CN106220898A - A kind of electrochromism nano-cellulose composite and preparation method thereof - Google Patents
A kind of electrochromism nano-cellulose composite and preparation method thereof Download PDFInfo
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- C08L1/02—Cellulose; Modified cellulose
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- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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Abstract
A kind of electrochromism nano-cellulose composite and preparation method thereof, belongs to intellectual material technical field.Electrochromism nano-cellulose composite, including nano-cellulose, Polyethylene Glycol and aniline, solvent is N, N dimethyl acetylamide, its preparation method, comprises the following steps: (1) proportionally, by material dissolution in a solvent, 70 ~ 80 DEG C dissolve 1 ~ 4h, obtain the mixed solution of nano-cellulose；(2) by the mixed solution of nano-cellulose, under vacuum, 60 ~ 70 DEG C are deposited with, and obtain nano-cellulose thin film；(3) under inert gas shielding, by nano-cellulose thin film, carry out plasma radiation, obtain polyaniline nano fiber element composite；(4) by polyaniline nano fiber element composite, with soak with sulphuric acid, washing, dry, obtain electrochromism nano-cellulose composite.This electrochromism nano-cellulose composite, has preparation method simple, and environmental pollution is little, the feature that application prospect is huge.
Description
Technical field
A kind of electrochromism nano-cellulose composite of the present invention and preparation method thereof, belongs to intellectual material technology neck
Territory.
Background technology
Electrochromism refers to that material occurs the phenomenon that redox reaction causes color to change under electrochemical action, electroluminescent
Variable color is widely used at smart window, Anti-glare rearview mirror and display screen etc..Electrochromic device is in terms of driving voltage, stability
All there is high requirement.
Polyaniline is a kind of electrochromic conjugated conductive macromolecule, has raw material and is easy to get, and synthesis technique is simple, has good
The advantages such as good environmental stability and obtained studying widely and applying.Its color change many, cyclic reversibility good it is considered to be
The most electrochromic material of prospect.
Research currently for electrochromic material focuses mostly in improving polyaniline aspect of performance, is combined with other polymer
Form double-decker etc., less for flexible electrochromism investigation of materials.
In nature, cellulose can be described as a kind of inexhaustible, nexhaustible natural macromolecular material.And nanometer material
Material has small-size effect, skin effect, quantum effect, the physical properties such as adsorptivity, catalytic, optical, electrical, magnetic and chemistry,
Mechanical property has the performance of excellence.
Use cellulose as matrix, material prepared by composite polyphenylene amine, all have excellent in terms of flexibility, mechanical property
Gesture.
Summary of the invention
It is an object of the invention to provide a kind of electrochromism nano-cellulose composite and preparation method thereof, the method is led to
Cross and will there is the polyaniline of electrochromism and there is low-expansion transparent nanofiber element Film laminated, it is thus achieved that electroluminescent
Variable color nano-cellulose composite.
A kind of electrochromism nano-cellulose composite of the present invention, including nano-cellulose, Polyethylene Glycol and aniline,
Solvent is N,N-dimethylacetamide, wherein, in mass ratio, and nano-cellulose: Polyethylene Glycol: aniline=84 ~ 87:1 ~ 3:10 ~
15；The concentration in a solvent of nano-cellulose is 0.5 ~ 1.5g/ml；
Wherein, described polyethylene glycol relative molecular weight is 600 ~ 6000；
The preparation method of a kind of electrochromism nano-cellulose composite of the present invention, comprises the following steps:
(1) proportionally, by nano-cellulose, Polyethylene Glycol, aniline, being dissolved in N,N-dimethylacetamide, 70 ~ 80 DEG C molten
Solve 1 ~ 4h, obtain the mixed solution of nano-cellulose；
(2) by the mixed solution of nano-cellulose, under vacuum, 60 ~ 70 DEG C are deposited with, obtain nano-cellulose thin
Film；
Wherein said film thickness is 50 μm ~ 50nm；
(3) under inert gas shielding, by nano-cellulose thin film, carry out plasma radiation, obtain polyaniline nano fiber element multiple
Condensation material；
(4) by polyaniline nano fiber element composite, with soak with sulphuric acid 1 ~ 6h, then wash with water, 50 ~ 60 DEG C of drying,
Obtain electrochromism nano-cellulose composite；
Described noble gas is N2Or the one in Ar.
