CN107400322A - A kind of dispersion liquid with thermochromic properties, PVB films and preparation method thereof - Google Patents
A kind of dispersion liquid with thermochromic properties, PVB films and preparation method thereof Download PDFInfo
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- CN107400322A CN107400322A CN201610339356.7A CN201610339356A CN107400322A CN 107400322 A CN107400322 A CN 107400322A CN 201610339356 A CN201610339356 A CN 201610339356A CN 107400322 A CN107400322 A CN 107400322A
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- 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
-
- 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
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- 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
- C08K3/02—Elements
- C08K3/08—Metals
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- 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
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
-
- 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
- B32B2250/02—2 layers
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- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0887—Tungsten
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The present invention relates to a kind of dispersion liquid with thermochromic properties, PVB films and preparation method thereof, including：Hypovanadic oxide powder, liquid plasticiser and dispersing aid, wherein hypovanadic oxide powder and dispersing aid are dispersed in liquid plasticiser.Relative to General Decentralized process in the present invention, dispersing aid addition is larger, so in dispersion process, its dispersing aid can form one layer of thicker thin layer on hypovanadic oxide powder surface, itself and air exclusion are opened, it is sufficient to ensure that the property retention of the hypovanadic oxide powder in subsequent high temperature extrusion is constant.After doubling glass is made, glue-line and air contact area very little containing hypovanadic oxide powder, it is sufficient to ensure that the thermocolour property retention of glass is constant for a long time.
Description
Technical field
The invention belongs to functional nano-composite material field, and in particular to a kind of doubling glass with temperature-control energy-saving function
PVB (polyvinyl butyral resin) film with thermochromic properties preparation method, available for building with automobile section
Energy.
Background technology
It is becoming tight with the day of energy supply, is all carrying out the measure of energy-saving and emission-reduction in worldwide.Such as in the seventies
After energy crisis, developed country starts to be directed to research with carrying out energy-saving building technology, and China ignores asking for this aspect
Topic.Even to this day, China's building energy conservation is horizontal lags far behind developed country.China's building energy conservation is mainly reflected in illumination at present
Economize on electricity and reduction air-conditioning power etc., in terms of being also seldom related to Energy Saving Windows at present.
The vanadium dioxide of M/R phases is a kind of transition metal oxide with phase-change characteristic, and this material is reaching one relatively
The metallic state of Tetragonal, in this process, this material can be transformed into after relatively low temperature from the semiconductor form of monoclinic phase
Optics, electricity, magnetic performance all change a lot.For optics aspect, vanadium dioxide can be from the transparent state to near-infrared
Become the reflection state of paired near-infrared, so as to reach the purpose of intelligent regulation infrared transmitting rate.In research before, people
Using this property of vanadium dioxide, the purpose that vanadium dioxide coated glass realizes infrared ray in Intelligent adjustment sunshine is prepared into.
Preparing vanadium dioxide functional layer mainly has two methods at present, and the first is the physical method using magnetron sputtering, or
The methods of person's sol-gal process, this several method was due to preparing work directly in the vanadium dioxide functional layer of one layer of pure phase of deposition on glass
The reason for skill, cost was higher, was unfavorable for large area production, and be difficult to long-time retention property.There is a method in which it is exactly to pass through
Chemical method prepares hypovanadic oxide powder, then composite coating or pad pasting use are prepared into by way of dispersion mixing, this
Method is more favorable for large area production, cheap, so being more received by the market.Patent CN102399072A,
CN102120615A, CN102464354A, CN102336528A refer to using the scattered rear film of hypovanadic oxide powder
Method, but because the selection of system, these films all do not have caking property with glass in itself in presently disclosed method, in order to
Enough uses also need to be further added by one layer of glue-line, undoubtedly which increase process, also increase cost.
It is exactly doubling glass to also have a kind of the most frequently used functional glass now, is exactly sticking using a kind of tough and tool
Resin film sticks together two panels safety glass at high temperature under high pressure, makes it have sound insulation, a series of premium properties such as explosion-proof.This
Kind glass is widely applied to high-rise glass curtain wall, automobile etc..This glass interlayer normally only possess at present every ultraviolet or
Person completely cuts off the non intelligent regulation and control such as infrared, so this material of vanadium dioxide is added into the resin bed among doubling glass makes its tool
The ability for having intelligent temperature control undoubtedly has good market prospects.
