CN105906846A - Cyanoethyl cellulose-based high-dielectric nano composite film and preparation method thereof - Google Patents
Cyanoethyl cellulose-based high-dielectric nano composite film and preparation method thereof Download PDFInfo
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- CN105906846A CN105906846A CN201610290761.4A CN201610290761A CN105906846A CN 105906846 A CN105906846 A CN 105906846A CN 201610290761 A CN201610290761 A CN 201610290761A CN 105906846 A CN105906846 A CN 105906846A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
The invention relates to cyanoethyl cellulose-based high-dielectric nano composite film and a preparation method thereof and aims to provide a degradable high-dielectric flexible nano composite film high in dielectric constant, low in dielectric loss and good in mechanical property and thermal performance, and a preparation method thereof. The preparation method includes: using cyanoethyl cellulose as a base, graphene as a filer and montmorillonite as a dispersant, preparing a solution with a solvent and forming the film by casting. The cyanoethyl cellulose for preparing the high-dielectric flexible nano composite film is a renewable source, the composite film is high in dielectric performance, low in dielectric loss, applicable to electronics, motor and cable industries and is also certainly applicable to the fields such as artificial muscle, wave-absorbing materials and drug slow release, the production method is safe, a process is simple, production cost is low, and therefore the film has a promising market prospect.
Description
Technical field
The present invention relates to a kind of high dielectric material and preparation method thereof, be specifically related to a kind of cyanethyl cellulose base
High dielectric nano composite membrane and preparation method thereof.
Background technology
High dielectric material is a kind of application prospect material widely.Along with capacitor, resonator, filtering
Numerous important electronic device such as device, memorizer, to high performance and the development in miniaturization direction, has high dielectric
The polymer based nanocomposites of constant is paid attention to by increasing scientific research personnel.Owing to polymer has
There are high breakdown strength, low dielectric loss, good processing characteristics and low cost, thus it is usually used in
Energy storage.But the dielectric constant of general high polymer is relatively low, therefore, original well at reservation polymer
Improve its dielectric properties on the basis of performance and become an important problem.
For improving the dielectric properties of polymer matrix composite, researcher develops a lot of system.One
Simple method is the ceramic packing adding in the polymer matrix and having high-k, but uses this side
Method, even if the ceramic packing adding high-load is also difficult to the composite obtaining dielectric constant higher than 100, and
And high filer content can make composite have high mass density, more hole and the pliability of difference.
Another conventional method is to add conductive filler in the polymer matrix, such as CNT, white carbon black, graphite
Alkene, carbon fiber, metallic particles etc..In these conductive fillers, owing to Graphene has high specific surface
The performances such as long-pending and excellent optics, electricity, calorifics and machinery, it has lower in the composite
Percolation threshold, therefore suffers from more paying close attention to.According to seepage theory, when the addition of Graphene oozes close to it
During stream threshold value, the dielectric constant of composite can dramatically increase.But, strong owing to existing between Graphene
Van der Waals force, therefore they be very easy to assemble, thus cause its in the composite dispersibility very poor.
Patent CN201310089200.4 reports with cyanethyl cellulose as base material, is prepared for cyanoethyl fiber
Element/graphene composite material, but its preparation method is complex, and the hydrogen iodide utilizing corrosivity stronger enters
Row in-situ reducing, has bigger corrosion damage to the surface of composite.For improving Graphene in the base
Dispersibility and the compatibility, have two kinds of more effective methods, and one is Physical, is i.e. made by electrostatic interaction
It disperses and improves its compatibility, and then improves its dielectric constant；Another kind of method is exactly chemical method, the most right
Graphenic surface carries out covalent modified, introduces macromolecular chain on its surface, thus suppresses between graphene sheet layer
Reunion.But chemical method preparation process is complex, and Physical is the most simple to operate, one of can yet be regarded as
Efficient approach.For improving Nano filling dispersibility in the base, patent CN104672502A is invented
A kind of method that barium titanate nano granule carrys out dispersing Nano carbon tubes, may certify that physical method can be effectively
Improve Nano filling dispersibility in the base and the compatibility, obtain the nano composite material that dielectric constant is higher.
