CN108948622A - A kind of epoxy-modified graphene film and preparation method thereof - Google Patents
A kind of epoxy-modified graphene film and preparation method thereof Download PDFInfo
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- CN108948622A CN108948622A CN201810682243.6A CN201810682243A CN108948622A CN 108948622 A CN108948622 A CN 108948622A CN 201810682243 A CN201810682243 A CN 201810682243A CN 108948622 A CN108948622 A CN 108948622A
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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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
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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
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
-
- 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
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
Abstract
The invention discloses a kind of epoxy-modified graphene films and preparation method thereof, and the film is made of the raw material of following weight parts: lithium methoxide 0.07-0.1, epoxy prapanol 10-13, methyl methacrylate 25-30, graphene oxide 100-110, amination polyester emulsion 46-50, hexabromocyclododecane 2-3.The present invention is using methyl methacrylate, epoxy prapanol as feedstock processing activated graphene, obtain epoxy-modified graphene, finally be blended with amination polyester emulsion promote epoxy ring-opening, so as to improve the compatibility between each raw material, thus improve finished films mechanics and uniform and stable property.
Description
Technical field
The invention belongs to film applications, and in particular to a kind of epoxy-modified graphene film and preparation method thereof.
Background technique
Conductive film is the functional material that liquid crystal display, touch panel etc. must use.At this stage mature preparation process,
The conductive film of function admirable is mainly based on metallic film and metal-oxide film, and tin indium oxide is with good optics and electricity
Property is learned, shown industry is widely used.But since sputtering ito film layer needs to carry out at high temperature, and its microstructure is
Column structure, is accordingly used in flexible substrates low temperature or room temperature plated film is just limited to, and significantly limits flexible display technologies
Development；
Therefore, finding, there is high conduction performance, flexible and transparent and cheap substance ITO to be replaced to be development trend, from
Since two-dimensional material graphene comes out, excellent electrology characteristic and good light transmittance cause the extensive concern of people.
Meanwhile graphene is recognized the atomic-level thickness of vertical direction, atomically flating, surface inertness and zero trap states the features such as
To be the material for replacing ITO most potential, become the research hotspot of current international display field.However, current graphene is thin
Film application range is smaller, functional more single.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of epoxy-modified graphene film and
Preparation method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of epoxy-modified graphene film, it is composed of the following raw materials by weight:
Lithium methoxide 0.07-0.1, epoxy prapanol 10-13, methyl methacrylate 25-30, graphene oxide 100-110, amine
Change polyester emulsion 46-50, hexabromocyclododecane 2-3.
A kind of epoxy-modified graphene film, the preparation method of the amination polyester emulsion, including following step
It is rapid:
(1) ammonium persulfate for taking 1-2 parts by weight is added in the deionized water of 30-40 times of its weight, stirs evenly；
(2) methyl acrylate of 30-40 parts by weight, the butyl acrylate mixing of 10-15 parts by weight are taken, is added to above-mentioned mixed
It closes in the deionized water for expecting 6-9 times of weight, stirs evenly, be sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is
65-70 DEG C, the diethylenetriamine of above-mentioned ammonium persulfate aqueous solution, 4-5 parts by weight is added, insulated and stirred 4-6 hours, discharges cold
But to get.
The preparation method of the epoxy-modified graphene film, comprising the following steps:
(1) hexabromocyclododecane is taken, is added in the dehydrated alcohol of 20-24 times of its weight, stirs evenly, oxidation stone is added
Black alkene, increasing temperature is 55-60 DEG C, insulated and stirred 2-3 hours, ethyl alcohol is distilled off, obtains activated graphene；
(2) methyl methacrylate, epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen, is adjusted anti-
Answering kettle temperature degree is 90-105 DEG C, is stirred to react 1-2 hours, and lithium methoxide, activated graphene is added, and adjusting temperature of reaction kettle is 150-
160 DEG C, insulated and stirred 3-4 hours, discharging cooling obtained epoxy-modified graphene；
(3) above-mentioned epoxy-modified graphene is taken, is added in amination polyester emulsion, stirs evenly, is stirred at 25-30 DEG C
1-2 hours, increasing temperature was 160-180 DEG C, and dimethylformamide is added, insulated and stirred 100-140 minutes, is uniformly coated in
It on glass plate, is sent into baking oven, 10-13 hours dry at 70-75 DEG C, discharging cooling takes off film to get the epoxy-modified stone
Black alkene film.
