CN108424618B - Graphene/epoxy resin composite material and preparation method thereof - Google Patents
Graphene/epoxy resin composite material and preparation method thereof Download PDFInfo
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- CN108424618B CN108424618B CN201810225103.6A CN201810225103A CN108424618B CN 108424618 B CN108424618 B CN 108424618B CN 201810225103 A CN201810225103 A CN 201810225103A CN 108424618 B CN108424618 B CN 108424618B
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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
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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Abstract
The invention discloses a graphene/epoxy resin composite material which comprises the following components in parts by weight: 300 parts of bisphenol A type liquid epoxy resin, 0.3-43.5 parts of graphene microchip, 0.96-200.7 parts of bisphenol A and 0.2-0.3 part of catalyst, wherein the epoxy equivalent of the bisphenol A type liquid epoxy resin is 171-. The preparation method comprises the steps of dispersing graphene in bisphenol A type liquid epoxy resin in advance, carrying out polymerization reaction on the graphene/bisphenol A type liquid epoxy resin and bisphenol A under the action of a catalyst, opening vacuum at 130 ℃ by utilizing chemical energy generated by the polymerization reaction, and carrying out redispersion and stripping on the graphene under the negative pressure condition, so that the graphene/epoxy resin composite material with uniform dispersion and excellent performance is prepared.
Description
Technical Field
The invention relates to the technical field of preparation of epoxy resin composite materials, in particular to a graphene/epoxy resin composite material and a preparation method thereof.
Background
Graphene is a novel two-dimensional planar composite material, and the special monoatomic layer of graphene determines that graphene has rich and novel physical properties. Researches show that the graphene has excellent electrical properties, mechanical properties and processability. The epoxy resin has a unique two-dimensional structure and a plurality of excellent properties, and has great application potential in the aspects of improving the thermal property, the electromagnetic property, the mechanical property and the like of EP (epoxy resin).
However, in the process of preparing the graphene/epoxy resin composite material, due to the size effect, an agglomeration phenomenon is easy to occur between the graphene, and the graphene is easy to disperse unevenly due to the high viscosity of the epoxy resin matrix, so that the performance and the application of the graphene/EP composite material are limited to a certain extent.
Disclosure of Invention
In order to solve the problems, the invention provides the graphene/epoxy resin composite material and the preparation method thereof, and the graphene is more uniformly dispersed in the matrix and has better performance.
The technical scheme adopted by the invention is as follows: the graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
0.3-43.5 parts of graphene nanoplatelets;
0.96-200.7 parts of bisphenol A;
0.2-0.3 part of catalyst;
wherein the catalyst is triphenylphosphine and derivatives thereof, the molecular weight range of the prepared graphene/epoxy resin composite material is 345-20000, and the content of the graphene is 0.1-8%.
The bisphenol A type liquid epoxy resin has an epoxy equivalent of 171-244.
Preferably, the graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
0.32 part of graphene nanoplatelets;
1.0 part of bisphenol A;
0.2 part of catalyst;
wherein, the epoxy equivalent of the bisphenol A type liquid epoxy resin is 171, the catalyst is triphenylphosphine and derivatives thereof, the molecular weight of the prepared graphene/epoxy resin composite material is 345, and the graphene content is 0.1%.
Preferably, the graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
30 parts of graphene nanoplatelets;
98 parts of bisphenol A;
0.2 part of catalyst;
wherein, the epoxy equivalent of the bisphenol A liquid epoxy resin is 184, the catalyst is triphenylphosphine and derivatives thereof, the molecular weight of the prepared graphene/epoxy resin composite material is 910, and the graphene content is 7%.
Preferably, the graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
32 parts of graphene nanoplatelets;
151.2 parts of bisphenol A;
0.25 part of catalyst;
wherein, the epoxy equivalent of the bisphenol A liquid epoxy resin is 184, the catalyst is triphenylphosphine and derivatives thereof, the molecular weight of the prepared graphene/epoxy resin composite material is 3000, and the graphene content is 6.60%.
The preparation method of the graphene/epoxy resin composite material comprises the following steps:
(1) adding the low molecular weight bisphenol A type liquid epoxy resin with the formula amount into a reaction kettle, starting a stirrer for stirring, and starting steam to heat to 40 ℃;
(2) adding the graphene nanoplatelets with the formula amount under the low-speed stirring of 20-30 r/min, heating to 80 ℃ after adding, increasing the rotating speed to 150 r/min at the temperature, and quickly stirring for 40 min;
(3) adjusting the stirring speed to 20-30 r/min, adding bisphenol A with the formula amount, stirring and melting at 80 ℃ for 30min, adding catalyst with the formula amount, slowly increasing the rotating speed to 150 r/min, heating to 120 ℃, closing steam, and allowing the steam to automatically heat by virtue of reaction heat;
(4) and when the temperature reaches 130 ℃, opening a vacuum pump to ensure that the vacuum degree is gradually increased from 0 to more than-0.095 MP, keeping the temperature between 130 and 200 ℃ for reaction for 60min, closing the vacuum pump, filling high-purity nitrogen, discharging and dishing, and cooling to room temperature to obtain the graphene/epoxy resin composite material. The vacuum is opened from 130 ℃ to carry out negative pressure reaction, so that the produced graphene/epoxy resin composite material has narrower molecular weight distribution range, the graphene is more uniformly dispersed in the composite material, the resin color is lighter after the graphene is dissolved, filtered and removed, the consumption of the produced graphene/epoxy resin composite material with various contents in various anticorrosive coatings, powder coatings, fireproof coatings, conductive coatings, pouring sealants and adhesives can be reduced by more than 10%, the economic benefit is obviously improved, and the performance is more excellent.
