CN106750466A - reversible thermochromic film and preparation method thereof - Google Patents
reversible thermochromic film and preparation method thereof Download PDFInfo
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- CN106750466A CN106750466A CN201710025395.4A CN201710025395A CN106750466A CN 106750466 A CN106750466 A CN 106750466A CN 201710025395 A CN201710025395 A CN 201710025395A CN 106750466 A CN106750466 A CN 106750466A
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Abstract
The present invention relates to a kind of reversible thermochromic film and preparation method thereof.The reversible thermochromic film includes PET film layer and anorganic thermochromic coating liquid layer, and anorganic thermochromic coating liquid layer includes the component of following weight portion：5~130 parts of inorganic nano slurry, organic polymer disperse matrix A5~130 part, 10~120 parts of solvent orange 2 A, age resister A0.01~0.1 part.The preparation method of the reversible thermochromic film is：By modified VO2Nanometer powder, grinding distribution agent B, solvent B and age resister B stirring mixing, are positioned over the grinding of sand mill high speed, obtain inorganic nano slurry；Add in organic polymer disperse matrix A, stirring mixing sequentially adds solvent orange 2 A and age resister A, obtains anorganic thermochromic coating liquid, is coated with PET film layer.Reversible thermochromic film low cost of the invention, preparation for processing is simple, with more preferable environmental stability and service life.
Description
Technical field
The present invention relates to intelligent dimming composite film material field, and in particular to a kind of for the reversible of intelligent dimming glass
Thermochromic thin film and preparation method thereof.
Background technology
Intelligent glass be a kind of transmission that sunshine can be adjusted under the conditions of environmental stimuli or manual control, reflection or
The functional glass of absorption spectrum, the intelligent glass is generally divided into two kinds of preparation methods：One is that inductive material is made into membranaceous being combined
To unorganic glass surface or it is mixed in the middle of two-layer simple glass；Two is that glass is modified in itself using inductive material.
Intelligent glass complex process, the high cost for obtaining in view of glass is modified in itself, application example is few, the research and development of current intelligent glass with
Prepare most in the majority with first method.
Intelligent glass inductive material mainly includes thermochromism, electrochromism and gas-discoloration three types, passes through respectively
Environment temperature, extra electric field and sensitive gas stimulate to change spectral quality.For the Reversible Thermochromic Materials of intelligent glass
Mainly there are three classes：Inorganic material class, liquid crystal type, organic material class.Relative to organic thermochromic material, inorganic has more preferable
Weatherability, durability and preferably hybrid process.
Thermochromism glass is plated last layer Reversible Thermochromic Materials by simple glass and is made.In numerous inorganics
In Reversible Thermochromic Materials, the film coating based on the oxide of vanadium is the focus of people's research.VO2Film have compared with
Low temperature transmitance and very low high temperature transmitance high.By methods such as doping, can be VO2The phase transition temperature of film is reduced to
Near room temperature, can be used for the thin-film material of building window and vehicle glass, i.e. intelligent dimming glass, and control indoor temperature reaches
Effect cool in summer and warm in winter, side group reduction air conditioner load, saving energy consumption.
VO2Performance with intelligent thermoregulating, but to realize being applied in building or vehicle glass, it is necessary to solve following two
Problem：One is VO2Phase transition temperature be 68 DEG C, it is necessary to by adulterating or changing preparation method etc., by VO2Phase transition temperature drop
As little as near room temperature.Ion doping can change band gap, crystal internal stress, microstructure, vanadium ion valence state and crystal and lack
Falling into etc. factor influences VO2Thermochromic properties, that is, change thermochromic temperature.At present, for metal ion mixing, non-
Metal ion mixing and it is binary doped all have achievement in research.Such as 1988, F.C.Case deposited by electron beam evaporation method was blue precious
Ground mass has been coated with the VO that phase transition temperature is 38 DEG C on the ground2Film, wherein being doped with 0.9% W；Two is the transmission for adjusting visible ray
Than.Above-mentioned research shows VO2No matter visible light transmissivity is all relatively low before and after film phase transformation, majority both less than 40%.At present still
There is not preferable preparation method to adjust VO2Visible transmission ratio before and after thin film phase change.
