CN106750466B - Reversible thermochromic film and preparation method thereof - Google Patents
Reversible thermochromic film and preparation method thereof Download PDFInfo
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- CN106750466B CN106750466B CN201710025395.4A CN201710025395A CN106750466B CN 106750466 B CN106750466 B CN 106750466B CN 201710025395 A CN201710025395 A CN 201710025395A CN 106750466 B CN106750466 B CN 106750466B
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Abstract
The present invention relates to a kind of reversible thermochromic films 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 parts by weight: 5~130 parts of inorganic nano slurry, organic polymer disperse matrix A5~130 part, 10~120 parts of solvent 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 are stirred, and are placed in the grinding of sand mill high speed, are obtained inorganic nano slurry；It adds in organic polymer disperse matrix A, is stirred, sequentially add solvent A and age resister A, obtain anorganic thermochromic coating liquid, be coated on PET film layer.Reversible thermochromic film of the invention is at low cost, and preparation for processing is simple, has better environmental stability and service life.
Description
Technical field
The present invention relates to intelligent dimming composite film material fields, and in particular to a kind of for the reversible of intelligent dimming glass
Thermochromic thin film and preparation method thereof.
Background technique
Intelligent glass is a kind of transmission that can adjust sunlight under environmental stimuli or artificial control condition, reflect or
The functional glass of absorption spectrum, the intelligent glass are generally divided into two kinds of preparation methods: first is that inductive material is made membranaceous compound
To unorganic glass surface or it is mixed among two layers of simple glass；Second is that being modified using inductive material to glass itself.
In view of the modified intelligent glass complex process obtained of glass itself, at high cost, application example is few, the research and development of intelligent glass at present with
Preparation is most in the majority with first method.
Intelligent glass inductive material mainly includes thermochromism, electrochromism and gas-discoloration three types, is passed through respectively
Environment temperature, extra electric field and sensitive gas stimulation are to change spectral property.Reversible Thermochromic Materials for 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 preferable hybrid process.
Thermochromism glass is plated one layer of 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 hot spot of people's research.VO2Film have compared with
High low temperature transmitance and very low high temperature transmitance.It, can be VO by the methods of doping2The 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 room temperature reaches
Effect cool in summer and warm in winter, side group reduce air conditioner load, energy saving.
VO2Performance with intelligent thermoregulating, but to realize and be applied in building or vehicle glass, it is necessary to solve following two
Problem: first is that VO2Phase transition temperature be 68 DEG C, it is necessary to by adulterating or changing preparation method etc., by VO2Phase transition temperature drop
Down near room temperature.Ion doping can change band gap, crystal internal stress, microstructure, vanadium ion valence state and crystal and lack
Fall into etc. because usually influencing VO2Thermochromic properties, i.e., change thermochromic temperature.Currently, for metal ion mixing, non-
Metal ion mixing and binary doped all existing researches achievement.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；Second is that the transmission of adjustment visible light
Than.It is above-mentioned research shows that VO2No matter rear visible light transmittance is all lower before phase change for film, 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.
Summary of the invention
Based on this, the present invention provide it is a kind of it is nontoxic, stability is high, environment amenable reversible thermochromic film, can
Regulate and control spectral property according to the change of temperature, is used to prepare intelligent dimming glass.
The present invention also provides the preparation methods of above-mentioned reversible thermochromic film.
In order to achieve the object of the present invention, the invention adopts the following technical scheme:
A kind of reversible thermochromic film, the inorganic heat including PET film layer and coated on the PET film layer surface
Mutagens color coats liquid layer, and the anorganic thermochromic coating liquid layer includes the component of following parts by weight:
Reversible thermochromic film of the invention, is prepared for ion doping VO first2Then nanometer powder passes through grinding point
Scattered technique is prepared into nano pulp, and compounding with the macromolecule disperse matrix A of function admirable, which becomes anorganic thermochromic, applies
Covering liquid is finally coated on the polyphenylene ethyl dioctyl phthalate second diester surface (PET) and forms transparent polymer reversible thermochromic film, most
The glass of reversible thermochromic film is posted afterwards, which is existing commodity unorganic glass or organic glass etc., 0~
The light-bleed effect for changing each wavelength in sunlight between 70 DEG C, plays the effect of intelligent dimming.The reversible thermochromic is thin
Film is based on ep-type material, and service life, by inorganic nano-particle and macromolecule compound system, passed through ion at 5 years or more
The VO of doping vario-property2It is undergone phase transition at 45 DEG C or so, the transmitance of light in 380nm~2500nm wave-length coverage is made to substantially change this
One special nature, so that a kind of thermochromic thin film for temperature control response type intelligent dimming glass be made.What is prepared is thermotropic
Inorganic nano-particle is uniformly embedded in organic polymer disperse matrix A in optically variable films, and apparent mass is good, it is uniform 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, which can facilitate, realizes big face
Product production.