The step of described plasma radiation is: be placed on low-temperature plasma generator pallet by nano-cellulose thin film,
Air, after dried, enters in the reaction chamber of low-temperature plasma generator, and evacuation, after stable gas pressure, carries out microwave
Electric discharge, is 25 ~ 100W in radiant power, and radiated time is 1 ~ 2h, stop electric discharge, close power supply, be passed through air to normal pressure.
Described drying uses vacuum drying oven to dry.
It is an advantage of the current invention that: this electrochromism nano-cellulose composite there is preparation method simple, to environment
Pollute little, the feature that application prospect is huge.Meanwhile, the present invention use lower temperature plasma technology have low temperature, quickly, efficiently,
The feature such as pollution-free.
Detailed description of the invention
Below in conjunction with specific embodiment case, the present invention it is described and is further appreciated by the present invention, not representing structure of the present invention
Whole technical scheme under Siing, it is impossible to be interpreted as the restriction to technical scheme.
Following example plasma radiation uses microwave low-temperature plasma generator.
Embodiment 1
A kind of electrochromism nano-cellulose composite, including nano-cellulose, Polyethylene Glycol and aniline, solvent is N, N-bis-
Methylacetamide, wherein, in mass ratio, nano-cellulose: Polyethylene Glycol: aniline=84:3:13；Nano-cellulose at solvent
In concentration be 0.5g/ml；Polyethylene glycol relative molecular weight is 6000；
The preparation method of a kind of electrochromism nano-cellulose composite, comprises the following steps:
(1) according to aforementioned proportion, in there-necked flask, by nano-cellulose, Polyethylene Glycol, aniline, it is dissolved in N, N-dimethyl
In acetamide, in water-bath, it is heated to 70 DEG C and dissolves 4h, obtain the mixed solution of nano-cellulose；
(2) by the mixed solution of nano-cellulose, on film forming mould, under vacuum, 60 DEG C are deposited with, obtain nanometer
Cellulose membrane；Film thickness is 10nm；
(3) at N2Under protection, being placed on low-temperature plasma generator pallet by nano-cellulose thin film, air is through dried
After, enter in the reaction chamber of low-temperature plasma generator, evacuation, after stable gas pressure, carry out microwave discharge, in radiant power be
25W, radiated time is 2h, stop electric discharge, close power supply, be passed through air to normal pressure；Complete plasma radiation process, gathered
Aniline nano-fiber element composite；
(4) by polyaniline nano fiber element composite, use soak with sulphuric acid 6h, then wash with water, 50 DEG C of drying, obtain electricity
Mutagens color nano-cellulose composite.
Embodiment 2
A kind of electrochromism nano-cellulose composite, including nano-cellulose, Polyethylene Glycol and aniline, solvent is N, N-bis-
Methylacetamide, wherein, in mass ratio, nano-cellulose: Polyethylene Glycol: aniline=87:3:10；Nano-cellulose at solvent
In concentration be 1.0g/ml；Polyethylene glycol relative molecular weight is 4000；
The preparation method of a kind of electrochromism nano-cellulose composite, comprises the following steps:
(1) according to aforementioned proportion, in there-necked flask, by nano-cellulose, Polyethylene Glycol, aniline, it is dissolved in N, N-dimethyl
In acetamide, in water-bath, it is heated to 80 DEG C and dissolves 1h, obtain the mixed solution of nano-cellulose；
(2) by the mixed solution of nano-cellulose, on film forming mould, under vacuum, 70 DEG C are deposited with, obtain nanometer
Cellulose membrane；Film thickness is 50nm；
(3) under Ar gas shielded, being placed on low-temperature plasma generator pallet by nano-cellulose thin film, air is through being dried place
After reason, enter in the reaction chamber of low-temperature plasma generator, evacuation, after stable gas pressure, carry out microwave discharge, in radiant power
For 100W, radiated time is 1h, stop electric discharge, close power supply, be passed through air to normal pressure；Complete plasma radiation process, obtain
Polyaniline nano fiber element composite；
(4) by polyaniline nano fiber element composite, use soak with sulphuric acid 1h, then wash with water, 60 DEG C of drying, obtain electricity
Mutagens color nano-cellulose composite.