The content of the invention
Based on this, a kind of nontoxic, stability of present invention offer is high, environment amenable reversible thermochromic film, can
Change according to temperature regulates and controls spectral quality, for preparing intelligent dimming glass.
The present invention also provides the preparation method of above-mentioned reversible thermochromic film.
In order to realize the purpose of the present invention, the present invention uses following technical scheme：
A kind of reversible thermochromic film, including PET film layer and it is coated on the inorganic heat of the PET film layer surface
Mutagens color coats liquid layer, and the anorganic thermochromic coating liquid layer includes the component of following weight portion：
Reversible thermochromic film of the invention, is prepared for ion doping VO first2Nanometer powder, then by grinding point
Scattered technique is prepared into nano pulp, and the macromolecule disperse matrix A compoundings with function admirable are applied as anorganic thermochromic
Covering liquid, is finally coated on polyphenylene ethyl dioctyl phthalate second diester (PET) surface and forms transparent polymer reversible thermochromic film, most
The glass of reversible thermochromic film is posted afterwards, and the glass is existing commodity unorganic glass or lucite etc., 0~
Change the light-bleed effect of each wavelength in sunshine between 70 DEG C, play the effect of intelligent dimming.The reversible thermochromic is thin
Film be based on ep-type material, service life more than 5 years, by inorganic nano-particle and macromolecule compound system, by ion
The VO of doping vario-property2Undergone phase transition at 45 DEG C or so, the transmitance of light in 380nm~2500nm wave-length coverages is substantially changed this
One special nature, so as to a kind of thermochromic thin film for temperature control response type intelligent dimming glass is obtained.The thermic for preparing
Inorganic nano-particle is uniformly embedded in organic polymer disperse matrix A in optically variable films, and apparent mass is good, it is homogeneous light to present
Yellow, and translucency is good, the reaction of optics performance of control is fast.The preparation method of the reversible thermochromic film can conveniently realize big face
Product production.
Reversible thermochromic film of the invention is by the VO after ion doping2Particle diameter in 10~30nm, its phase transformation
Temperature is reduced to 45 DEG C from 68 DEG C, and reduces VO2Crystallite dimension and reduce VO2Energy gap, the nanometer of gained
VO2Powder constitution is single, even particle size distribution, with low cost；The VO2 nano-particles of doping vario-property keep dividing for more than three months
Stability is dissipated, sedimentation phenomenon does not occur.
Reversible thermochromic film of the invention uses one or more nontoxic, stable, environment-friendly organic or nothings
Machine composite compounding is formed, by the VO of doping vario-property2, undergo phase transition at a lower temperature, the environmental stability of the system
Height, reaction rate is fast；For ambient temperature conditions change belong to autonomous generation stress behavior, it is not necessary to artificial adjustment, and reaching
To the purpose of Intelligent adjustment, belong to a kind of intelligent power saving product；It is prepared by reversible thermochromic film low cost of the invention, processing
Method is simple, with more preferable environmental stability and service life, is widely used on building or vehicle glass.
Wherein in some embodiments, the inorganic nano slurry includes the component of following weight portion：
Wherein in some embodiments, the modified VO2Nanometer powder is with the percentage by weight of the grinding distribution agent B
10:1。
Wherein in some embodiments, the modified VO2The preparation of nanometer powder comprises the following steps：
By V2O5Powder is dissolved in NaOH solution, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl and H to component A2O2Solution, stirs after solution switchs to navy blue, obtains pH value
It is 1 component B；
Add NaOH solution suspended up to solution generation to component B, add a small amount of white tungstic acid, obtain component C；
Component C is fitted into reactor, under conditions of HTHP, is reacted, room temperature is cooled to after reaction, obtained
Component D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over air blast
In drying box, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
Wherein in some embodiments, the tungsten is 1 than scope with the atom number of vanadium:100~1:20.
