CN106987244A - A kind of composite electrochromic material and preparation method thereof - Google Patents
A kind of composite electrochromic material and preparation method thereof Download PDFInfo
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- CN106987244A CN106987244A CN201710337962.XA CN201710337962A CN106987244A CN 106987244 A CN106987244 A CN 106987244A CN 201710337962 A CN201710337962 A CN 201710337962A CN 106987244 A CN106987244 A CN 106987244A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
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Abstract
The present invention relates to a kind of composite electrochromic material and preparation method thereof, belong to functional material preparing technical field.The composite electrochromic material of the present invention is based on core shell structure, is double-layer hollow spherical structure, 30~200 μm of external diameter, 5~20 μm of wall thickness;Outer layer is Polymer Electrochromic material;Internal layer is the non-electrochromic material of the macromolecule containing inorganic electrochromic material, 2~10 μm of wall thickness;The integral coating rate of inorganic electrochromic material is 2~15%.Prepared using the method for emulsion polymerization, it is simple, efficient.The hollow-core construction of material of the present invention adds inorganic and organic electrochromic material specific surface area well, compared to the consumption that solid construction reduces electrochromic material;The non-electrochromic material of internal layer macromolecule, secures inorganic electrochromic powder, improves stability well;The aniline of electric conductivity, the use of thiophene Polymer Electrochromic material are effectively reduced resistance.
Description
Technical field
The present invention relates to a kind of composite electrochromic material and preparation method thereof, belong to functional material preparing technical field.
Background technology
Electrochromism refers in the presence of external electrical field, and materials from oxidizing or reduction reaction causes its transmission to light
Reversible change is produced with reflection, the phenomenon of the reversible change of color and transparency is then shown as in appearance.From Deb in 1969
Since (De Bu) develops the first electrochromic device using tungstic acid, based on various material systems, different structure and difference
The electrochromic device of Discoloration mechanism continuously emerges.Electrochromic material is because its substance classes is more, color change abundant, preparation side
The advantages of method is simple, has huge application potential in fields such as automobile, buildings.
Different according to the species of electrochromic material, electrochromic material can be divided into inorganic electrochromic material and Organic Electricity
Cause off-color material (species containing conducting polymer).Inorganic electrochromic material and organic electrochromic material is each advantageous and deficiency,
The molecular structure that wherein inorganic electrochromic material is consolidated in itself by inorganic material so that it has higher cyclical stability,
But processing cost is expensive;And the molecular structure of organic electrochromic material is easy to modification, color is more rich, and response speed is more
It hurry up, but cyclical stability is poor, therefore it is desirable to improve its performance by modes such as doped and compoundeds.
Chinese patent notification number CN103172274A has reported a kind of system of nickel oxide/polyaniline composite electrochromic film
Preparation Method, this method realizes the compound of inorganic-organic electrochromic material, improves optical property, the stability of material and sound
Speed etc. is answered, but polyaniline has simply been covered in nickel oxide surfaces by the method, its bar-shaped composite electrochromic material prepared
Material has the shortcomings that small surface area, electric conductivity poor (synthesis does not adjust electric conductivity), resistance are big, it is impossible to which sufficient performance is each
The advantage of material.
Therefore inorganic, organic electrochromic material is combined, preparing has Stability Analysis of Structures, high circulation, rich color
There is important Research Significance with the electrochromic material of fast response time and value is widely applied.
The content of the invention
There is problem or deficiency for above-mentioned, the invention provides a kind of composite electrochromic material and preparation method thereof,
It is prepared simply, efficiently, based on core shell structure.
The composite electrochromic material that the present invention is provided, is prepared using the method for emulsion polymerization, is double-layer hollow spherical junctions
Structure, 30~200 μm of external diameter, 5~20 μm of wall thickness;Outer layer is Polymer Electrochromic material;Internal layer is to contain inorganic electrochromic
The non-electrochromic material of macromolecule of material, 2~10 μm of wall thickness;The integral coating rate of inorganic electrochromic material is 2~15%.