Embodiment 3
A kind of electrochromism nano-cellulose composite, including nano-cellulose, Polyethylene Glycol and aniline, solvent is N, N-bis-
Methylacetamide, wherein, in mass ratio, nano-cellulose: Polyethylene Glycol: aniline=87:3:10；Nano-cellulose at solvent
In concentration be 1.0g/ml；Polyethylene glycol relative molecular weight is 4000；
The preparation method of a kind of electrochromism nano-cellulose composite, comprises the following steps:
(1) according to aforementioned proportion, in there-necked flask, by nano-cellulose, Polyethylene Glycol, aniline, it is dissolved in N, N-dimethyl
In acetamide, in water-bath, it is heated to 80 DEG C and dissolves 1h, obtain the mixed solution of nano-cellulose；
(2) by the mixed solution of nano-cellulose, on film forming mould, under vacuum, 70 DEG C are deposited with, obtain nanometer
Cellulose membrane；Film thickness is 50nm；
(3) under Ar gas shielded, being placed on low-temperature plasma generator pallet by nano-cellulose thin film, air is through being dried place
After reason, enter in the reaction chamber of low-temperature plasma generator, evacuation, after stable gas pressure, carry out microwave discharge, in radiant power
For 100W, radiated time is 1h, stop electric discharge, close power supply, be passed through air to normal pressure；Complete plasma radiation process, obtain
Polyaniline nano fiber element composite；
(4) by polyaniline nano fiber element composite, use soak with sulphuric acid 1h, then wash with water, 60 DEG C of drying, obtain electricity
Mutagens color nano-cellulose composite.
Embodiment 4
A kind of electrochromism nano-cellulose composite, including nano-cellulose, Polyethylene Glycol and aniline, solvent is N, N-bis-
Methylacetamide, wherein, in mass ratio, nano-cellulose: Polyethylene Glycol: aniline=84:2:14；Nano-cellulose at solvent
In concentration be 1.5g/ml；Polyethylene glycol relative molecular weight is 600；
The preparation method of a kind of electrochromism nano-cellulose composite, comprises the following steps:
(1) according to aforementioned proportion, in there-necked flask, by nano-cellulose, Polyethylene Glycol, aniline, it is dissolved in N, N-dimethyl
In acetamide, in water-bath, it is heated to 75 DEG C and dissolves 2h, obtain the mixed solution of nano-cellulose；
(2) by the mixed solution of nano-cellulose, on film forming mould, under vacuum, 70 DEG C are deposited with, obtain nanometer
Cellulose membrane；Film thickness is 50 μm；
(3) under Ar gas shielded, being placed on low-temperature plasma generator pallet by nano-cellulose thin film, air is through being dried place
After reason, enter in the reaction chamber of low-temperature plasma generator, evacuation, after stable gas pressure, carry out microwave discharge, in radiant power
For 50W, radiated time is 1h, stop electric discharge, close power supply, be passed through air to normal pressure；Complete plasma radiation process, obtain
Polyaniline nano fiber element composite；
(4) by polyaniline nano fiber element composite, use soak with sulphuric acid 3h, then wash with water, 60 DEG C of drying, obtain electricity
Mutagens color nano-cellulose composite.
Embodiment 4
A kind of electrochromism nano-cellulose composite, including nano-cellulose, Polyethylene Glycol and aniline, solvent is N, N-bis-
Methylacetamide, wherein, in mass ratio, nano-cellulose: Polyethylene Glycol: aniline=84:1:15；Nano-cellulose at solvent
In concentration be 1.0g/ml；Polyethylene glycol relative molecular weight is 4000；
The preparation method of a kind of electrochromism nano-cellulose composite, comprises the following steps:
(1) according to aforementioned proportion, in there-necked flask, by nano-cellulose, Polyethylene Glycol, aniline, it is dissolved in N, N-dimethyl
In acetamide, in water-bath, it is heated to 80 DEG C and dissolves 1h, obtain the mixed solution of nano-cellulose；
(2) by the mixed solution of nano-cellulose, on film forming mould, under vacuum, 70 DEG C are deposited with, obtain nanometer
Cellulose membrane；Film thickness is 25nm；
(3) under Ar gas shielded, being placed on low-temperature plasma generator pallet by nano-cellulose thin film, air is through being dried place
After reason, enter in the reaction chamber of low-temperature plasma generator, evacuation, after stable gas pressure, carry out microwave discharge, in radiant power
For 25W, radiated time is 1h, stop electric discharge, close power supply, be passed through air to normal pressure；Complete plasma radiation process, obtain
Polyaniline nano fiber element composite；
(4) by polyaniline nano fiber element composite, use soak with sulphuric acid 3h, then wash with water, 50 DEG C of drying, obtain electricity
Mutagens color nano-cellulose composite.