At present, polymer base high-dielectric composite material matrix mainly with Kynoar (PVDF) copolymer,
Polyimides, epoxy resin, polyethylene and polymethyl methacrylate etc. are base material, by with ceramic, golden
Belong to, prepared by organic semiconductor doped and compounded.General polymerization thing base material is except Kynoar and copolymer thereof
Dielectric constant is higher than beyond 5, and other polymer is generally less than 5.Patent CN201410638440.X and
Patent CN201210179758.7 discloses a kind of Graphene/polymer base high dielectric material, but general poly-
Compound matrix such as PVDF is difficult to degrade, and raw material cannot regenerate.Therefore prepare new, wide material sources, can
Biodegradable composite material with high dielectric constant is the trend of a certainty.
Cellulose is the natural polymer that distributed in nature is the widest, reserves are maximum, and having can degradable, nothing
Pollution, the advantage of good biocompatibility, be a kind of inexhaustible Renewable resource, be people
Generally acknowledge future source of energy, chemical materials.Cellulose derivative has been acted on the biocompatibility of cellulose, can drop
Xie Xing.Cyanethyl cellulose (CEC) is a kind of cellulose ether, has higher dielectric constant, typically exists
More than 10.The CEC of high substituted degree also has the features such as high water proofing property, high-insulativity and self-extinguishment.With its be
High dielectric material prepared by base material is because the dielectric properties of himself are higher, biocompatibility preferable, in biological work
Journey field has a wide range of applications.
Summary of the invention
The invention aims to provide one to have high-k, low-dielectric loss, good mechanical
Can be with degradable high dielectric flexible nano composite membrane of hot property and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is: a kind of cyanethyl cellulose base high dielectric
Nano composite membrane comprises following parts by weight of component and mixes: cyanethyl cellulose 10 parts, Graphene 0.1-1.5 part,
Solvent 300-500 part；Described nano composite membrane, with described cyanethyl cellulose as matrix, with described Graphene is
Filler, with montmorillonite as dispersant, is configured to solution with described solvent, prepares through casting film-forming.
Further, described nano composite membrane includes following parts by weight of component: cyanethyl cellulose 10 parts, stone
1 part of alkene of ink, solvent 400 parts.
Further, described cyanethyl cellulose substitution value is 2.4-2.6.
Further, the carbon-to-oxygen ratio of described Graphene is 7-18.
Further, described solvent is DMF, N,N-dimethylacetamide, N-methyl pyrrole
Any one in pyrrolidone.
Further, the thickness of described dried composite membrane is 0.030-0.100mm.
The preparation method of above-mentioned cyanethyl cellulose base height dielectric nano composite membrane includes step:
A. graphene oxide is prepared: use Hummers method to prepare graphene oxide；
B. redox graphene: use graphene oxide prepared by microwave method or heating reduction step A；
Wherein microwave method step is: by 10 parts of graphene oxide ultrasonic disperse to solvent, add the reduction of 0.01 part
Agent, is placed in reduction reaction in microwave reactor, and power is 100-800W, and temperature is 40-60 DEG C, during reaction
Between be 5-20min, reaction is centrifuged, washs after terminating, be dried and prepare redox graphene；
Heating reduction step is: graphene oxide reduces at 980-1000 DEG C 30s；
C. prepared by composite membrane: be dissolved in 300 parts of solvents by 10 parts of cyanethyl celluloses, by 0.5-2 part stone
Ink alkene and 0.1-1 part montmorillonite are distributed in 100 parts of solvents, fine by joining cyanoethyl in aftermentioned solution stirring
Dimension cellulose solution prepares preparation liquid, preparation liquid is poured on ganoid culture dish, casting film-forming, so
It is placed in baking oven, is drying to obtain at 50-60 DEG C.
Further, described reducing agent is phenylhydrazine or hydrazine hydrate.That is two kinds of reducing agents are used equally to this
The preparation method of the high dielectric flexible nano composite membrane described in invention.
Further, solvent described in the preparation method of cyanethyl cellulose base height dielectric nano composite membrane be water,
One in N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone.
Use the inventive method to prepare high dielectric flexible nano composite membrane to have the advantage that
1. the raw material sources preparing cyanethyl cellulose are extensive, and fully biodegradable is pollution-free, are a kind of
Inexhaustible, nexhaustible Renewable resource.