At present, Chinese patent CN103214989A discloses a kind of intelligent dimming PVB films and intelligent dimming PVB doublings
The specific preparation method of glass, its specifically disclose the nano vanadium dioxide powder with thermochromic properties is prepared into it is scattered
Liquid, then this dispersion liquid is distributed in the PVB resin with caking property, is prepared into PVB films through plastifying extrusion, so
Hot pressing and piece are prepared into intelligent dimming PVB doubling glass afterwards.But the technology have at present one it is critically important the problem of, that is,
This method must first by being dispersed in decentralized medium of nano vanadium dioxide point (such as alcohol, ketone, benzene, ester etc.) solvent,
Then mixed again with resin, but the composition requirement of actually PVB resin is very strict, makes unavoidably in this way
Substantial amounts of unrelated even harmful composition is mixed into, tremendous influence finally is caused to doubling glass performance in use.And
This method additionally must also use decentralized medium more, cause cost to improve the hidden danger with safety and environmental protection.
Also a Chinese patent CN103525320B provides another thermochromism PVB intermediate coats and its preparation side
Method, it discloses the nano vanadium dioxide powder first prepared charcoal bag and covered, squeezed at high temperature after then being mixed with plasticiser and resin
Go out film forming, then the PVB doubling glass for possessing intelligent dimming is prepared through hot pressing piece.The method avoids with PVB components
The introducing of unrelated composition, but it is in situ under a more step hydrothermal condition during preparing this carbon coating hypovanadic oxide powder
Carbon coating process, complex process degree is added, and finished films can be made to be a bit darkish in color after increasing carbon coating layer, part reduces
Powder characteristic.
The content of the invention
In view of the above-mentioned problems existing in the prior art, it is more suitable the purpose of the present invention is to propose to a kind of new price is cheaper
Close the dispersion liquid with thermochromic properties of large-scale production and the preparation method of PVB films.
On the one hand, the invention provides a kind of dispersion liquid with thermochromic properties, including：Hypovanadic oxide powder, liquid
State plasticiser and dispersing aid, wherein hypovanadic oxide powder and dispersing aid are dispersed in liquid plasticiser.Preferably, originally
The invention dispersion liquid with thermochromic properties is made up of hypovanadic oxide powder, liquid plasticiser and dispersing aid.
It is preferred that the mass ratio of the hypovanadic oxide powder and dispersing aid and plasticiser is (0.0001-0.025)：
(0.0001-0.01)：1, be preferably (0.005-0.015)：(0.003-0.009)：1.
It is preferred that the hypovanadic oxide powder is M phases or/and R phases, its three dimension scale is 40-200nm, preferably small
In 80nm, phase transition temperature is 10-90 DEG C adjustable.
It is preferred that the hypovanadic oxide powder includes dopant, the dopant be tungsten, molybdenum, niobium, tantalum, chromium, zirconium,
At least one of fluorine, phosphorus, doping molar content are 0-10%.
It is preferred that the plasticiser is triethylene glycol two (2 ethyl hexanoic acid) ester, DPG dibenzoic acid is cruel, adjacent benzene two
Formic acid dibutyl ester (DBP), diisobutyl phthalate (DBIP), phthalic acid two (butoxy second) ester
(DBEP), at least one of phthalic acid two (methoxyl group second) ester (DMEP), SA dibutyl ester.
It is preferred that the dispersing aid is polyvinylpyrrolidone, silane coupler, titanate coupling agent, organosilicon tree
At least one of fat, polyacrylate.
Present invention also offers a kind of preparation method of the PVB films with thermochromic properties, including：Will be described scattered
Liquid mixes extrusion molding with PVB resin and obtains the PVB films with thermochromic properties.
It is preferred that it is preferred that the dispersion liquid and the mass ratio of PVB resin are (2:8)~(4:6).
It is preferred that temperature during extrusion is 100 DEG C -200 DEG C.
On the other hand present invention also offers a kind of PVB films with thermochromic properties prepared by the above method.
Another aspect, the present invention provide a kind of preparation method of thermochromism doubling glass, including：
PVB films with thermochromic properties are prepared according to the above method；And
The PVB films of gained are closed into piece in two sheet glass intermediary press at a temperature of 100 DEG C -200 DEG C, prepared with thermal discoloration
The PVB doubling glass of energy.
The present invention also provides a kind of thermochromism doubling glass for including the above-mentioned PVB films with thermochromic properties.