Reversible thermochromic film of the invention passes through the VO after ion doping2Partial size in 10~30nm, phase transformation
Temperature is reduced to 45 DEG C from 68 DEG C, and reduces VO2Crystallite dimension and reduce VO2Forbidden bandwidth, resulting nanometer
VO2Powder constitution is single, even particle size distribution, low in cost；The holding of VO2 nanoparticle three months or more points of doping vario-property
Stability is dissipated, sedimentation phenomenon does not occur.
Reversible thermochromic film of the invention is using one or more kinds of nontoxic, stable, environmental-friendly organic or nothings
Machine composite material compounds, and passes through the VO of doping vario-property2, undergo phase transition at a lower temperature, the environmental stability of the system
Height, reaction rate are fast；Ambient temperature conditions variation is belonged to independently generate stress behavior, do not need artificial adjustment, and reach
To the purpose intelligently adjusted, belong to a kind of intelligent power saving product；Reversible thermochromic film of the invention is at low cost, processing preparation
Method is simple, has better environmental stability and service life, is widely used on building or vehicle glass.
In wherein some embodiments, the inorganic nano slurry includes the component of following parts by weight:
In wherein some embodiments, the modified VO2The weight percent of nanometer powder and the grinding distribution agent B is
10:1。
In wherein some embodiments, the modified VO2The preparation of nanometer powder includes the following steps:
By V2O5Powder is dissolved in NaOH solution and obtains component A after stirring becomes colorless to solution；
Dilute HCl and H slowly gradually is added to component A2O2Solution stirs evenly after solution switchs to navy blue, obtains pH value
For 1 component B；
To component B addition NaOH solution until solution generation is suspended, a small amount of white tungstic acid is added, component C is obtained；
Component C is fitted into reaction kettle, under conditions of high temperature and pressure, is reacted, is cooled to room temperature after reaction, obtained
Component D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in air blast
In drying box, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
In wherein some embodiments, the atom number of the tungsten and vanadium is 1:100~1:20 than range.
In wherein some embodiments, the modified VO2The particle size range of nanometer powder is 10~30nm.
In wherein some embodiments, the weight hundred of the inorganic nano slurry and the organic polymer disperse matrix A
Divide than being 1:1.
In wherein some embodiments, the organic polymer disperse matrix A is polyurethane or polyacrylic acid.
A kind of preparation method of reversible thermochromic film, includes the following steps:
First step: following component material: PET film layer and anorganic thermochromic coating liquid layer is provided；
The anorganic thermochromic coating liquid layer includes the component of following parts by weight:
The inorganic nano slurry includes the component of following parts by weight:
Second step: by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B is stirred, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano
Slurry；
Third step: the inorganic nano slurry being added in the organic polymer disperse matrix A, is stirred, then
Solvent A and age resister A are sequentially added, after high speed shear disperses 2h, obtains 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.
In wherein some embodiments, the reversible thermochromic film with a thickness of 10 μm~50 μm.