2. the dielectric of the flexible high dielectric nano composite membrane of the cyanethyl cellulose/Graphene prepared/montmorillonite
Performance is higher, and dielectric loss is relatively low, can apply to electronics, motor and cable industry, and artificial muscle
Also there is certain application prospect in the fields such as meat, absorbing material and medicament slow release.
3. the flexible high dielectric nano composite film surface of the cyanethyl cellulose/Graphene prepared/montmorillonite has
Gloss, good looking appearance, there is certain pliability.
4. the flexible high dielectric nano composite membrane of the cyanethyl cellulose/Graphene prepared/montmorillonite has good
Good mechanical performance and hot property.
5. the flexible high dielectric nano composite membrane producer of the cyanethyl cellulose/Graphene prepared/montmorillonite
Method safety, flow process is simple, and production cost is low, therefore good market prospects.
6. the dielectric of the flexible high dielectric nano composite membrane of the cyanethyl cellulose/Graphene prepared/montmorillonite
Constant is higher than not adding the dielectric constant of montmorillonite, such as, Graphene content all when 5%, respectively 39.6
With 21.9.
Accompanying drawing explanation
Fig. 1 is Graphene and Graphene/montmorillonite is dispersed in DMF the digital photograph after standing 5 days respectively.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.Described embodiment is only the excellent of the present invention
Selecting embodiment, be not limited to the present invention, for a person skilled in the art, the present invention can
There to be various modifications and variations.All within the spirit and principles in the present invention, any amendment of being made, equivalent
Replacement, improvement etc., should be included within the scope of the present invention.In embodiment one to four, product
Dielectric properties use Agilent 4294A electric impedance analyzer to be measured, and heat stability uses TG-DTA
6200LAB SYS type thermogravimetric differential thermal Thermal Synthetic Analysis instrument is measured.
In Fig. 1, a bottle i.e. this bottle of the left side is the photo after graphene dispersion stands 5 days in DMF, and b bottle is i.e.
This bottle of the right is that Graphene/montmorillonite is dispersed in the photo after DMF stands 3 days, is the most intuitively apparent from
The dispersion effect of both Graphenes is entirely different, and the dispersion effect of the latter is significantly better than the former.
Embodiment one
0.6g cyanethyl cellulose is dissolved in 20gDMF, magnetic agitation 2h, dissolves.0.006g graphite
Alkene and 0.06g montmorillonite ultrasonic disperse, in 20g DMF, stir 1h, ultrasonic disperse 6h.After dispersion
Graphene/montmorillonite suspension liquid joins in the solution of cyanethyl cellulose, obtains mixed solution, magnetic agitation
4h, ultrasonic 4h.Film forming solution is poured in surface plate, is placed in 60 DEG C of dry about 48h in baking oven, cooling
After take off film, i.e. can get cyanethyl cellulose/Graphene/montmorillonite height dielectric flexible nano composite membrane.
Property with the standby cyanethyl cellulose base height dielectric flexible nano composite membrane of this component and weight in grams numeral system
Can be: dielectric constant and dielectric loss are respectively 27.0 and 0.46 (100Hz)；Heat decomposition temperature is 327 DEG C.
Embodiment two
0.6g cyanethyl cellulose is dissolved in 20gDMF, magnetic agitation 2h, dissolves.0.03g graphite
Alkene and 0.06g montmorillonite ultrasonic disperse, in 20gDMF, stir 1h, ultrasonic disperse 6h.After dispersion
Graphene/montmorillonite suspension liquid joins in the solution of cyanethyl cellulose, obtains mixed solution, magnetic agitation
4h, ultrasonic 4h.Film forming solution is poured in surface plate, is placed in 60 DEG C of dry about 48h in baking oven, cooling
After take off film, i.e. can get cyanethyl cellulose/Graphene/montmorillonite height dielectric flexible nano composite membrane.
Property with the standby cyanethyl cellulose base height dielectric flexible nano composite membrane of this component and weight in grams numeral system
Can be: dielectric constant and dielectric loss are respectively 39.6 and 0.047 (100Hz)；Heat decomposition temperature is 319.3 DEG C.
