, can not limiting the scope of the invention being interpreted as.
Testing tool
Laser particle analyzer DTS5101 Britain MARLVERLTDU.K.
Transmittance ultraviolet/the test of visible/near infrared spectrophotometer Lambda750s, PerkinElmer, sweep limit 190 ~ 2500nm, bandwidth 0.17 ~ 5nm continuously adjustabe.Plateholder is tested between two slide glasss.
The heat insulation temperature difference of glued membrane is test in self-control hot box (see Fig. 1, irradiation light is common infrared lamp).Be of a size of between 100mm × 100mm simple glass in two panels, glued membrane prepared by the inventive method of pressing from both sides one deck 100mm × 100mm, film thickness is about 0.4mm, then will use medical proof fabric edge sealing around doubling glass.The temperature head T of the record upper and lower both sides of doubling glass 1, upper and lower two blocks of glass are compressed by glued membrane in the middle of removing, and adopt same method to detect, the temperature head T of the record upper and lower both sides of glass 2, T 1with T 2difference is the heat insulation temperature difference.Test 4 and repeat sample, average.Film thickness is about 0.4mm.Glass is simple glass.
The detection of stripping strength is according to GB GB/T7124-2008/ISO4587:2003 test, and glued membrane is clipped between two panels slide glass and tests.
Embodiment 1
0.4kg dimethyl tetradecyl amine is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 60 DEG C of magnetic agitation.Add 2kg indium hydroxide reaction 4h.After filtration, washing, disperses product in 80L dehydrated alcohol, adds the backflow of 1.5L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
Orderly for 1kg microporous oxide nanoparticle is added reactor, adds 15L toluene, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyvinyl butyral acetal, 2kg vinylbenzene, 0.03kg benzoyl peroxide adds reactor and mixes, 25 DEG C of reactions.Proceed in mould after reaction terminates, after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 9-10 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 2
0.4kg polyoxyethylene-poly-oxypropylene polyoxyethylene copolymer is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 60 DEG C of magnetic agitation.Add 2kg tindichloride reaction 4h.After filtration, washing, disperses product in 80L dehydrated alcohol, adds the backflow of 1.5L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
Orderly for 0.5kg microporous oxide nanoparticle is added reactor, adds 15L toluene, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyethylene terephthalate, 0.03kg benzoyl peroxide, 0.5kg methyl methacrylate adds reactor and mixes, 35 DEG C of reactions.Proceed in mould after reaction terminates, after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 9 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 3
The preparation of orderly microporous oxide nanoparticle:
Sodium laurylsulfonate 0.4kg is dissolved in 150L deionized water, adds the 1.2L2MNaOH aqueous solution, 80 DEG C of magnetic agitation.Add 1.2kg indium chloride reaction 2h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 1.5L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.5kg microporous oxide nanoparticle is added reactor, adds 15L chloroform, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg ethylene-vinyl acetate copolymer, 0.02kg benzoyl peroxide adds reactor and mixes, and adds 0.5kg propylene glycol diacrylate and mixes, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 10 DEG C after tested.
Stripping strength is 50N/cm.
Embodiment 4
The preparation of orderly microporous oxide nanoparticle:
Sodium laurylsulfonate 0.4kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 60 DEG C of magnetic agitation.Add 0.8kg positive quanmethyl silicate reaction 1.5h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 1L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.8kg microporous oxide nanoparticle is added reactor, adds 10L acetone, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyvinyl butyral acetal, 0.01kg Diisopropyl azodicarboxylate adds reactor and mixes, and adds 1kg vinyl toluene and mixes, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 9 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 5
The preparation of orderly microporous oxide nanoparticle:
Cetyl trimethylammonium bromide 0.4kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 70 DEG C of magnetic agitation.Add 1kg tindichloride reaction 2h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 2L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.05kg microporous oxide nanoparticle is added reactor, adds 15L chloroform, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyvinyl butyral acetal, 0.02kg benzoyl peroxide adds reactor and mixes, and adds 0.05kg butyl methacrylate and mixes, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 10 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 6
The preparation of orderly microporous oxide nanoparticle:
4-propyl bromide 0.4kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 50 DEG C of magnetic agitation.Add 1kg tindichloride reaction 1h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 1.5L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.5kg microporous oxide nanoparticle is added reactor, adds 15L ethyl acetate, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyethylene terephthalate, 0.02kg Diisopropyl azodicarboxylate adds reactor and mixes, and 0.5kg methyl methacrylate adds reactor and mixes, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 8 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 7
The preparation of orderly microporous oxide nanoparticle:
0.4kg sodium laurylsulfonate is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 80 DEG C of magnetic agitation.Add 2kg indium hydroxide reaction 4h.After filtration, washing, disperses product in 80L dehydrated alcohol, adds the backflow of 1.5L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 1.5kg microporous oxide nanoparticle is added reactor, adds 15L toluene, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg ethylene-vinyl acetate copolymer, 0.5kg ethyl propenoate, 0.03kg benzoyl peroxide adds reactor and mixes, 30 DEG C of reactions.Proceed in mould after reaction terminates, after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 9 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 8
The preparation of orderly microporous oxide nanoparticle:
Cetyl trimethylammonium bromide 0.4kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 90 DEG C of magnetic agitation.Add 1L vinyl silicate reaction 2h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 2L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.05kg microporous oxide nanoparticle is added reactor, adds 15L ethyl acetate, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyvinyl butyral acetal, 0.02kg benzoyl peroxide adds reactor and mixes, and adds 1.5kg2-β-dimethyl-aminoethylmethacrylate and mixes, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 10 DEG C after tested.