Specific embodiment
It to facilitate the understanding of the present invention, below will be to invention is more fully described.But the present invention can be to be permitted
Mostly different form is realized, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is makes
It is more thorough and comprehensive to the understanding of the disclosure.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention 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, the inorganic heat including PET film layer and coated on the PET film layer surface
Mutagens color coats liquid layer, and the anorganic thermochromic coating liquid layer includes the component of following parts by weight:
Reversible thermochromic film of the invention, is prepared for ion doping VO first2Then nanometer powder passes through grinding point
Scattered technique is prepared into nano pulp, and compounding with the macromolecule disperse matrix A of function admirable, which becomes anorganic thermochromic, applies
Covering liquid is finally coated on the polyphenylene ethyl dioctyl phthalate second diester surface (PET) and forms transparent polymer reversible thermochromic film, most
The glass of reversible thermochromic film is posted afterwards, which is existing commodity unorganic glass or organic glass etc., 0~
The light-bleed effect for changing each wavelength in sunlight between 70 DEG C, plays the effect of intelligent dimming.The reversible thermochromic is thin
Film is based on ep-type material, and service life, by inorganic nano-particle and macromolecule compound system, passed through ion at 5 years or more
The VO of doping vario-property2It is undergone phase transition at 45 DEG C or so, the transmitance of light in 380nm~2500nm wave-length coverage is made to substantially change this
One special nature, so that a kind of thermochromic thin film for temperature control response type intelligent dimming glass be made.What is prepared is thermotropic
Inorganic nano-particle is uniformly embedded in organic polymer disperse matrix A in optically variable films, and apparent mass is good, it is uniform 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, which can facilitate, realizes big face
Product production.
Reversible thermochromic film of the invention passes through the VO after ion doping2Partial size in 10~30nm, phase transformation
Temperature is reduced to 45 DEG C from 68 DEG C, and reduces VO2Crystallite dimension and reduce VO2Forbidden bandwidth, resulting nanometer
VO2Powder constitution is single, even particle size distribution, low in cost；The holding of VO2 nanoparticle three months or more points of doping vario-property
Stability is dissipated, sedimentation phenomenon does not occur.
Reversible thermochromic film of the invention is using one or more kinds of nontoxic, stable, environmental-friendly organic or nothings
Machine composite material compounds, and passes through the VO of doping vario-property2, undergo phase transition at a lower temperature, the environmental stability of the system
Height, reaction rate are fast；Ambient temperature conditions variation is belonged to independently generate stress behavior, do not need artificial adjustment, and reach
To the purpose intelligently adjusted, belong to a kind of intelligent power saving product；Reversible thermochromic film of the invention is at low cost, processing preparation
Method is simple, has better environmental stability and service life, is widely used on building or vehicle glass.
In wherein some embodiments, the inorganic nano slurry includes the component of following parts by weight:
In wherein some embodiments, the modified VO2The weight percent of nanometer powder and the grinding distribution agent B is
10:1。
In wherein some embodiments, the modified VO2The preparation of nanometer powder includes the following steps:
By V2O5Powder is dissolved in NaOH solution and obtains component A after stirring becomes colorless to solution；
Dilute HCl and H slowly gradually is added to component A2O2Solution stirs evenly after solution switchs to navy blue, obtains pH value
For 1 component B；
To component B addition NaOH solution until solution generation is suspended, a small amount of white tungstic acid is added, component C is obtained；
Component C is fitted into reaction kettle, under conditions of high temperature and pressure, is reacted, is cooled to room temperature after reaction, obtained
Component D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in air blast
In drying box, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
In wherein some embodiments, the atom number of the tungsten and vanadium is 1:100~1:20 than range.
In wherein some embodiments, the modified VO2The particle size range of nanometer powder is 10~30nm.
In wherein some embodiments, the weight hundred of the inorganic nano slurry and the organic polymer disperse matrix A
Divide than being 1:1.
In wherein some embodiments, the organic polymer disperse matrix A is polyurethane or polyacrylic acid.
A kind of preparation method of reversible thermochromic film, includes the following steps:
First step: following component material: PET film layer and anorganic thermochromic coating liquid layer is provided；
The anorganic thermochromic coating liquid layer includes the component of following parts by weight:
The inorganic nano slurry includes the component of following parts by weight:
Second step: by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B is stirred, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano
Slurry；
Third step: the inorganic nano slurry being added in the organic polymer disperse matrix A, is stirred, then
Solvent A and age resister A are sequentially added, after high speed shear disperses 2h, obtains 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.
In wherein some embodiments, the reversible thermochromic film with a thickness of 10 μm~50 μm.