Embodiment three
0.6g cyanethyl cellulose is dissolved in 20gDMF, magnetic agitation 2h, dissolves.0.042g graphite
Alkene and 0.06g montmorillonite ultrasonic disperse, in 20gDMF, stir 1h, ultrasonic disperse 6h.After dispersion
Graphene/montmorillonite suspension liquid joins in the solution of cyanethyl cellulose, obtains mixed solution, magnetic agitation
4h, ultrasonic 4h.Film forming solution is poured in surface plate, is placed in 60 DEG C of dry about 48h in baking oven, cooling
After take off film, i.e. can get cyanethyl cellulose/Graphene/montmorillonite height dielectric flexible nano composite membrane.
Property with the standby cyanethyl cellulose base height dielectric flexible nano composite membrane of this component and weight in grams numeral system
Can be: dielectric constant and dielectric loss are respectively 62.7 and 0.073 (100Hz)；Heat decomposition temperature is 266.6 DEG C
With 315.6 DEG C.
Embodiment four
The flexible high dielectric nano composite membrane of cyanethyl cellulose/Graphene/montmorillonite, its component and weight grams
For, cyanethyl cellulose 0.6g, thermal reduction Graphene 0.072g, montmorillonite 0.036g.
0.6g cyanethyl cellulose is dissolved in 20gDMF, magnetic agitation 2h, dissolves.0.072g graphite
Alkene and 0.06g montmorillonite ultrasonic disperse, in 20gDMF, stir 1h, ultrasonic disperse 6h.After dissolving
Polyacrylonitrile-grafted modified Graphene joins in the solution of cyanethyl cellulose, obtains mixed solution, magnetic force
Stirring 4h, ultrasonic 4h.Film forming solution is poured in surface plate, is placed in 60 DEG C of dry about 48h in baking oven,
Take off film after cooling, i.e. can get cyanethyl cellulose/Graphene/montmorillonite height dielectric flexible nano composite membrane.
Property with the standby cyanethyl cellulose base height dielectric flexible nano composite membrane of this component and weight in grams numeral system
Can be: dielectric constant and dielectric loss are respectively 912 and 17 (100Hz)；Heat decomposition temperature 313.3 DEG C.
Embodiment five
0.6g cyanethyl cellulose is dissolved in 20gDMF, magnetic agitation 2h, dissolves.0.03g graphite
Alkene and 0.06g montmorillonite ultrasonic disperse, in 20gDMF, stir 1h, ultrasonic disperse 6h.After dispersion
Graphene/montmorillonite suspension liquid joins in the solution of cyanethyl cellulose, obtains mixed solution, magnetic agitation
4h, ultrasonic 4h.Film forming solution is poured in surface plate, is placed in 60 DEG C of dry about 48h in baking oven, cooling
After take off film, i.e. can get cyanethyl cellulose/Graphene/montmorillonite height dielectric flexible nano composite membrane.
Property with the standby cyanethyl cellulose base height dielectric flexible nano composite membrane of this component and weight in grams numeral system
Can be: dielectric constant and dielectric loss are respectively 30.01 and 0.404 (100Hz).
Embodiment six
The flexible high dielectric nano composite membrane of cyanethyl cellulose/Graphene/montmorillonite, its component and weight grams
For, cyanethyl cellulose 0.6g, the Graphene 0.06g of microwave reduction, montmorillonite 0.06g.
0.6g cyanethyl cellulose is dissolved in 20gDMF, magnetic agitation 2h, dissolves.0.06g graphite
Alkene and 0.06g montmorillonite ultrasonic disperse, in 20gDMF, stir 1h, ultrasonic disperse 6h.After dispersion
Graphene/montmorillonite suspension liquid joins in the solution of cyanethyl cellulose, obtains mixed solution, magnetic agitation
4h, ultrasonic 4h.Film forming solution is poured in surface plate, is placed in 60 DEG C of dry about 48h in baking oven, cooling
After take off film, i.e. can get cyanethyl cellulose/Graphene/montmorillonite height dielectric flexible nano composite membrane.
Property with the standby cyanethyl cellulose base height dielectric flexible nano composite membrane of this component and weight in grams numeral system
Can be: dielectric constant and dielectric loss are respectively 110.1 and 0.75 (100Hz).