Claims (6)
1. an electrochromism nano-cellulose composite, it is characterised in that include nano-cellulose, Polyethylene Glycol and benzene
Amine, solvent is N,N-dimethylacetamide, wherein, in mass ratio, nano-cellulose: Polyethylene Glycol: aniline=84 ~ 87:1 ~ 3:10
~15；The concentration in a solvent of nano-cellulose is 0.5 ~ 1.5g/ml.
2. require described electrochromism nano-cellulose composite according to right 1, it is characterised in that described Polyethylene Glycol
Relative molecular mass is 600 ~ 6000.
3. the preparation method of a kind of electrochromism nano-cellulose composite of right 1, it is characterised in that include following step
Rapid:
(1) proportionally, by nano-cellulose, Polyethylene Glycol, aniline, being dissolved in N,N-dimethylacetamide, 70 ~ 80 DEG C molten
Solve 1 ~ 4h, obtain the mixed solution of nano-cellulose；
(2) by the mixed solution of nano-cellulose, under vacuum, 60 ~ 70 DEG C are deposited with, obtain nano-cellulose thin
Film；
Wherein said film thickness is 50 μm ~ 50nm；
(3) under inert gas shielding, by nano-cellulose thin film, carry out plasma radiation, obtain polyaniline nano fiber element multiple
Condensation material；
(4) by polyaniline nano fiber element composite, with soak with sulphuric acid 1 ~ 6h, then wash with water, 50 ~ 60 DEG C of drying,
Obtain electrochromism nano-cellulose composite.
4. require the preparation method of described electrochromism nano-cellulose composite according to right 3, it is characterised in that described
(3) noble gas in is N2Or the one in Ar.
5. require the preparation method of described electrochromism nano-cellulose composite according to right 3, it is characterised in that described
(3) step of the plasma radiation in is: be placed on low-temperature plasma generator pallet by nano-cellulose thin film, and air passes through
After dried, enter in the reaction chamber of low-temperature plasma generator, evacuation, after stable gas pressure, carry out microwave discharge, at spoke
Penetrating power is 25 ~ 100W, and radiated time is 1 ~ 2h, stop electric discharge, close power supply, be passed through air to normal pressure.
6. require the preparation method of described electrochromism nano-cellulose composite according to right 3, it is characterised in that described
(4) drying in uses vacuum drying oven to dry.
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Cited By (4)
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| CN107501617A (en) * | 2017-08-02 | 2017-12-22 | 青岛科技大学 | A kind of purpurine/Cellulose nanocrystal composite membrane and preparation method thereof and detachable electrochromic device |
| CN108102106A (en) * | 2017-12-06 | 2018-06-01 | 陕西科技大学 | A kind of photochromic fibre element and preparation method thereof |
| CN110551300A (en) * | 2018-05-30 | 2019-12-10 | 华南理工大学 | Water-resistant transparent cellulose-based film and preparation method thereof |
| CN110551301A (en) * | 2018-05-30 | 2019-12-10 | 华南理工大学 | Water-resistant nano cellulose film and preparation method thereof |
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| CN108102106A (en) * | 2017-12-06 | 2018-06-01 | 陕西科技大学 | A kind of photochromic fibre element and preparation method thereof |
| CN108102106B (en) * | 2017-12-06 | 2021-02-26 | 陕西科技大学 | Photochromic cellulose and preparation method thereof |
| CN110551300A (en) * | 2018-05-30 | 2019-12-10 | 华南理工大学 | Water-resistant transparent cellulose-based film and preparation method thereof |
| CN110551301A (en) * | 2018-05-30 | 2019-12-10 | 华南理工大学 | Water-resistant nano cellulose film and preparation method thereof |
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Application publication date: 20161214 |