Hereinafter the solution of the present invention will be further illustrated by several embodiments.
Embodiment one
The inorganic heat of reversible thermochromic film of the invention by PET film layer and coated on the PET film layer surface
Mutagens color coats liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following parts by weight: 5
Part；A:5 parts of organic polymer disperse matrix；Solvent A: 10 parts；A:0.01 parts of age resister；Inorganic nano slurry includes following weight
Measure the component of part: modified VO2Nanometer powder: 2.65 parts；B:0.26 parts of grinding distribution agent；B:2.13 parts of solvent；Age resister B:
0.01 part.
First step prepares modified VO2Nanometer powder:
By V2O5Powder is dissolved in the NaOH solution that concentration is 20% and obtains component A after stirring becomes colorless to solution；
Dilute HCl that concentration is 10% and the H that concentration is 10% slowly gradually is added to component A2O2Solution, stir evenly to
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To component B be added concentration be 40% NaOH solution until solution generate it is suspended, add a small amount of white tungstic acid (tungsten
Than range it is 1:100 with the atom number of vanadium), obtain component C；
Component C is fitted into the reaction kettle of 100mL, under conditions of high temperature and pressure, is reacted, room is cooled to after reaction
Temperature obtains component D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in air blast
In drying box, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B is stirred, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano
Slurry.
The inorganic nano slurry is added in the organic polymer disperse matrix A, is stirred by third step, then
Solvent A and age resister A are sequentially added, after high speed shear disperses 2h, obtains 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
The inorganic heat of reversible thermochromic film of the invention by PET film layer and coated on the PET film layer surface
Mutagens color coats liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following parts by weight:
30 parts；A:30 parts of organic polymer disperse matrix；Solvent A: 20 parts；A:0.05 parts of age resister；Inorganic nano slurry includes such as
The component of lower parts by weight: modified VO2Nanometer powder: 10 parts；B:1 parts of grinding distribution agent；B:18.92 parts of solvent；Age resister B:
0.08 part.
First step prepares modified VO2Nanometer powder:
By V2O5Powder is dissolved in the NaOH solution that concentration is 20% and obtains component A after stirring becomes colorless to solution；
Dilute HCl that concentration is 10% and the H that concentration is 10% slowly gradually is added to component A2O2Solution, stir evenly to
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To component B be added concentration be 40% NaOH solution until solution generate it is suspended, add a small amount of white tungstic acid (tungsten
Than range it is 1:60 with the atom number of vanadium), obtain component C；
Component C is fitted into the reaction kettle of 100mL, under conditions of high temperature and pressure, is reacted, room is cooled to after reaction
Temperature obtains component D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in air blast
In drying box, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B is stirred, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano
Slurry.
The inorganic nano slurry is added in the organic polymer disperse matrix A, is stirred by third step, then
Solvent A and age resister A are sequentially added, after high speed shear disperses 2h, obtains 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
The inorganic heat of reversible thermochromic film of the invention by PET film layer and coated on the PET film layer surface
Mutagens color coats liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following parts by weight:
80 parts；A:80 parts of organic polymer disperse matrix；Solvent A: 70 parts；A:0.08 parts of age resister；Inorganic nano slurry includes such as
The component of lower parts by weight: modified VO2Nanometer powder: 30 parts；B:3 parts of grinding distribution agent；B:46.9 parts of solvent；Age resister B:
0.1 part.
First step prepares modified VO2Nanometer powder:
By V2O5Powder is dissolved in the NaOH solution that concentration is 20% and obtains component A after stirring becomes colorless to solution；
Dilute HCl that concentration is 10% and the H that concentration is 10% slowly gradually is added to component A2O2Solution, stir evenly to
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To component B be added concentration be 40% NaOH solution until solution generate it is suspended, add a small amount of white tungstic acid (tungsten
Than range it is 1:20 with the atom number of vanadium), obtain component C；
Component C is fitted into the reaction kettle of 100mL, under conditions of high temperature and pressure, is reacted, room is cooled to after reaction
Temperature obtains component D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in air blast
In drying box, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B is stirred, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano
Slurry.