Wherein in some embodiments, the modified VO2The particle size range of nanometer powder is 10~30nm.
Wherein in some embodiments, the weight hundred of the inorganic nano slurry and the organic polymer disperse matrix A
Divide than being 1:1.
Wherein in some embodiments, the organic polymer disperse matrix A is polyurethane or polyacrylic acid.
A kind of preparation method of reversible thermochromic film, comprises the following steps：
First step：Following component material is provided：PET film layer and anorganic thermochromic coating liquid layer；
The anorganic thermochromic coating liquid layer includes the component of following weight portion：
The inorganic nano slurry includes the component of following weight portion：
Second step：By the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B stirring mixing, then be positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano
Slurry；
Third step：By in the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then
Solvent orange 2 A and age resister A are sequentially added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid；
Four steps：Again by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer
On, after drying, obtain reversible thermochromic film.
Wherein in some embodiments, the thickness of the reversible thermochromic film is 10 μm~50 μm.
Specific embodiment
For the ease of understanding the present invention, the present invention will be described more fully below.But, the present invention can be with perhaps
More different form is realized, however it is not limited to embodiment described herein.On the contrary, the purpose for providing these embodiments is to make
Understanding to the disclosure is more thorough comprehensive.
Unless otherwise defined, all of technologies and scientific terms used here by the article with belong to technical field of the invention
The implication that technical staff is generally understood that is identical.The term for being used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
A kind of reversible thermochromic film, including PET film layer and it is coated on the inorganic heat of the PET film layer surface
Mutagens color coats liquid layer, and the anorganic thermochromic coating liquid layer includes the component of following weight portion：
Reversible thermochromic film of the invention, is prepared for ion doping VO first2Nanometer powder, then by grinding point
Scattered technique is prepared into nano pulp, and the macromolecule disperse matrix A compoundings with function admirable are applied as anorganic thermochromic
Covering liquid, is finally coated on polyphenylene ethyl dioctyl phthalate second diester (PET) surface and forms transparent polymer reversible thermochromic film, most
The glass of reversible thermochromic film is posted afterwards, and the glass is existing commodity unorganic glass or lucite etc., 0~
Change the light-bleed effect of each wavelength in sunshine between 70 DEG C, play the effect of intelligent dimming.The reversible thermochromic is thin
Film be based on ep-type material, service life more than 5 years, by inorganic nano-particle and macromolecule compound system, by ion
The VO of doping vario-property2Undergone phase transition at 45 DEG C or so, the transmitance of light in 380nm~2500nm wave-length coverages is substantially changed this
One special nature, so as to a kind of thermochromic thin film for temperature control response type intelligent dimming glass is obtained.The thermic for preparing
Inorganic nano-particle is uniformly embedded in organic polymer disperse matrix A in optically variable films, and apparent mass is good, it is homogeneous light to present
Yellow, and translucency is good, the reaction of optics performance of control is fast.The preparation method of the reversible thermochromic film can conveniently realize big face
Product production.
Reversible thermochromic film of the invention is by the VO after ion doping2Particle diameter in 10~30nm, its phase transformation
Temperature is reduced to 45 DEG C from 68 DEG C, and reduces VO2Crystallite dimension and reduce VO2Energy gap, the nanometer of gained
VO2Powder constitution is single, even particle size distribution, with low cost；The VO2 nano-particles of doping vario-property keep dividing for more than three months
Stability is dissipated, sedimentation phenomenon does not occur.
Reversible thermochromic film of the invention uses one or more nontoxic, stable, environment-friendly organic or nothings
Machine composite compounding is formed, by the VO of doping vario-property2, undergo phase transition at a lower temperature, the environmental stability of the system
Height, reaction rate is fast；For ambient temperature conditions change belong to autonomous generation stress behavior, it is not necessary to artificial adjustment, and reaching
To the purpose of Intelligent adjustment, belong to a kind of intelligent power saving product；It is prepared by reversible thermochromic film low cost of the invention, processing
Method is simple, with more preferable environmental stability and service life, is widely used on building or vehicle glass.