The present invention is following using directly having the method that nano vanadium dioxide powder is dispersed in liquid plasticiser
Advantage：
(1) composition unrelated with PVB components will not be introduced, unrelated component (such as ethanol) is greatly avoided and doubling glass is used
The influence of performance；
(2) compared to the method for patent CN103525320B carbon coating vanadium dioxide, preparation process of the present invention is completely without being related to
This high-temperature high-voltage reaction container of hydro-thermal reaction, reduce cost and reduce the security risk in production.And will not introduce carbon this
The deeper impurity of kind color, can improve the performances such as optical property, the glossiness of doubling glass；
(3) relative to General Decentralized process in the present invention, dispersing aid addition is larger, so in dispersion process, it disperses to help
Agent can form one layer of thicker thin layer on hypovanadic oxide powder surface, it be opened with air exclusion, it is sufficient to ensure to squeeze in subsequent high temperature
The property retention of hypovanadic oxide powder is constant during going out.After doubling glass is made, glue-line and sky containing hypovanadic oxide powder
Gas contact area very little, it is sufficient to ensure that the thermocolour property retention of glass is constant for a long time.
Brief description of the drawings
Fig. 1 is the spectra at high and low temperatures figure of thermochromism doubling glass prepared by the embodiment of the present invention 1.
Embodiment
The present invention is further illustrated below in conjunction with following embodiments, it should be appreciated that following embodiments are merely to illustrate
The present invention, it is not intended to limit the present invention.
The present invention is prepared for one kind with plasticiser, nano vanadium dioxide powder, dispersing aid etc. for raw material has thermochromism
The dispersion liquid of performance.Method used in the present invention is that pure nano vanadium dioxide directly is uniformly dispersed in into liquid plasticiser
In, it is only necessary to a small amount of dispersing aid is added, by ultrasound, is sheared, grinding, ball milling or sand milling are scattered, can prepare
The dispersion liquid of good dispersion property.Then PVB film of the extrusion with thermochromic properties is mixed with PVB resin, finally by
Hot pressing piece prepares the doubling glass with thermochromic properties.Illustrate to following exemplary provided by the invention there is thermotropic
The preparation method of the dispersion liquid of color performance.
By hypovanadic oxide powder, plasticiser, dispersing aid obtains dispersion liquid after uniformly mixing.Wherein described plasticiser can be
Triethylene glycol two (2 ethyl hexanoic acid) ester, DPG dibenzoic acid are cruel, dibutyl phthalate (DBP), phthalic acid two
Isobutyl ester (DBIP), phthalic acid two (butoxy second) ester (DBEP), phthalic acid two (methoxyl group second) ester (DMEP), certain herbaceous plants with big flowers
At least one of adipate.The dispersing aid can be polyvinylpyrrolidone, all kinds of silane couplers, all kinds of metatitanic acids
At least one of ester coupling agent, organic siliconresin, polyacrylate.The hypovanadic oxide powder and dispersing aid and plasticiser
Mass ratio can be (0.0001-0.025)：(0.0001-0.01)：1, be preferably (0.005-0.015)：(0.003-
0.009)：1.The mass ratio of hypovanadic oxide powder and dispersing aid can be 0.1:1~10：1, preferably 1:1~2.5:1.
As by hypovanadic oxide powder, plasticiser, the mixed uniformly method of dispersing aid, include but is not limited to ultrasound, cut
Cut, grind, ball milling or sand milling etc..Incorporation time can be 2-40 hours.
Above-mentioned hypovanadic oxide powder be M phases (monoclinic crystal body phase)/R phases (Rutile Type) nano-powder, its three-dimensional chi
Spend for 35-200nm, preferably less than 80nm.Phase transition temperature can be 20-90 DEG C adjustable., can when choosing hypovanadic oxide powder
For pure hypovanadic oxide powder.Dopant is may also include, the dopant can be in tungsten, molybdenum, niobium, tantalum, chromium, zirconium, fluorine, phosphorus
At least one, doping molar content can be 0-10%, preferably 0.1-5%.By mixing dopant, vanadium dioxide can be adjusted
Phase transition temperature.In addition, the hypovanadic oxide powder of the present invention is preferably not contain clad, so as to simplify technique and avoid
Introduce the deeper impurity of color.