The inorganic nano slurry is added in the organic polymer disperse matrix A, is stirred by third step, then
Solvent A and age resister A are sequentially added, after high speed shear disperses 2h, obtains 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
The inorganic heat of reversible thermochromic film of the invention by PET film layer and coated on the PET film layer surface
Mutagens color coats liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following parts by weight:
120 parts；A:120 parts of organic polymer disperse matrix；Solvent A: 120 parts；A:0.1 parts of age resister；Inorganic nano slurry includes
The component of following parts by weight: modified VO2Nanometer powder: 40 parts；B:4 parts of grinding distribution agent；B:85.9 parts of solvent；Age resister B:
0.1 part.
First step prepares modified VO2Nanometer powder:
By V2O5Powder is dissolved in the NaOH solution that concentration is 20% and obtains component A after stirring becomes colorless to solution；
Dilute HCl that concentration is 10% and the H that concentration is 10% slowly gradually is added to component A2O2Solution, stir evenly to
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To component B be added concentration be 40% NaOH solution until solution generate it is suspended, add a small amount of white tungstic acid (tungsten
Than range it is 1:20 with the atom number of vanadium), obtain component C；
Component C is fitted into the reaction kettle of 100mL, under conditions of high temperature and pressure, is reacted, room is cooled to after reaction
Temperature obtains component D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in air blast
In drying box, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B is stirred, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano
Slurry.
The inorganic nano slurry is added in the organic polymer disperse matrix A, is stirred by third step, then
Solvent A and age resister A are sequentially added, after high speed shear disperses 2h, obtains 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
The inorganic heat of reversible thermochromic film of the invention by PET film layer and coated on the PET film layer surface
Mutagens color coats liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following parts by weight: 5
Part；A:5 parts of organic polymer disperse matrix；Solvent A: 10 parts；A:0.01 parts of age resister；Inorganic nano slurry includes following weight
Measure the component of part: modified VO2Nanometer powder: 2.65 parts；B:0.26 parts of grinding distribution agent；B:2.13 parts of solvent；Age resister B:
0.01 part.
First step prepares modified VO2Nanometer powder:
By V2O5Powder is dissolved in the NaOH solution that concentration is 20% and obtains component A after stirring becomes colorless to solution；
Dilute HCl that concentration is 10% and the H that concentration is 10% slowly gradually is added to component A2O2Solution, stir evenly to
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To component B be added concentration be 40% NaOH solution until solution generate it is suspended, add a small amount of white tungstic acid (tungsten
Than range it is 1:100 with the atom number of vanadium), obtain component C；
Component C is fitted into the reaction kettle of 100mL, under conditions of high temperature and pressure, is reacted, room is cooled to after reaction
Temperature obtains component D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in air blast
In drying box, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B is stirred, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano
Slurry.
The inorganic nano slurry is added in the organic polymer disperse matrix A, is stirred by third step, then
Solvent A and age resister A are sequentially added, after high speed shear disperses 2h, obtains 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
The inorganic heat of reversible thermochromic film of the invention by PET film layer and coated on the PET film layer surface
Mutagens color coats liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following parts by weight:
30 parts；A:30 parts of organic polymer disperse matrix；Solvent A: 20 parts；A:0.05 parts of age resister；Inorganic nano slurry includes such as
The component of lower parts by weight: modified VO2Nanometer powder: 10 parts；B:1 parts of grinding distribution agent；B:18.92 parts of solvent；Age resister B:
0.08 part.
First step prepares modified VO2Nanometer powder:
By V2O5Powder is dissolved in the NaOH solution that concentration is 20% and obtains component A after stirring becomes colorless to solution；
Dilute HCl that concentration is 10% and the H that concentration is 10% slowly gradually is added to component A2O2Solution, stir evenly to
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To component B be added concentration be 40% NaOH solution until solution generate it is suspended, add a small amount of white tungstic acid (tungsten
Than range it is 1:60 with the atom number of vanadium), obtain component C；
Component C is fitted into the reaction kettle of 100mL, under conditions of high temperature and pressure, is reacted, room is cooled to after reaction
Temperature obtains component D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in air blast
In drying box, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B is stirred, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano
Slurry.