Its preparation method comprises the following steps:
Step 1, the prepolymer water for configuring the non-electrochromic material of the macromolecule containing inorganic electrochromic material at room temperature
Solution;
The nothing of 0.05~0.2 times of monomer solution quality is added in the aqueous solution of the non-electrochromism material monomer of macromolecule
Machine electrochromic material, then under 300~1500rpm mixing speed, is heated to 30~60 DEG C, is kept stirring for speed and adds
Hot 1~1.5h of temperature.
Step 2, by solution made from step 1 and mass percent concentration it is that 1~5% aqueous surfactant solution presses quality
Than 1:3~1:5 mixing, add the oiliness liquid core of above-mentioned 0.05~0.2 times of mixed liquor gross mass, in 300~1200rpm
Mixing speed under react 5~10min, mixing speed drops to 300~800rpm afterwards, reacts 20~60min, subsequent rotating speed
150~300rpm is down to, and is heated to 40~60 DEG C, 40~60min of stirring.Finally, room temperature is naturally cooled to, is used
Deionized water is washed 3~5 times, filtering, obtains micro-nano capsule.
Step 3, at room temperature, micro-nano made from the aqueous solution to the step 2 for the monomer for adding Polymer Electrochromic material
Rice glue capsule, lasting stirring, until Polymer Electrochromic material is aggregated in micro-nano capsule surface, forms the macromolecule electricity of outer layer
Mutagens color material layer;Then it is washed with deionized water 3~5 times, filters, obtains the micro-nano rice glue of Polymer Electrochromic material parcel
Capsule.
Step 4, the micro-nano capsule for obtaining step 3, are put into removal oiliness liquid core in proton solvent, then filter
Micro-nano capsule is collected, operates 3~5 times, is dried afterwards in vacuum drying chamber repeatedly, you can obtain outer layer electroluminescent for macromolecule
Discoloration material layer, internal layer is the hollow-core construction compound electric of the macromolecule non-electrical mutagens color material layer containing inorganic electrochromic material
Cause off-color material.
Inorganic electrochromic material in the step 1 is the titanium dioxide, tungstic acid, oxidation of micro-nano powder shape
Nickel, many wolframic acids, molybdenum trioxide or vanadic anhydride.
Obtained prepolymer in the step 1 is urea-formaldehyde prepolymer, carbamide prepolymer, polyurethane
Prepolymer or isocyanate prepolymer.
Surfactant in the step 2 is Arabic gum, gelatin, neopelex, dodecyl sulphate
Sodium, polyvinyl-maleic anhydride copolymer, styrene-maleic anhydride copolymer or sorbitan ester fatty acid ester.
Oiliness liquid core in the step 2 is toluene, ethylbenzene, paraffin, octadecane, eicosane, benzene, 1,6- ethylidene
Diisocyanate or lipid.
Polymer Electrochromic material monomer in the step 3 is aniline, pyrroles or thiophene.
Proton solvent in the step 4 is acetone or tetrahydrofuran.
Beneficial effects of the present invention are:
1st, the double-layer hollow spherical structure for the Electrochromic composite material that the present invention is provided, regular shape, size uniform, outside
30~200 μm of footpath, 5~20 μm of wall thickness;Outer layer is Polymer Electrochromic material, and internal layer is to contain inorganic electrochromic material
The non-electrochromism material of macromolecule, the integral coating rate of inorganic electrochromic material is 2~15%.
2nd, hollow-core construction of the invention can be very good inorganic and organic electrochromic material the specific surface area of increase, hollow
Structure also reduces the consumption of electrochromic material compared with solid construction;
3rd, the non-electrochromic material of internal layer macromolecule of the invention, fixed inorganic electrochromism powder work can be played very well
With raising stability.
4th, the macromolecule electrochromic material such as aniline, thiophene for using of the present invention itself has good electric conductivity, can be with
It is effective to reduce resistance.
In summary, the hollow-core construction of material of the present invention adds inorganic and organic electrochromic material ratio table well
Area, compared to the consumption that solid construction reduces electrochromic material;The non-electrochromic material of internal layer macromolecule, it is fixed well
Inorganic electrochromic powder, improves stability;The use of the aniline, thiophene Polymer Electrochromic material of electric conductivity is effective
Reduce resistance.