The invention has the beneficial effects that: 1. by adopting the method, the graphene/epoxy resin composite material with the molecular weight range of 345-20000 can be prepared. 2. In the preparation process, vacuum is opened from 130 ℃ to carry out negative pressure reaction, so that the produced graphene/epoxy resin composite material is narrower in molecular weight distribution range, the graphene is more uniformly dispersed in the composite material, the resin color is lighter after the graphene is dissolved, filtered and removed, the use amount of the produced graphene/epoxy resin composite material with various contents in various anticorrosive coatings, powder coatings, fireproof coatings, conductive coatings, pouring sealants and adhesives can be reduced by more than 10%, the economic benefit is obviously improved, and the performance is more excellent.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the present invention.
Example 1
The graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
0.32 part of graphene nanoplatelets;
1.0 part of bisphenol A;
0.2 part of catalyst;
wherein the bisphenol A type liquid epoxy resin has an epoxy equivalent of 171.
The preparation method of the graphene/epoxy resin composite material comprises the following steps:
(1) adding 300 parts by weight of bisphenol A type liquid epoxy resin into a reaction kettle, starting a stirrer for stirring, and starting steam to heat to 40 ℃;
(2) 0.32 weight part of graphene nanoplatelets are added under the low-speed stirring of 20-30 r/min, the temperature is raised to 80 ℃ after the adding is finished, and the graphene nanoplatelets are quickly stirred for 40min at the temperature;
(3) adjusting the stirring speed to 20-30 r/min, adding 1.0 part by weight of bisphenol A, stirring and melting at 80 ℃ for 30min, adding 0.2 part by weight of catalyst, slowly increasing the speed to 150 r/min, heating to 120 ℃, closing steam, and allowing the steam to automatically heat by virtue of reaction heat;
(4) and when the temperature reaches 130 ℃, opening a vacuum pump to gradually increase the negative pressure from 0 to above 0.095MP, keeping the temperature between 130 and 200 ℃ for reaction for 60min, closing the vacuum pump, filling high-purity nitrogen, and discharging to obtain the graphene epoxy resin composite material. The technical indexes are as follows: the graphene/epoxy resin contains 0.1% of graphene, and the molecular weight of the graphene/epoxy resin is 345.
Example 2
The graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
30 parts of graphene nanoplatelets;
98 parts of bisphenol A;
0.2 part of catalyst;
wherein the bisphenol A type liquid epoxy resin has an epoxy equivalent of 184.
The preparation process is the same as that of example 1, and the technical indexes are as follows: the graphene/epoxy resin contains 7.0% of graphene, and has a molecular weight of 910, and electron microscope tests show that the graphene is uniformly dispersed.
Example 3
The graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
30 parts of graphene nanoplatelets;
98 parts of bisphenol A;
0.2 part of catalyst;
wherein the bisphenol A type liquid epoxy resin has an epoxy equivalent of 184.
The preparation process differs from example 1 in that the negative pressure reaction is carried out by starting from 160 ℃ under vacuum. The technical indexes are as follows: the graphene/epoxy resin contains 7.0% of graphene, and has a molecular weight of 940. an electron microscope comparative test shows that the dispersion uniformity of graphene is inferior to that of example 2, and the molecular weight distribution range of the epoxy resin tested by a GPC method is obviously wider than that of example 2.
Example 4
The graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
32 parts of graphene nanoplatelets;
151.2 parts of bisphenol A;
0.25 part of catalyst;
wherein the bisphenol A type liquid epoxy resin has an epoxy equivalent of 184.
The preparation process is the same as that of example 1, and the technical indexes are as follows: the graphene/epoxy resin contains 6.60% of graphene and has a molecular weight of 3000, and electron microscope tests show that the graphene is uniformly dispersed.
Example 5
The graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
60 parts of graphene nanoplatelets;
98 parts of bisphenol A;
0.2 part of catalyst;
wherein the bisphenol A type liquid epoxy resin has an epoxy equivalent of 184.
The preparation process is the same as that of example 1, and the technical indexes are as follows: the graphene/epoxy resin contains 13.09% of graphene and has a molecular weight of 912, and electron microscope tests show that the graphene is stacked and is unevenly dispersed.
Example 6
The graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
20 parts of graphene nanoplatelets;
98 parts of bisphenol A;
0.2 part of catalyst;
wherein the bisphenol A type liquid epoxy resin has an epoxy equivalent of 190.