The inorganic nano slurry is added in the organic polymer disperse matrix A, is stirred by third step, then
Solvent A and age resister A are sequentially added, after high speed shear disperses 2h, obtains 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
The inorganic heat of reversible thermochromic film of the invention by PET film layer and coated on the PET film layer surface
Mutagens color coats liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following parts by weight:
80 parts；A:80 parts of organic polymer disperse matrix；Solvent A: 70 parts；A:0.08 parts of age resister；Inorganic nano slurry includes such as
The component of lower parts by weight: modified VO2Nanometer powder: 30 parts；B:3 parts of grinding distribution agent；B:46.9 parts of solvent；Age resister B:
0.1 part.
First step prepares modified VO2Nanometer powder:
By V2O5Powder is dissolved in the NaOH solution that concentration is 20% and obtains component A after stirring becomes colorless to solution；
Dilute HCl that concentration is 10% and the H that concentration is 10% slowly gradually is added to component A2O2Solution, stir evenly to
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To component B be added concentration be 40% NaOH solution until solution generate it is suspended, add a small amount of white tungstic acid (tungsten
Than range it is 1:20 with the atom number of vanadium), obtain component C；
Component C is fitted into the reaction kettle of 100mL, under conditions of high temperature and pressure, is reacted, room is cooled to after reaction
Temperature obtains component D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in air blast
In drying box, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B is stirred, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano
Slurry.
The inorganic nano slurry is added in the organic polymer disperse matrix A, is stirred by third step, then
Solvent A and age resister A are sequentially added, after high speed shear disperses 2h, obtains 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
The inorganic heat of reversible thermochromic film of the invention by PET film layer and coated on the PET film layer surface
Mutagens color coats liquid layer composition；The anorganic thermochromic coating liquid layer includes the component inorganic nano slurry of following parts by weight:
120 parts；A:120 parts of organic polymer disperse matrix；Solvent A: 120 parts；A:0.1 parts of age resister；Inorganic nano slurry includes
The component of following parts by weight: modified VO2Nanometer powder: 40 parts；B:4 parts of grinding distribution agent；B:85.9 parts of solvent；Age resister B:
0.1 part.
First step prepares modified VO2Nanometer powder:
By V2O5Powder is dissolved in the NaOH solution that concentration is 20% and obtains component A after stirring becomes colorless to solution；
Dilute HCl that concentration is 10% and the H that concentration is 10% slowly gradually is added to component A2O2Solution, stir evenly to
After solution switchs to navy blue, the component B that pH value is 1 is obtained；
To component B be added concentration be 40% NaOH solution until solution generate it is suspended, add a small amount of white tungstic acid (tungsten
Than range it is 1:20 with the atom number of vanadium), obtain component C；
Component C is fitted into the reaction kettle of 100mL, under conditions of high temperature and pressure, is reacted, room is cooled to after reaction
Temperature obtains component D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in air blast
In drying box, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
Second step, by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and described anti-aging
Agent B is stirred, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano
Slurry.
The inorganic nano slurry is added in the organic polymer disperse matrix A, is stirred by third step, then
Solvent A and age resister A are sequentially added, after high speed shear disperses 2h, obtains 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.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those 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
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (8)
1. a kind of reversible thermochromic film, including PET film layer and coated on the inorganic thermotropic of the PET film layer surface
Discoloration coating liquid layer, which is characterized in that the anorganic thermochromic coating liquid layer includes the component of following parts by weight:
The inorganic nano slurry includes the component of following parts by weight:
The modified VO2The preparation of nanometer powder includes the following steps:
By V2O5Powder is dissolved in NaOH solution and obtains component A after stirring becomes colorless to solution；
Dilute HCl and H slowly gradually is added to component A2O2Solution stirs evenly after solution switchs to navy blue, and obtaining pH value is 1
Component B；
To component B addition NaOH solution until solution generation is suspended, a small amount of white tungstic acid is added, component C is obtained；
Component C is fitted into reaction kettle, under conditions of high temperature and pressure, is reacted, is cooled to room temperature after reaction, obtain component
D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in forced air drying
In case, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar.
2. reversible thermochromic film according to claim 1, which is characterized in that the modified VO2Nanometer powder with it is described
The weight percent of grinding distribution agent B is 10:1.