Wherein in some embodiments, the inorganic nano slurry includes the component of following weight portion：
Wherein in some embodiments, the modified VO2Nanometer powder is with the percentage by weight of the grinding distribution agent B
10:1。
Wherein in some embodiments, the modified VO2The preparation of nanometer powder comprises the following steps：
By V2O5Powder is dissolved in NaOH solution, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl and H to component A2O2Solution, stirs after solution switchs to navy blue, obtains pH value
It is 1 component B；
Add NaOH solution suspended up to solution generation to component B, add a small amount of white tungstic acid, obtain component C；
Component C is fitted into reactor, under conditions of HTHP, is reacted, room temperature is cooled to after reaction, obtained
Component D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over air blast
In drying box, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
Wherein in some embodiments, the tungsten is 1 than scope with the atom number of vanadium:100~1:20.
Wherein in some embodiments, the modified VO2The particle size range of nanometer powder is 10~30nm.
Wherein in some embodiments, the weight hundred of the inorganic nano slurry and the organic polymer disperse matrix A
Divide than being 1:1.
Wherein in some embodiments, the organic polymer disperse matrix A is polyurethane or polyacrylic acid.
A kind of preparation method of reversible thermochromic film, comprises the following steps：
First step：Following component material is provided：PET film layer and anorganic thermochromic coating liquid layer；
The anorganic thermochromic coating liquid layer includes the component of following weight portion：
The inorganic nano slurry includes the component of following weight portion：
Second step：By the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B stirring mixing, then be positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano
Slurry；
Third step：By in the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then
Solvent orange 2 A and age resister A are sequentially added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid；
Four steps：Again by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer
On, after drying, obtain reversible thermochromic film.
Wherein in some embodiments, the thickness of the reversible thermochromic film is 10 μm~50 μm.
The solution of the present invention below will be further illustrated by several embodiments.
Embodiment one
Reversible thermochromic film of the invention is by PET film layer and is coated on the inorganic heat of the PET film layer surface
Mutagens color coating liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following weight portion：5
Part；Organic polymer disperse matrix A：5 parts；Solvent orange 2 A：10 parts；Age resister A：0.01 part；Inorganic nano slurry includes following weight
Measure the component of part：Modified VO2Nanometer powder：2.65 parts；Grinding distribution agent B：0.26 part；Solvent B：2.13 parts；Age resister B：
0.01 part.
First step, prepares modified VO2Nanometer powder：
By V2O5Powder is dissolved in the NaOH solution that concentration is 20%, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl that concentration is 10% and the H that concentration is 10% to component A2O2Solution, stirs and treats
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To the NaOH solution that component B additions concentration is 40% until solution generation is suspended, a small amount of white tungstic acid (tungsten is added
Atom number with vanadium is 1 than scope:100) component C, is obtained；
Component C is fitted into the reactor of 100mL, under conditions of HTHP, is reacted, room is cooled to after reaction
Temperature, obtains component D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over air blast
In drying box, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B stirring mixing, then be positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano
Slurry.
Third step, by the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then
Solvent orange 2 A and age resister A are sequentially added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid.It is described
Organic polymer disperse matrix A is polyurethane.
Four steps, then by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer
On, after drying, obtain reversible thermochromic film.
Embodiment two
Reversible thermochromic film of the invention is by PET film layer and is coated on the inorganic heat of the PET film layer surface
Mutagens color coating liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following weight portion：
30 parts；Organic polymer disperse matrix A：30 parts；Solvent orange 2 A：20 parts；Age resister A：0.05 part；Inorganic nano slurry is included such as
The component of lower weight portion：Modified VO2Nanometer powder：10 parts；Grinding distribution agent B：1 part；Solvent B：18.92 parts；Age resister B：
0.08 part.