Claims (9)
1. a cyanethyl cellulose base height dielectric nano composite membrane, it is characterised in that: comprise following weight portion
Component mixes: cyanethyl cellulose 10 parts, Graphene 0.1-1.5 part, solvent 300-500 part；Described nanometer
Composite membrane is with described cyanethyl cellulose as matrix, with described Graphene as filler, with montmorillonite as dispersant,
It is configured to solution with described solvent, prepares through casting film-forming.
Nano composite membrane the most according to claim 1, it is characterised in that: described nano composite membrane includes
Following parts by weight of component: cyanethyl cellulose 10 parts, Graphene 0.1-1 part, solvent 300-500 part.
Nano composite membrane the most according to claim 1 and 2, it is characterised in that: described cyanoethyl fiber
Element substitution value is 2.4-2.6.
Nano composite membrane the most according to claim 1 and 2, it is characterised in that: the carbon of described Graphene
Oxygen is than for 7-18.
Nano composite membrane the most according to claim 1 and 2, it is characterised in that: described solvent is N, N-
Any one in dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone.
Nano composite membrane the most according to claim 1 and 2, it is characterised in that: described dried multiple
The thickness closing film is 0.030-0.100mm.
Cyanethyl cellulose base height dielectric nano the most as claimed in any of claims 1 to 6 is combined
The preparation method of film, it is characterised in that: include step:
A. graphene oxide is prepared: use Hummers method to prepare graphene oxide；
B. redox graphene: use graphene oxide prepared by microwave method or heating reduction step A；
Wherein microwave method step is: by 10 parts of graphene oxide ultrasonic disperse to solvent, add the reduction of 0.01 part
Agent, is placed in reduction reaction in microwave reactor, and power is 100-800W, and temperature is 40-60 DEG C, during reaction
Between be 5-20min, reaction is centrifuged, washs after terminating, be dried and prepare redox graphene；
Heating reduction step is: graphene oxide reduces at 980-1000 DEG C 30s；
C. prepared by composite membrane: be dissolved in 300 parts of solvents by 10 parts of cyanethyl celluloses, by 0.1-1 part stone
Ink alkene and 0.1-1 part montmorillonite are distributed in 100 parts of solvents, fine by joining cyanoethyl in aftermentioned solution stirring
Dimension cellulose solution prepares preparation liquid, preparation liquid is poured on ganoid culture dish, casting film-forming, so
It is placed in baking oven, is drying to obtain at 50-60 DEG C.
The preparation method of nano composite membrane the most according to claim 7, it is characterised in that: described reduction
Agent is phenylhydrazine or hydrazine hydrate.
The preparation method of nano composite membrane the most according to claim 7, it is characterised in that: described solvent
For the one in water, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone.
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| CN106947103A (en) * | 2017-04-11 | 2017-07-14 | 深圳市佩成科技有限责任公司 | The preparation method of the related serial composite membrane of graphene |
| WO2018187923A1 (en) * | 2017-04-11 | 2018-10-18 | 深圳市佩成科技有限责任公司 | Preparation method for graphene-related series of composite films |
| CN109266641A (en) * | 2018-09-27 | 2019-01-25 | 福建海峡石墨烯产业技术研究院有限公司 | A kind of method and detecting electrode that enzyme is fixed on graphene based on glutaraldehyde |
| CN111565481A (en) * | 2020-05-20 | 2020-08-21 | 宁波石墨烯创新中心有限公司 | Graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106947103A (en) * | 2017-04-11 | 2017-07-14 | 深圳市佩成科技有限责任公司 | The preparation method of the related serial composite membrane of graphene |
| WO2018187923A1 (en) * | 2017-04-11 | 2018-10-18 | 深圳市佩成科技有限责任公司 | Preparation method for graphene-related series of composite films |
| CN109266641A (en) * | 2018-09-27 | 2019-01-25 | 福建海峡石墨烯产业技术研究院有限公司 | A kind of method and detecting electrode that enzyme is fixed on graphene based on glutaraldehyde |
| CN111565481A (en) * | 2020-05-20 | 2020-08-21 | 宁波石墨烯创新中心有限公司 | Graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film and preparation method thereof |
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