The present invention is prepared for a kind of PVB films with thermochromic properties with PVB resin, the dispersion liquid of preparation for raw material
(PVB intermediate layers).Specifically, dispersion liquid is well mixed with PVB resin to obtain compound B.The dispersion liquid with
The mass ratio of PVB resin can be (2:8)~(4:6).In addition the dispersion liquid with thermochromic properties that prepared by the present invention is also
PET film or film are prepared available for material mixings such as PET.
The heated thawing extrusion moldings of compound B are obtained into the PVB films with thermochromic properties.It is specific next
Say, single screw extrusion machine can be added mixture into extrusion is plastified under the conditions of 100 DEG C -200 DEG C, it is suitable directly to be extruded by mould
The PVB films of size.The thickness of PVB films can be 0.38mm-5mm.
Present invention also offers a kind of PVB films with thermochromic properties, it can be made by the above method.
The present invention by the PVB films with thermochromic properties prepared at a temperature of 100 DEG C -200 DEG C in two sheet glass
Intermediary press closes piece, prepares the PVB doubling glass with thermochromic properties.Thickness of glass can be but be not limited only to
0.1mm-30mm, preferably 1mm-30mm.
Embodiment of illustrating further below is to describe the present invention in detail.It will similarly be understood that following examples are served only for this hair
It is bright to be further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential modifications and adaptations that the above is made belong to protection scope of the present invention.The specific temperature of following examples,
Time, inventory etc. are also only an examples in OK range, i.e., those skilled in the art can be done by this paper explanation
Selected in suitable scope, and do not really want to be defined in the concrete numerical value of hereafter example.
Method of testing：
Transmitance：Ultraviolet-visible-near infrared spectrometer is characterized (HIT, UH4150), test wavelength scope
300-2600nm, sweep speed 600nm/min.
Embodiment 1
(1) take 10 grams undoped with hypovanadic oxide powder；Diameter of particle is 80nm；
(2) 1000 grams of plasticiser dibutyl phthalates (DBP) are taken, add silane coupler γ-methacryloxy thereto
1 gram of propyl trimethoxy silicane, and nano vanadium dioxide powder is added thereto and is stirred, obtain compound；
(3) add mixture into sand mill sand milling and obtain dispersion liquid in 35 hours；
(4) 1000 grams and 2400 grams PVB resins of dispersion liquid are mixed 30 minutes, obtains well mixed powder material B；
(5) powder material B is added into single screw extrusion machine, 150 DEG C of extrusion temperature, film extrusion, obtains that there are thermochromic properties
PVB films, measured through slide measure instrument or method, the PVB film stock thickness is 0.79mm；
(6) PVB that will there are thermochromic properties obtained by two panels simple glass (thickness 1mm) and the present embodiment using tablet press machine
Film pressurizeed at 120 DEG C close piece produce the PVB doubling glass with thermochromic properties.After tested, its visual transmitance
For 70%.
Embodiment 2
(1) hypovanadic oxide powder of 5 grams of Doped Tungstens is taken；Diameter of particle is 35nm；Witch culture amount is mol ratio 1%；
(2) 1000 grams of plasticiser dibutyl phthalates (DBP) are taken, add silane coupler 3- glycidol ether epoxides thereto
1 gram of propyl trimethoxy silicane, and the nano vanadium dioxide powder of Doped Tungsten is added thereto and is stirred, mixed
Material；
(3) add mixture into sand mill sand milling and obtain dispersion liquid in 35 hours；
(4) 1000 grams and 2400 grams PVB resins of dispersion liquid are mixed 30 minutes, obtains well mixed powder material B；
(5) powder material B is added into single screw extrusion machine, 150 DEG C of extrusion temperature, film extrusion, obtains that there are thermochromic properties
PVB films, measured through slide measure instrument or method, the PVB film stock thickness is 0.90mm；
(6) PVB that will there are thermochromic properties obtained by two panels simple glass (thickness 1mm) and the present embodiment using tablet press machine
Film pressurizeed at 120 DEG C close piece produce the PVB doubling glass with thermochromic properties.After tested, its visual transmitance
For 78%.