First step, prepares modified VO2Nanometer powder：
By V2O5Powder is dissolved in the NaOH solution that concentration is 20%, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl that concentration is 10% and the H that concentration is 10% to component A2O2Solution, stirs and treats
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To the NaOH solution that component B additions concentration is 40% until solution generation is suspended, a small amount of white tungstic acid (tungsten is added
Atom number with vanadium is 1 than scope:60) component C, is obtained；
Component C is fitted into the reactor of 100mL, under conditions of HTHP, is reacted, room is cooled to after reaction
Temperature, obtains component D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over air blast
In drying box, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B stirring mixing, then be positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano
Slurry.
Third step, by the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then
Solvent orange 2 A and age resister A are sequentially added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid.It is described
Organic polymer disperse matrix A is polyurethane.
Four steps, then by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer
On, after drying, obtain reversible thermochromic film.
Embodiment three
Reversible thermochromic film of the invention is by PET film layer and is coated on the inorganic heat of the PET film layer surface
Mutagens color coating liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following weight portion：
80 parts；Organic polymer disperse matrix A：80 parts；Solvent orange 2 A：70 parts；Age resister A：0.08 part；Inorganic nano slurry is included such as
The component of lower weight portion：Modified VO2Nanometer powder：30 parts；Grinding distribution agent B：3 parts；Solvent B：46.9 parts；Age resister B：
0.1 part.
First step, prepares modified VO2Nanometer powder：
By V2O5Powder is dissolved in the NaOH solution that concentration is 20%, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl that concentration is 10% and the H that concentration is 10% to component A2O2Solution, stirs and treats
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To the NaOH solution that component B additions concentration is 40% until solution generation is suspended, a small amount of white tungstic acid (tungsten is added
Atom number with vanadium is 1 than scope:20) component C, is obtained；
Component C is fitted into the reactor of 100mL, under conditions of HTHP, is reacted, room is cooled to after reaction
Temperature, obtains component D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over air blast
In drying box, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B stirring mixing, then be positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano
Slurry.
Third step, by the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then
Solvent orange 2 A and age resister A are sequentially added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid.It is described
Organic polymer disperse matrix A is polyurethane.
Four steps, then by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer
On, after drying, obtain reversible thermochromic film.
Example IV
Reversible thermochromic film of the invention is by PET film layer and is coated on the inorganic heat of the PET film layer surface
Mutagens color coating liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following weight portion：
120 parts；Organic polymer disperse matrix A：120 parts；Solvent orange 2 A：120 parts；Age resister A：0.1 part；Inorganic nano slurry includes
The component of following weight portion：Modified VO2Nanometer powder：40 parts；Grinding distribution agent B：4 parts；Solvent B：85.9 parts；Age resister B：
0.1 part.
First step, prepares modified VO2Nanometer powder：
By V2O5Powder is dissolved in the NaOH solution that concentration is 20%, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl that concentration is 10% and the H that concentration is 10% to component A2O2Solution, stirs and treats
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To the NaOH solution that component B additions concentration is 40% until solution generation is suspended, a small amount of white tungstic acid (tungsten is added
Atom number with vanadium is 1 than scope:20) component C, is obtained；
Component C is fitted into the reactor of 100mL, under conditions of HTHP, is reacted, room is cooled to after reaction
Temperature, obtains component D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over air blast
In drying box, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B stirring mixing, then be positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano
Slurry.
Third step, by the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then
Solvent orange 2 A and age resister A are sequentially added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid.It is described
Organic polymer disperse matrix A is polyurethane.
Four steps, then by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer
On, after drying, obtain reversible thermochromic film.
Embodiment five
Reversible thermochromic film of the invention is by PET film layer and is coated on the inorganic heat of the PET film layer surface
Mutagens color coating liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following weight portion：5
Part；Organic polymer disperse matrix A：5 parts；Solvent orange 2 A：10 parts；Age resister A：0.01 part；Inorganic nano slurry includes following weight
Measure the component of part：Modified VO2Nanometer powder：2.65 parts；Grinding distribution agent B：0.26 part；Solvent B：2.13 parts；Age resister B：
0.01 part.