Brief description of the drawings
Fig. 1 is the structural representation of material of the present invention;
Fig. 2 is micro-nano capsule prepared by the step 2 of embodiment 1;2-a is the SEM image of 1000 times of amplification;2-b is amplification
3000 times of SEM image;2-c is broken amplification by 5000 times of SEM image;2-d is that micro-nano capsule surface amplifies 5000 times
SEM image;
Fig. 3 is the composite electrochromic material that embodiment 1 is finally prepared;3-a is amplification by 3000 times of SEM image;3-b
For the SEM image of 3000 times broken of amplification;
Fig. 4 is the composite electrochromic material that embodiment 1 is finally prepared;Composite electrochromic material prepared by 4-a;4-b
By sintering the titanium dioxide remained in 800 DEG C of air;
Reference:1-1 inorganic electrochromic material particles, 1-2 macromolecule compacted zones, 1-3 Polymer Electrochromic materials
Material, 1-4 high polymer materials.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
The experimental method used in following embodiments, is conventional method unless otherwise specified;Agents useful for same, material etc.,
Unless otherwise specified, commercially obtain.
Embodiment 1.
A kind of composite electrochromic material and preparation method thereof, comprises the following steps:
Step 1:2.5g urea and 6.33g formalins are mixed, 0.25g titanium dioxide is added, uses sodium hydroxide
Its pH to 9 is adjusted, in stirring reaction 1h at 80 DEG C, white opacity liquid is obtained, as titanium dioxide-urea-formaldehyde prepolymer
Solution;
Step 2:The aqueous solution of the liquor-saturated copolymer of ethylene maleic acid of mass percent concentration 1.375% is prepared, in room temperature
Under, the solution that step 1 is obtained is added in the aqueous solution of the liquor-saturated copolymer of ethylene maleic acid, and aqueous phase is adjusted with aqueous citric acid solution
PH to 2.00, adds 10g toluene solvants, with after stirring 5min under 900rpm speed;Reduce mixing speed extremely afterwards
450rmp reacts 30min, and further reduction mixing speed continues to react 60min to 200rpm;Then raise temperature to 55 DEG C, reaction
90min, is cooled to room temperature, after products therefrom is cleaned 5 times through deionized water successively, is filtered by 500 mesh sieve, removes and do not participate in
The nano titanium oxide of reaction is tested, micro-nano capsule (Fig. 2) is obtained;
Step 3:At room temperature, the aniline and mass percent concentration that addition mass percent concentration is 3.33% are 8.33%
Camphorsulfonic acid the 30g aqueous solution into above-mentioned micro-nano capsule, and the mechanical agitation under 200rpm rotating speed.After 5min, divide 8
Secondary, per minor tick 10min, addition 8.33wt% persulfuric acid is by the 30g aqueous solution of hydrochloric acid into the above-mentioned aqueous solution.At room temperature after
Continuous stirring 12h, obtained product is cleaned 6 times through deionized water, is filtrated to get outer layer for the micro-nano capsule of polyaniline.
Step 4:Micro-nano capsule will will be obtained in step 3, and be put into removal oiliness liquid core in acetone solvent, repeat 5
It is secondary, dried afterwards in vacuum drying chamber, outer layer is obtained afterwards for polyaniline, internal layer is the Lauxite containing titanium dioxide
Hollow composite electrochromic material (Fig. 3).
Embodiment 2.