Embodiment 3
(1) take 0.1 gram undoped with hypovanadic oxide powder；Diameter of particle is 80nm；
(2) 1000 grams of plasticiser SA dibutyl esters are taken, add silane coupler 3- glycydoxy trimethoxies thereto
1 gram of base silane, and nano vanadium dioxide powder is added thereto and is stirred, obtain compound；
(3) add mixture into sand mill sand milling and obtain dispersion liquid in 35 hours；
(4) 1000 grams and 2400 grams PVB resins of dispersion liquid are mixed 30 minutes, obtains well mixed powder material B；
(5) powder material B is added into single screw extrusion machine, 150 DEG C of extrusion temperature, film extrusion, obtains that there are thermochromic properties
PVB films, measured through slide measure instrument or method, the PVB film stock thickness is 0.82mm；
(6) PVB that will there are thermochromic properties obtained by two panels simple glass (thickness 1mm) and the present embodiment using tablet press machine
Film pressurizeed at 120 DEG C close piece produce the PVB doubling glass with thermochromic properties.After tested, its visual transmitance
For 91%.
Embodiment 4
(1) take 25 grams undoped with hypovanadic oxide powder；Diameter of particle is 80nm；
(2) 1000 grams of plasticiser dibutyl phthalates (DBP) are taken, add silane coupler γ-methacryloxy thereto
10 grams of propyl trimethoxy silicane, and nano vanadium dioxide powder is added thereto and is stirred, obtain compound；
(3) add mixture into sand mill sand milling and obtain dispersion liquid in 35 hours；
(4) 1000 grams and 2400 grams PVB resins of dispersion liquid are mixed 30 minutes, obtains well mixed powder material B；
(5) powder material B is added into single screw extrusion machine, 150 DEG C of extrusion temperature, film extrusion, obtains that there are thermochromic properties
PVB films, measured through slide measure instrument or method, the PVB film stock thickness is 0.82mm；
(6) PVB that will there are thermochromic properties obtained by two panels simple glass (thickness 1mm) and the present embodiment using tablet press machine
Film pressurizeed at 120 DEG C close piece produce the PVB doubling glass with thermochromic properties.After tested, its visual transmitance
For 51%.
Embodiment 5
(1) take 0.1 gram undoped with hypovanadic oxide powder；Diameter of particle is 80nm；
(2) 1000 grams of plasticiser dibutyl phthalates (DBP) are taken, add silane coupler γ-methacryloxy thereto
0.1 gram of propyl trimethoxy silicane, and nano vanadium dioxide powder is added thereto and is stirred, obtain compound；
(3) add mixture into sand mill sand milling and obtain dispersion liquid in 35 hours；
(4) 1000 grams and 2400 grams PVB resins of dispersion liquid are mixed 30 minutes, obtains well mixed powder material B；
(5) powder material B is added into single screw extrusion machine, 150 DEG C of extrusion temperature, film extrusion, obtains that there are thermochromic properties
PVB films, measured through slide measure instrument or method, the PVB film stock thickness is 0.83mm；
(6) PVB that will there are thermochromic properties obtained by two panels simple glass (thickness 1mm) and the present embodiment using tablet press machine
Film pressurizeed at 120 DEG C close piece produce the PVB doubling glass with thermochromic properties.After tested, its visual transmitance
For 97%.
Fig. 1 is the spectra at high and low temperatures figure of thermochromism doubling glass prepared by the embodiment of the present invention 1.From fig. 1, it can be seen that this
Thermochromism doubling glass has thermochromic properties made from invention.
Comparative example 1
(1) take 10 grams undoped with hypovanadic oxide powder；Diameter of particle is 80nm；
(2) 1000 grams of plasticiser dibutyl phthalates (DBP) are taken, add silane coupler γ-methacryloxy thereto
0.01 gram of propyl trimethoxy silicane, and nano vanadium dioxide powder is added thereto and is stirred, obtain compound；
(3) add mixture into sand mill sand milling and obtain dispersion liquid in 35 hours；
(4) 1000 grams and 2400 grams PVB resins of dispersion liquid are mixed 30 minutes, obtains well mixed powder material B；
(5) powder material B is added into single screw extrusion machine, 150 DEG C of extrusion temperature, film extrusion, obtains that there are thermochromic properties
PVB films, measured through slide measure instrument or method, the PVB film stock thickness is 0.76；
(6) PVB that will there are thermochromic properties obtained by two panels simple glass (thickness 1mm) and this comparative example using tablet press machine
Film pressurizeed at 120 DEG C close piece produce the PVB doubling glass with thermochromic properties.After tested, its visual transmitance
For 61%.
Claims (10)
- A kind of 1. dispersion liquid with thermochromic properties, it is characterised in that including：Hypovanadic oxide powder, liquid plasticiser and dispersing aid, wherein hypovanadic oxide powder and dispersing aid are dispersed in liquid plasticiser.