First step, prepares modified VO2Nanometer powder：
By V2O5Powder is dissolved in the NaOH solution that concentration is 20%, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl that concentration is 10% and the H that concentration is 10% to component A2O2Solution, stirs and treats
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To the NaOH solution that component B additions concentration is 40% until solution generation is suspended, a small amount of white tungstic acid (tungsten is added
Atom number with vanadium is 1 than scope:100) component C, is obtained；
Component C is fitted into the reactor of 100mL, under conditions of HTHP, is reacted, room is cooled to after reaction
Temperature, obtains component D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over air blast
In drying box, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B stirring mixing, then be positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano
Slurry.
Third step, by the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then
Solvent orange 2 A and age resister A are sequentially added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid.It is described
Organic polymer disperse matrix A is polyacrylic acid.
Four steps, then by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer
On, after drying, obtain reversible thermochromic film.
Embodiment six
Reversible thermochromic film of the invention is by PET film layer and is coated on the inorganic heat of the PET film layer surface
Mutagens color coating liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following weight portion：
30 parts；Organic polymer disperse matrix A：30 parts；Solvent orange 2 A：20 parts；Age resister A：0.05 part；Inorganic nano slurry is included such as
The component of lower weight portion：Modified VO2Nanometer powder：10 parts；Grinding distribution agent B：1 part；Solvent B：18.92 parts；Age resister B：
0.08 part.
First step, prepares modified VO2Nanometer powder：
By V2O5Powder is dissolved in the NaOH solution that concentration is 20%, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl that concentration is 10% and the H that concentration is 10% to component A2O2Solution, stirs and treats
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To the NaOH solution that component B additions concentration is 40% until solution generation is suspended, a small amount of white tungstic acid (tungsten is added
Atom number with vanadium is 1 than scope:60) component C, is obtained；
Component C is fitted into the reactor of 100mL, under conditions of HTHP, is reacted, room is cooled to after reaction
Temperature, obtains component D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over air blast
In drying box, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B stirring mixing, then be positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano
Slurry.
Third step, by the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then
Solvent orange 2 A and age resister A are sequentially added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid.It is described
Organic polymer disperse matrix A is polyacrylic acid.
Four steps, then by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer
On, after drying, obtain reversible thermochromic film.
Embodiment seven
Reversible thermochromic film of the invention is by PET film layer and is coated on the inorganic heat of the PET film layer surface
Mutagens color coating liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following weight portion：
80 parts；Organic polymer disperse matrix A：80 parts；Solvent orange 2 A：70 parts；Age resister A：0.08 part；Inorganic nano slurry is included such as
The component of lower weight portion：Modified VO2Nanometer powder：30 parts；Grinding distribution agent B：3 parts；Solvent B：46.9 parts；Age resister B：
0.1 part.
First step, prepares modified VO2Nanometer powder：
By V2O5Powder is dissolved in the NaOH solution that concentration is 20%, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl that concentration is 10% and the H that concentration is 10% to component A2O2Solution, stirs and treats
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To the NaOH solution that component B additions concentration is 40% until solution generation is suspended, a small amount of white tungstic acid (tungsten is added
Atom number with vanadium is 1 than scope:20) component C, is obtained；
Component C is fitted into the reactor of 100mL, under conditions of HTHP, is reacted, room is cooled to after reaction
Temperature, obtains component D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over air blast
In drying box, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B stirring mixing, then be positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano
Slurry.
Third step, by the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then
Solvent orange 2 A and age resister A are sequentially added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid.It is described
Organic polymer disperse matrix A is polyacrylic acid.
Four steps, then by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer
On, after drying, obtain reversible thermochromic film.
Embodiment eight
Reversible thermochromic film of the invention is by PET film layer and is coated on the inorganic heat of the PET film layer surface
Mutagens color coating liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following weight portion：
120 parts；Organic polymer disperse matrix A：120 parts；Solvent orange 2 A：120 parts；Age resister A：0.1 part；Inorganic nano slurry includes
The component of following weight portion：Modified VO2Nanometer powder：40 parts；Grinding distribution agent B：4 parts；Solvent B：85.9 parts；Age resister B：
0.1 part.