Stripping strength is 46N/cm.
Embodiment 9
The preparation of orderly microporous oxide nanoparticle:
Disodium ethylene diamine tetraacetate 1kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 90 DEG C of magnetic agitation.Add 1L vinyl silicate reaction 2h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 2L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.05kg microporous oxide nanoparticle is added reactor, adds 15L ethyl acetate, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyvinyl butyral acetal, 0.02kg benzoyl peroxide adds reactor and mixes, and adds 1.5kg isobornylene crylic acid ester mixture evenly, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 10 DEG C after tested.
Stripping strength is 46N/cm.
Embodiment 10
The preparation of orderly microporous oxide nanoparticle:
Polyoxyethylene glycol 0.4kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 60 DEG C of magnetic agitation.Add 1L vinyl silicate reaction 2h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 2L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.08kg microporous oxide nanoparticle is added reactor, adds 15L ethyl acetate, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg ethylene-vinyl acetate copolymer, 0.02kg Potassium Persulphate adds reactor and mixes, and adds 0.1kg vinyl acetate and mixes, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 8 DEG C after tested.
Stripping strength is 49N/cm.
Embodiment 11
The preparation of orderly microporous oxide nanoparticle:
Sodium laurylsulfonate 0.4kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 60 DEG C of magnetic agitation.Add 1kg antimony chloride reaction 2h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 1.5L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.8kg microporous oxide nanoparticle is added reactor, adds 10L acetone, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyvinyl butyral acetal, 0.05kg Diisopropyl azodicarboxylate adds reactor and mixes, and adds 1kg vinyl toluene and mixes, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 9 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 12
The preparation of orderly microporous oxide nanoparticle:
0.4kg cetyl trimethylammonium bromide is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 60 DEG C of magnetic agitation.Add 2L tetraethyl orthosilicate reaction 4h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 1.5L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.2kg microporous oxide nanoparticle is added reactor, adds 15L toluene, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg ethylene-vinyl acetate copolymer, 0.03kg benzoyl peroxide, 1.2kg methyl methacrylate adds reactor and mixes, 70 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 9 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 13
The preparation of orderly microporous oxide nanoparticle:
Sodium laurylsulfonate 0.4kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 90 DEG C of magnetic agitation.Add 1kg indium hydroxide reaction 2h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 1L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 1kg microporous oxide nanoparticle is added reactor, adds 10L acetone, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyvinyl butyral acetal, 0.05kg Diisopropyl azodicarboxylate adds reactor and mixes, and adds 1.5kg ethyl propenoate and mixes, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 9 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 14
The preparation of orderly microporous oxide nanoparticle:
Polypropylene glycol 0.4kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 85 DEG C of magnetic agitation.Add 1kg indium chloride reaction 2h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 0.8L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.8kg microporous oxide nanoparticle is added reactor, adds 10L acetone, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg urethane, 0.05kg Diisopropyl azodicarboxylate adds reactor and mixes, and adds 1kg vinyl toluene and mixes, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 9 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 15
The preparation of orderly microporous oxide nanoparticle:
Sodium laurylsulfonate 0.4kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 60 DEG C of magnetic agitation.Add 1kg antimony chloride reaction 2h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 1.5L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.8kg microporous oxide nanoparticle is added reactor, adds 10L acetone, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyvinyl butyral acetal, 0.05kg Diisopropyl azodicarboxylate adds reactor and mixes, and adds 1kg vinyl toluene and mixes, 85 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 9 DEG C after tested.
Stripping strength is 48N/cm.
Embodiment 16
The preparation of orderly microporous oxide nanoparticle:
Polyoxyethylene glycol 0.8kg is dissolved in 200L deionized water, adds the 1.2L2MNaOH aqueous solution, 60 DEG C of magnetic agitation.Add 0.5kg antimony chloride reaction 2h.After filtration, washing, disperses product in dehydrated alcohol, adds the backflow of 1L concentrated hydrochloric acid.Centrifugal, washing with alcohol, vacuum-drying, obtains orderly microporous oxide nanoparticle.