3. reversible thermochromic film according to claim 1, which is characterized in that the atom number of the tungsten and vanadium compares model
It encloses for 1:100~1:20.
4. reversible thermochromic film according to claim 1, which is characterized in that the modified VO2The partial size of nanometer powder
Range is 10~30nm.
5. reversible thermochromic film according to claim 1, which is characterized in that the inorganic nano slurry has with described
The weight percent of machine macromolecule disperse matrix A is 1:1.
6. reversible thermochromic film according to claim 1, which is characterized in that the organic polymer disperse matrix A
For polyurethane or polyacrylic acid.
7. a kind of preparation method of reversible thermochromic film, which comprises the steps of:
First step: following component material: PET film layer and anorganic thermochromic coating liquid layer is provided；
The anorganic thermochromic coating liquid layer includes the component of following parts by weight:
The inorganic nano slurry includes the component of following parts by weight:
The modified VO2The preparation of nanometer powder includes the following steps:
By V2O5Powder is dissolved in NaOH solution and obtains component A after stirring becomes colorless to solution；
Dilute HCl and H slowly gradually is added to component A2O2Solution stirs evenly after solution switchs to navy blue, and obtaining pH value is 1
Component B；
To component B addition NaOH solution until solution generation is suspended, a small amount of white tungstic acid is added, component C is obtained；
Component C is fitted into reaction kettle, under conditions of high temperature and pressure, is reacted, is cooled to room temperature after reaction, obtain component
D；
Component D is centrifugated by centrifuge, is repeatedly washed using dehydrated alcohol with deionized water, is placed in forced air drying
In case, in the case where temperature is 50 DEG C, drying is finally ground into uniform fine powder in the agate mortar；
Second step: by the modified VO2Nanometer powder, the grinding distribution agent B, the solvent B and the age resister B are stirred
Mixing is mixed, then is placed in sand mill, under 2500r/min revolving speed, after high speed grinding 10h, obtains the inorganic nano slurry；
Third step: the inorganic nano slurry is added in the organic polymer disperse matrix A, is stirred, then successively
Solvent A and age resister A is added, after high speed shear disperses 2h, obtains the anorganic thermochromic coating liquid；
Four steps: again by coating process, the anorganic thermochromic coating liquid is coated on the PET film layer, is dried
After dry, reversible thermochromic film is obtained.
8. the preparation method of reversible thermochromic film according to claim 7, which is characterized in that the reversible thermotropic change
Color film with a thickness of 10 μm~50 μm.
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| JP2021519831A (en) * | 2018-03-02 | 2021-08-12 | シャンハイ チュアンシー インダストリー グループ カンパニー リミテッドＳｈａｎｇｈａｉ Ｃｈｕａｎｇｓｈｉ Ｉｎｄｕｓｔｒｙ Ｇｒｏｕｐ Ｃｏ．， Ｌｔｄ． | Polymers, thermochromic agents, and / or hydrogel compositions and equipment, products that implement them, and methods and processes for their manufacture. |
| CN109537362B (en) * | 2018-11-16 | 2021-04-23 | 河南省科学院能源研究所有限公司 | Reversible thermochromic cellulose nano film and preparation method thereof |
| CN111057263A (en) * | 2019-12-31 | 2020-04-24 | 北京理工大学重庆创新中心 | Vanadium dioxide composite flexible film with organic layer protection function and preparation and application thereof |
| CN113861473A (en) * | 2021-07-21 | 2021-12-31 | 江苏双星彩塑新材料股份有限公司 | Thermochromic polyester release film and preparation method thereof |
| CN114672094A (en) * | 2022-04-02 | 2022-06-28 | 兰州大学 | Modified nanometer VO of intelligence window2High polymer composite membrane and preparation method thereof |
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| CN101265374A (en) * | 2008-01-24 | 2008-09-17 | 复旦大学 | Intelligent heat-insulating film and its preparing process |
| CN101863511A (en) * | 2010-07-05 | 2010-10-20 | 中国科学技术大学 | Method for preparing monoclinic phase vanadium dioxide and doped nano powder thereof |
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