First step, prepares modified VO2Nanometer powder：
By V2O5Powder is dissolved in the NaOH solution that concentration is 20%, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl that concentration is 10% and the H that concentration is 10% to component A2O2Solution, stirs and treats
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To the NaOH solution that component B additions concentration is 40% until solution generation is suspended, a small amount of white tungstic acid (tungsten is added
Atom number with vanadium is 1 than scope:20) component C, is obtained；
Component C is fitted into the reactor of 100mL, under conditions of HTHP, is reacted, room is cooled to after reaction
Temperature, obtains component D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over air blast
In drying box, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B stirring mixing, then be positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano
Slurry.
Third step, by the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then
Solvent orange 2 A and age resister A are sequentially added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid.It is described
Organic polymer disperse matrix A is polyacrylic acid.
Four steps, then by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer
On, after drying, obtain reversible thermochromic film.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Shield scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of reversible thermochromic film, including PET film layer and the inorganic thermic of the PET film layer surface is coated on
Discoloration coating liquid layer, it is characterised in that the anorganic thermochromic coating liquid layer includes the component of following weight portion：
2. reversible thermochromic film according to claim 1, it is characterised in that the inorganic nano slurry includes as follows
The component of weight portion：
3. reversible thermochromic film according to claim 2, it is characterised in that the modified VO2Nanometer powder with it is described
The percentage by weight of grinding distribution agent B is 10:1.
4. reversible thermochromic film according to claim 2, it is characterised in that the modified VO2The preparation of nanometer powder
Comprise the following steps：
By V2O5Powder is dissolved in NaOH solution, after stirring becomes colorless to solution, obtains component A；
Progressively slowly add dilute HCl and H to component A2O2Solution, stirs after solution switchs to navy blue, and it is 1 to obtain pH value
Component B；
Add NaOH solution suspended up to solution generation to component B, add a small amount of white tungstic acid, obtain component C；
Component C is fitted into reactor, under conditions of HTHP, is reacted, room temperature is cooled to after reaction, obtain component
D；
Component D is separated by centrifuge, then is repeatedly washed with deionized water by absolute ethyl alcohol, be positioned over forced air drying
In case, at being 50 DEG C in temperature, drying finally grinds to form uniform fine powder in agate mortar.
5. reversible thermochromic film according to claim 4, it is characterised in that the tungsten compares model with the atom number of vanadium
Enclose is 1:100~1:20.
6. reversible thermochromic film according to claim 4, it is characterised in that the modified VO2The particle diameter of nanometer powder
Scope is 10~30nm.
7. reversible thermochromic film according to claim 1, it is characterised in that the inorganic nano slurry has with described
The percentage by weight of machine macromolecule disperse matrix A is 1:1.
8. reversible thermochromic film according to claim 1, it is characterised in that the organic polymer disperse matrix A
It is polyurethane or polyacrylic acid.
9. a kind of preparation method of reversible thermochromic film, it is characterised in that comprise the following steps：
First step：Following component material is provided：PET film layer and anorganic thermochromic coating liquid layer；
The anorganic thermochromic coating liquid layer includes the component of following weight portion：
The inorganic nano slurry includes the component of following weight portion：
Second step：By the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and age resister B are stirred
Mixing is mixed, then is positioned in sand mill, under 2500r/min rotating speeds, after speed lapping 10h, obtain the inorganic nano slurry；
Third step：By in the inorganic nano slurry addition organic polymer disperse matrix A, stirring mixes, then successively
Solvent orange 2 A and age resister A are added, by after high speed shear dispersion 2h, obtaining the anorganic thermochromic coating liquid；
Four steps：Again by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer, dried
After dry, reversible thermochromic film is obtained.
10. the preparation method of reversible thermochromic film according to claim 9, it is characterised in that the reversible thermic
The thickness of optically variable films is 10 μm~50 μm.
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