The preparation of the nanometer particle-modified polymkeric substance glued membrane of microporous oxide:
Orderly for 0.8kg microporous oxide nanoparticle is added reactor, adds 10L chlorobenzene, rapid stirring or the ultrasonic nanoparticle that makes dispersed; By 5kg polyvinyl butyral acetal, 0.05kg Diisopropyl azodicarboxylate adds reactor and mixes, and adds 0.2kg vinyl toluene and mixes, 100 DEG C of reactions.Reaction end proceeds in mould, and after surface skining, dry solidification, obtains high heat insulation transparent polymkeric substance glued membrane.
By above-mentioned high heat insulation transparent polymer latex film preparation doubling glass.
The heat insulation temperature difference of glued membrane reaches 9 DEG C after tested.
Stripping strength is 48N/cm.

Claims (10)

1. a preparation method for high heat insulation transparent polymkeric substance glued membrane, is characterized in that: by orderly microporous oxide nanoparticle dispersion in a solvent, adds Vinylite monomer, glued membrane resin, initiator; Carry out in-situ polymerization 0.5-30h in 30 DEG C ~ 100 DEG C under being caused by initiator, except desolventizing, dry and obtain high heat insulation transparent polymkeric substance glued membrane;
Wherein, glued membrane resin, Vinylite monomer, initiator, the in order mass ratio of microporous oxide nanoparticle, solvent are 100:1 ~ 50:0.05 ~ 5:0.01 ~ 30:100 ~ 500;
The main component of described orderly microporous oxide nanoparticle is one or more in the oxide compound of indium, tin, silicon, aluminium or antimony.
2. the preparation method of high heat insulation transparent polymkeric substance glued membrane according to claim 1, it is characterized in that: described orderly microporous oxide nanoparticle is as follows by template synthesis: template is soluble in water, presoma is added, at 20-100 DEG C of reaction 0.2-10h under alkaline condition; Reaction terminates rear filtration, washing, ultrasonic disperse in dehydrated alcohol, acidolysis; Centrifugal, washing, vacuum-drying, namely obtains orderly microporous oxide nanoparticle; The mass ratio of template, presoma, water is: 100:300-5000:10 3~ 10 6.
Described presoma, comprises tin halide and antimony chloride, potassium antimonate, the NaSb (OH) such as the metal-salt of the indiums such as indium hydroxide, indium chloride, indium nitrate, positive quanmethyl silicate, tetraethyl orthosilicate, vinyl silicate, aluminium hydroxide, water glass, tindichloride, tin tetrachloride 6deng one or more.
3. the preparation method of a kind of high heat insulation transparent doubling glass cement film according to claim 1, is characterized in that described glued membrane resin is selected from polyvinyl butyral acetal, the one in ethylene-vinyl acetate copolymer, polyethylene terephthalate or urethane.
4. the preparation method of a kind of high heat insulation transparent polymkeric substance glued membrane according to claim 2, it is characterized in that described template is one or more in anionic templates agent, positively charged ion template and neutral template, comprise 4-propyl bromide, sarcosyl, sodium laurylsulfonate, disodium ethylene diamine tetraacetate, polyoxyethylene glycol, polypropylene glycol, cetyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, polymethylmethacrylate, dimethyl tetradecyl amine.
5. the preparation method of a kind of high heat insulation transparent polymkeric substance glued membrane according to claim 1, it is characterized in that described Vinylite monomer is in one in vinyl ether, vinyl acetate, vinylbenzene, vinyl toluene, methyl methacrylate, butyl methacrylate, ethyl propenoate, 2-methyl methacrylate and ethyl 2-methacrylate, isobornylene acrylate and propylene glycol diacrylate, 1,4 butanediol diacrylate or several.
6. the preparation method of a kind of high heat insulation transparent polymkeric substance glued membrane according to claim 1, it is characterized in that described initiator is azo-initiator, peroxide initiator and oxidation-reduction initiator, comprise Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), ammonium persulphate, Potassium Persulphate, benzoyl peroxide, methylethyl ketone peroxide, dicumyl peroxide etc., the present invention selects wherein one or more mixture.
7. the preparation method of a kind of high heat insulation transparent polymkeric substance glued membrane according to claim 1, is characterized in that described solvent is one or more mixtures in acetone, ethyl acetate, chlorobenzene, benzene, toluene, chloroform or ethanol.
8. the high heat insulation transparent polymkeric substance glued membrane that preparation method obtains as described in one of claim 1 ~ 7.
9. high heat insulation transparent polymkeric substance glued membrane according to claim 8, when thickness is 0.4mm, the heat insulation temperature difference reaches 8-10 DEG C.
10. adopt the laminated glass of high heat insulation transparent polymer latex film preparation as described in claim 8 or 9, described laminated glass visible light transmissivity is 85 ~ 92%.
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CN106281189A (en) * 2016-08-18 2017-01-04 付竹兰 A kind of preparation method of hot melt laminating Special safety film
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