Step 1:2.5g urea and 6.33g formalins are mixed, 0.25g titanium dioxide is added, with using hydroxide
Sodium adjusts its pH to 9, in stirring reaction 1h at 80 DEG C, obtains white opacity liquid, as titanium dioxide-urea-formaldehyde pre-polymerization
The solution of thing;
Step 2:The aqueous solution of the mass percent concentration for the 1.375% liquor-saturated copolymer of ethylene maleic acid is prepared, in room temperature
Under, step 1 is obtained into solution and is added in the aqueous solution of the liquor-saturated copolymer of ethylene maleic acid, aqueous phase is adjusted with aqueous citric acid solution
PH to 2.50, adds 10g toluene solvants, with after stirring 5min under 900rpm speed;Reduce mixing speed extremely afterwards
450rmp reacts 30min, and further reduction mixing speed continues to react 60min to 200rpm;Then raise temperature to 55 DEG C, reaction
90min, is cooled to room temperature, after products therefrom is cleaned 5 times through deionized water successively, is filtered by 500 mesh sieve, removes and do not participate in
The nano titanium oxide of reaction is tested, micro-nano capsule is filtrated to get;
Step 3:Addition 35.56g mass percent concentration is 15.64% iron chloride (III) aqueous hydrochloric acid solution at room temperature
Aqueous hydrochloric acid solution with 30g0.1mol/l is into above-mentioned micro-nano capsule, and the mechanical agitation under 200rpm rotating speed.10min
Afterwards, it is 3.23% pyrroles's aqueous solution to divide the mass percent concentration that 8 times are 31g per minor tick 10min total amount of adding.At room temperature
Continue to stir after 4.5h, obtained product is cleaned 6 times through deionized water, is then filtered, obtain outer layer for polypyrrole micro-nano rice glue
Capsule.
Step 4:Removal oiliness liquid core in acetone solvent by obtained micro-nano capsule, will be put into step 3, is repeated
5 times, dried afterwards in vacuum drying chamber, outer layer is obtained afterwards for polypyrrole, internal layer is the Lauxite containing titanium dioxide
Hollow composite electrochromic material.
Claims (8)
1. a kind of composite electrochromic material, it is characterised in that:Structure is that double-layer hollow is spherical, 30~200 μm of external diameter, wall thickness 5
~20 μm;Outer layer is Polymer Electrochromic material;Internal layer is the non-electrochromism of the macromolecule containing inorganic electrochromic material
Material, 2~10 μm of wall thickness;The integral coating rate of inorganic electrochromic material is 2~15%.
2. the preparation method of composite electrochromic material as claimed in claim 1, comprises the following steps:
Step 1, the prepolymer aqueous solution for configuring the non-electrochromic material of the macromolecule containing inorganic electrochromic material at room temperature;
Added in the aqueous solution of the non-electrochromism material monomer of macromolecule 0.05~0.2 times of monomer solution quality without electromechanics
Off-color material is caused, then under 300~1500rpm mixing speed, 30~60 DEG C are heated to, speed and heating temperature is kept stirring for
Spend 1~1.5h;
Step 2, by solution made from step 1 and mass percent concentration it is 1~5% aqueous surfactant solution in mass ratio 1:
3~1:5 mixing, add the oiliness liquid core of above-mentioned 0.05~0.2 times of mixed liquor gross mass, in stirring for 300~1200rpm
5~10min of reaction under speed is mixed, mixing speed drops to 300~800rpm afterwards, reacts 20~60min, and subsequent rotating speed is down to
150~300rpm, and it is heated to 40~60 DEG C, 40~60min of stirring.Finally, naturally cooled to room temperature, spend from
Sub- water washing 3~5 times, filtering, obtains micro-nano capsule;
Step 3, at room temperature, micro-nano rice glue made from the aqueous solution to the step 2 for the monomer for adding Polymer Electrochromic material
Capsule, lasting stirring, until Polymer Electrochromic material is aggregated in micro-nano capsule surface, forms the electroluminescent change of macromolecule of outer layer
Color material layer;Then it is washed with deionized water 3~5 times, filters, obtains the micro-nano capsule of Polymer Electrochromic material parcel;
Step 4, the micro-nano capsule for obtaining step 3, are put into removal oiliness liquid core in proton solvent, are then collected by filtration
Micro-nano capsule, operates 3~5 times, is dried afterwards in vacuum drying chamber repeatedly, you can obtain outer layer for Polymer Electrochromic
Material layer, internal layer is the hollow-core construction compound electric mutagens of the macromolecule non-electrical mutagens color material layer containing inorganic electrochromic material
Color material.