- 2. dispersion liquid according to claim 1, it is characterised in that the mass ratio of the hypovanadic oxide powder and dispersing aid and plasticiser is（0.0001-0.025）：（0.0001-0.01）：1, be preferably（0.005-0.015）：（0.003-0.009）：1.
- 3. dispersion liquid according to claim 1 or 2, it is characterised in that the hypovanadic oxide powder is M/R phases, and its three dimension scale is 35-200 Nm, preferably less than 80 nm, phase transition temperature are 10-90 DEG C adjustable.
- 4. according to the dispersion liquid described in claim any one of 1-3, it is characterised in that the hypovanadic oxide powder includes dopant, and the dopant is at least one of tungsten, molybdenum, niobium, tantalum, chromium, zirconium, fluorine, phosphorus, and doping molar content is 0-10%.
- 5. according to the dispersion liquid described in claim any one of 1-4, it is characterised in that the plasticiser is triethylene glycol two（2 ethyl hexanoic acid）Ester, DPG dibenzoic acid are cruel, dibutyl phthalate, diisobutyl phthalate, phthalic acid two（Butoxy second）Ester, phthalic acid two（Methoxyl group second）At least one of ester, SA dibutyl ester.
- 6. according to the dispersion liquid described in claim any one of 1-5, it is characterised in that the dispersing aid is at least one of polyvinylpyrrolidone, silane coupler, titanate coupling agent, organic siliconresin, polyacrylate.
- A kind of 7. preparation method of the PVB films with thermochromic properties, it is characterised in that including：Dispersion liquid according to any one of claim 1-6 is mixed into extrusion molding with PVB resin and obtains the PVB films with thermochromic properties.
- 8. preparation method according to claim 7, it is characterised in that the dispersion liquid and the mass ratio of PVB resin are（2:8）~（4:6）；Furthermore it is preferred that temperature during extrusion is 100 DEG C -200 DEG C.
- A kind of 9. PVB films with thermochromic properties prepared by preparation method according to claim 7 or 8.
- A kind of 10. preparation method of thermochromism doubling glass, it is characterised in that including：Preparation method according to claim 7 or 8 prepares the PVB films with thermochromic properties；AndThe PVB films of gained are closed into piece in two sheet glass intermediary press at a temperature of 100 DEG C -200 DEG C, prepare the PVB doubling glass with thermochromic properties.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610339356.7A CN107400322A (en) | 2016-05-20 | 2016-05-20 | A kind of dispersion liquid with thermochromic properties, PVB films and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610339356.7A CN107400322A (en) | 2016-05-20 | 2016-05-20 | A kind of dispersion liquid with thermochromic properties, PVB films and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109880553A (en) * | 2019-03-22 | 2019-06-14 | 苏州量子新材料科技有限公司 | A kind of PVB or EVA film of thermochromism |
| CN111347647A (en) * | 2020-03-27 | 2020-06-30 | 江苏奥天利新材料有限公司 | Preparation method of temperature-control color-changing PVB intermediate film |
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| CN102674713A (en) * | 2012-05-07 | 2012-09-19 | 信义超薄玻璃(东莞)有限公司 | Thermochromic laminated glass and manufacturing method thereof |
| CN103525320B (en) * | 2013-10-16 | 2015-08-19 | 中国科学院上海硅酸盐研究所 | Thermochromism PVB intermediate coat and preparation method thereof |
| CN105358502A (en) * | 2013-08-30 | 2016-02-24 | 积水化学工业株式会社 | Intermediate film for laminated glass, and laminated glass |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102674713A (en) * | 2012-05-07 | 2012-09-19 | 信义超薄玻璃(东莞)有限公司 | Thermochromic laminated glass and manufacturing method thereof |
| CN105358502A (en) * | 2013-08-30 | 2016-02-24 | 积水化学工业株式会社 | Intermediate film for laminated glass, and laminated glass |
| CN103525320B (en) * | 2013-10-16 | 2015-08-19 | 中国科学院上海硅酸盐研究所 | Thermochromism PVB intermediate coat and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109880553A (en) * | 2019-03-22 | 2019-06-14 | 苏州量子新材料科技有限公司 | A kind of PVB or EVA film of thermochromism |
| CN111347647A (en) * | 2020-03-27 | 2020-06-30 | 江苏奥天利新材料有限公司 | Preparation method of temperature-control color-changing PVB intermediate film |
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