Advantages of the present invention:
The present invention polymerize under initiator effect, uses in polymerization process using methyl acrylate, butyl acrylate as monomer
Diethylenetriamine is modified, obtains amination polyester liquid, later handles graphene using hexabromocyclododecane, it is thin to improve finished product
The hydrophobic properties of the surface of film, the present invention obtain epoxy using methyl methacrylate, epoxy prapanol as feedstock processing activated graphene
Modified graphene is finally blended with amination polyester emulsion and promotes epoxy ring-opening, so as to improve the compatibility between each raw material,
To improve finished films mechanics and uniform and stable property.
Specific embodiment
Embodiment 1
A kind of epoxy-modified graphene film, it is composed of the following raw materials by weight:
Lithium methoxide 0.1, epoxy prapanol 13, methyl methacrylate 30, graphene oxide 110, amination polyester emulsion 50, six
Bromine cyclododecane 3.
A kind of epoxy-modified graphene film, the preparation method of the amination polyester emulsion, including following step
It is rapid:
(1) ammonium persulfate for taking 2 parts by weight is added in the deionized water of 40 times of its weight, stirs evenly；
(2) methyl acrylate of 40 parts by weight, the butyl acrylate mixing of 15 parts by weight are taken, above-mentioned mixture weight is added to
It in the deionized water of 9 times of amount, stirs evenly, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is 70 DEG C, is added
The diethylenetriamine of above-mentioned ammonium persulfate aqueous solution, 5 parts by weight, insulated and stirred 6 hours, discharging it is cooling to get.
The preparation method of the epoxy-modified graphene film, comprising the following steps:
(1) hexabromocyclododecane is taken, is added in the dehydrated alcohol of 24 times of its weight, stirs evenly, graphite oxide is added
Alkene, increasing temperature is 60 DEG C, insulated and stirred 3 hours, ethyl alcohol is distilled off, obtains activated graphene；
(2) methyl methacrylate, epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen, is adjusted anti-
Answering kettle temperature degree is 105 DEG C, is stirred to react 2 hours, and lithium methoxide, activated graphene is added, and adjusting temperature of reaction kettle is 160 DEG C, is protected
Temperature stirring 4 hours, discharging cooling, obtains epoxy-modified graphene；
(3) above-mentioned epoxy-modified graphene is taken, is added in amination polyester emulsion, stirs evenly, it is small that 2 are stirred at 30 DEG C
When, increasing temperature is 180 DEG C, dimethylformamide is added, insulated and stirred 140 minutes, uniform coating on a glass, was sent into
13 hours dry at 75 DEG C in baking oven, discharging cooling takes off film to get the epoxy-modified graphene film.
Embodiment 2
A kind of epoxy-modified graphene film, it is composed of the following raw materials by weight:
Lithium methoxide 0.07, epoxy prapanol 10, methyl methacrylate 25, graphene oxide 100, amination polyester emulsion 46,
Hexabromocyclododecane 2.
A kind of epoxy-modified graphene film, the preparation method of the amination polyester emulsion, including following step
It is rapid:
(1) ammonium persulfate for taking 1 parts by weight is added in the deionized water of 30 times of its weight, stirs evenly；
(2) methyl acrylate of 30 parts by weight, the butyl acrylate mixing of 10 parts by weight are taken, above-mentioned mixture weight is added to
It in the deionized water of 6 times of amount, stirs evenly, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is 65 DEG C, is added
The diethylenetriamine of above-mentioned ammonium persulfate aqueous solution, 4 parts by weight, insulated and stirred 4 hours, discharging it is cooling to get.