3. the preparation method of composite electrochromic material as claimed in claim 2, it is characterised in that:
Inorganic electrochromic material is titanium dioxide, tungstic acid, nickel oxide, many tungsten of micro-nano powder shape in the step 1
Acid, molybdenum trioxide or vanadic anhydride.
4. the preparation method of composite electrochromic material as claimed in claim 2, it is characterised in that:
Prepolymer made from the step 1 be urea-formaldehyde prepolymer, carbamide prepolymer, polyurethane prepolymer or
Isocyanate prepolymer.
5. the preparation method of composite electrochromic material as claimed in claim 2, it is characterised in that:
Surfactant is Arabic gum, gelatin, neopelex, lauryl sodium sulfate, poly- second in the step 2
Alkene-copolymer-maleic anhydride, styrene-maleic anhydride copolymer or sorbitan ester fatty acid ester.
6. the preparation method of composite electrochromic material as claimed in claim 2, it is characterised in that:
The medium oil liquid core of step 2 is toluene, ethylbenzene, paraffin, octadecane, eicosane, benzene, 1,6- ethylene isocyanides
Acid esters or lipid.
7. the preparation method of composite electrochromic material as claimed in claim 2, it is characterised in that:Macromolecule in the step 3
Electrochromic material monomer is aniline, pyrroles or thiophene.
8. the preparation method of composite electrochromic material as claimed in claim 2, it is characterised in that:Proton is molten in the step 4
Agent is acetone or tetrahydrofuran.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111040423A (en) * | 2019-12-11 | 2020-04-21 | 东莞市雄林新材料科技股份有限公司 | Electroluminescence color-changing TPU film and preparation method thereof |
CN111908509A (en) * | 2020-08-05 | 2020-11-10 | 合肥工业大学 | Tungsten trioxide/polythiophene/tungsten trioxide electrochromic capacitor dual-function material and preparation method thereof |
CN112662389A (en) * | 2021-01-08 | 2021-04-16 | 深圳市华科创智技术有限公司 | Electrochromic material and preparation method thereof |
CN113979646A (en) * | 2021-11-25 | 2022-01-28 | 山东大学 | Multicolor electrochromic composite film and preparation method and application thereof |
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CN106220830A (en) * | 2016-07-12 | 2016-12-14 | 电子科技大学 | A kind of selfreparing electrochromic material and preparation method thereof |
CN106519105A (en) * | 2016-11-18 | 2017-03-22 | 陕西盛迈石油有限公司 | Method for preparing photochromic microspheres through self-emulsifying method |
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CN102071009A (en) * | 2011-01-21 | 2011-05-25 | 电子科技大学 | Preparation method of organic-inorganic composite electrochromic material |
CN106220830A (en) * | 2016-07-12 | 2016-12-14 | 电子科技大学 | A kind of selfreparing electrochromic material and preparation method thereof |
CN106519105A (en) * | 2016-11-18 | 2017-03-22 | 陕西盛迈石油有限公司 | Method for preparing photochromic microspheres through self-emulsifying method |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111040423A (en) * | 2019-12-11 | 2020-04-21 | 东莞市雄林新材料科技股份有限公司 | Electroluminescence color-changing TPU film and preparation method thereof |
CN111908509A (en) * | 2020-08-05 | 2020-11-10 | 合肥工业大学 | Tungsten trioxide/polythiophene/tungsten trioxide electrochromic capacitor dual-function material and preparation method thereof |
CN111908509B (en) * | 2020-08-05 | 2022-06-10 | 合肥工业大学 | Tungsten trioxide/polythiophene/tungsten trioxide electrochromic capacitor dual-function material and preparation method thereof |
CN112662389A (en) * | 2021-01-08 | 2021-04-16 | 深圳市华科创智技术有限公司 | Electrochromic material and preparation method thereof |
CN113979646A (en) * | 2021-11-25 | 2022-01-28 | 山东大学 | Multicolor electrochromic composite film and preparation method and application thereof |
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