The preparation method of the epoxy-modified graphene film, comprising the following steps:
(1) hexabromocyclododecane is taken, is added in the dehydrated alcohol of 20 times of its weight, stirs evenly, graphite oxide is added
Alkene, increasing temperature is 55 DEG C, insulated and stirred 2 hours, ethyl alcohol is distilled off, obtains activated graphene；
(2) methyl methacrylate, epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen, is adjusted anti-
Answering kettle temperature degree is 90 DEG C, is stirred to react 1 hour, and lithium methoxide, activated graphene is added, and adjusting temperature of reaction kettle is 150 DEG C, heat preservation
Stirring 3 hours, discharging cooling, obtains epoxy-modified graphene；
(3) above-mentioned epoxy-modified graphene is taken, is added in amination polyester emulsion, stirs evenly, it is small that 1 is stirred at 25 DEG C
When, increasing temperature is 160 DEG C, dimethylformamide is added, insulated and stirred 100 minutes, uniform coating on a glass, was sent into
10 hours dry at 70 DEG C in baking oven, discharging cooling takes off film to get the epoxy-modified graphene film.
Performance test:
Conductivity is 175.8-184.7Scm-1；
Epoxy-modified graphene film of the invention is adhered in glass fiber filter paper, is bent, bending angle is
150 °, bending 30000 times not broken.
Claims (3)
1. a kind of epoxy-modified graphene film, which is characterized in that it is composed of the following raw materials by weight:
Lithium methoxide 0.07-0.1, epoxy prapanol 10-13, methyl methacrylate 25-30, graphene oxide 100-110, amination are poly-
Ester lotion 46-50, hexabromocyclododecane 2-3.
2. a kind of epoxy-modified graphene film according to claim 1, which is characterized in that the amination polyester emulsion
Preparation method, comprising the following steps:
(1) ammonium persulfate for taking 1-2 parts by weight is added in the deionized water of 30-40 times of its weight, stirs evenly；
(2) methyl acrylate of 30-40 parts by weight, the butyl acrylate mixing of 10-15 parts by weight are taken, above-mentioned mixture is added to
It in 6-9 times of weight of deionized water, stirs evenly, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is 65-70
DEG C, the diethylenetriamine of above-mentioned ammonium persulfate aqueous solution, 4-5 parts by weight is added, insulated and stirred 4-6 hours, discharging cooled down, i.e.,
?.
3. a kind of preparation method of epoxy-modified graphene film as described in claim 1, which is characterized in that including following step
It is rapid:
(1) hexabromocyclododecane is taken, is added in the dehydrated alcohol of 20-24 times of its weight, stirs evenly, graphite oxide is added
Alkene, increasing temperature is 55-60 DEG C, insulated and stirred 2-3 hours, ethyl alcohol is distilled off, obtains activated graphene；
(2) methyl methacrylate, epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen, adjust reaction kettle
Temperature is 90-105 DEG C, is stirred to react 1-2 hours, and lithium methoxide, activated graphene is added, and adjusting temperature of reaction kettle is 150-160
DEG C, insulated and stirred 3-4 hours, discharging cooling obtained epoxy-modified graphene；
(3) above-mentioned epoxy-modified graphene is taken, is added in amination polyester emulsion, stirs evenly, stirs 1-2 at 25-30 DEG C
Hour, increasing temperature is 160-180 DEG C, and dimethylformamide is added, insulated and stirred 100-140 minutes, is uniformly coated in glass
It in glass plate, is sent into baking oven, 10-13 hours dry at 70-75 DEG C, discharging cooling takes off film to get the epoxy-modified graphite
Alkene film.
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| CN201810682243.6A CN108948622A (en) | 2018-06-28 | 2018-06-28 | A kind of epoxy-modified graphene film and preparation method thereof |
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| CN201810682243.6A CN108948622A (en) | 2018-06-28 | 2018-06-28 | A kind of epoxy-modified graphene film and preparation method thereof |
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Cited By (3)
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| CN110467784A (en) * | 2019-07-30 | 2019-11-19 | 安徽中科光电色选机械有限公司 | A kind of color selector sheath material and preparation method thereof |
| CN112898587A (en) * | 2021-01-22 | 2021-06-04 | 深圳市华创汇能技术有限公司 | Graphene grafted modified hyperbranched polyimide dielectric material and preparation method thereof |
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| CN112898587A (en) * | 2021-01-22 | 2021-06-04 | 深圳市华创汇能技术有限公司 | Graphene grafted modified hyperbranched polyimide dielectric material and preparation method thereof |
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