The preparation process differs from example 1 in that: carrying out negative pressure dispersion stripping without opening vacuum from 130 ℃, and having the following technical indexes: the graphene/epoxy resin contains 4.78% of graphene, the molecular weight is 1000, and electron microscope tests show that the graphene is not uniformly dispersed and is locally accumulated and agglomerated.
Example 7
The graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
22 parts of graphene nanoplatelets;
58.5 parts of bisphenol A;
0.2 part of catalyst;
wherein the bisphenol A type liquid epoxy resin has an epoxy equivalent of 260.
The preparation process is the same as that of example 1, and the technical indexes are as follows: the graphene/epoxy resin contains 5.76% of graphene, and has a molecular weight of 1120, and an electron microscope test shows that the graphene has a slight agglomeration phenomenon.
Example 8
The graphene/epoxy resin composite material comprises the following components in parts by weight:
300 parts of bisphenol A type solid epoxy resin;
12 parts of graphene nanoplatelets;
10 parts of bisphenol A;
0.2 part of catalyst;
wherein the bisphenol A type solid epoxy resin has an epoxy equivalent of 500.
The preparation method of the graphene/epoxy resin composite material comprises the following steps:
(1) adding 300 parts by weight of solid epoxy resin into a reaction kettle, starting steam, heating to 40 ℃ until the epoxy resin is not melted, and continuously heating to 95 ℃ for melting;
(2) and (3) putting the graphene under low-speed stirring at 20-30 r/min, and finding that a large amount of graphene overflows out of the kettle, so that the operation cannot be performed and the experiment fails.
In order to prepare graphene/EP composite materials with uniform dispersion and excellent performance, various preparation methods such as in-situ intercalation polymerization, solution intercalation, melt intercalation and the like have been explored, but the present invention is different from the above preparation methods, and is characterized in that functionalized graphene is dispersed in low molecular weight bisphenol a type liquid epoxy resin in advance, the graphene/bisphenol a type liquid epoxy resin and bisphenol a are subjected to polymerization reaction under the action of a catalyst, and the chemical energy generated by the polymerization reaction is utilized to redisperse and strip the graphene under the negative pressure condition, (i.e. the graphene is redispersed and stripped while the polymerization reaction is carried out under the negative pressure condition), so as to prepare various graphene/epoxy resin composite materials with uniform dispersion and excellent performance. The graphene/epoxy resin composite material with the graphene content as high as 2% and the epoxy equivalent of 800 is used for preparing powder coating with 20% of zinc content, and the salt spray resistance time is more than 2000 h. The graphene composite material is characterized by SEM and the like, and the result shows that the graphene is completely stripped and uniformly dispersed in the matrix, the interface compatibility of the graphene and the matrix is good, and the thermal stability of the composite material is improved. And simultaneously, the thermal stability of the glass transition temperature of EB is improved.
Claims (6)
1. The graphene/epoxy resin composite material is characterized by comprising the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
0.3-43.5 parts of graphene nanoplatelets;
0.96-200.7 parts of bisphenol A;
0.2-0.3 part of catalyst;
wherein the catalyst is triphenylphosphine and derivatives thereof, the molecular weight range of the prepared graphene/epoxy resin composite material is 345-20000, and the content of the graphene is 0.1-8%;
the preparation method of the graphene/epoxy resin composite material comprises the following steps:
(1) adding the low molecular weight bisphenol A type liquid epoxy resin with the formula amount into a reaction kettle, starting a stirrer for stirring, and starting steam to heat to 40 ℃;
(2) adding the graphene nanoplatelets with the formula amount under the low-speed stirring of 20-30 r/min, heating to 80 ℃ after adding, increasing the rotating speed to 150 r/min at the temperature, and quickly stirring for 40 min;
(3) adjusting the stirring speed to 20-30 r/min, adding bisphenol A with the formula amount, stirring and melting at 80 ℃ for 30min, adding catalyst with the formula amount, slowly increasing the rotating speed to 150 r/min, heating to 120 ℃, closing steam, and allowing the steam to automatically heat by virtue of reaction heat;
(4) and when the temperature reaches 130 ℃, opening a vacuum pump to ensure that the vacuum degree is gradually increased from 0 to more than-0.095 MPa, keeping the temperature between 130 and 200 ℃ for reaction for 60min, closing the vacuum pump, filling high-purity nitrogen, discharging and dishing, and cooling to room temperature to obtain the graphene/epoxy resin composite material.
2. The graphene/epoxy resin composite material according to claim 1, wherein the epoxy equivalent of the bisphenol A type liquid epoxy resin is 171-244.
3. The graphene/epoxy resin composite material according to claim 1, comprising the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
0.32 part of graphene nanoplatelets;
1.0 part of bisphenol A;
0.2 part of catalyst;
wherein, the epoxy equivalent of the bisphenol A type liquid epoxy resin is 171, the catalyst is triphenylphosphine and derivatives thereof, the molecular weight of the prepared graphene/epoxy resin composite material is 345, and the graphene content is 0.1%.
4. The graphene/epoxy resin composite material according to claim 1, comprising the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
30 parts of graphene nanoplatelets;
98 parts of bisphenol A;
0.2 part of catalyst;
wherein, the epoxy equivalent of the bisphenol A liquid epoxy resin is 184, the catalyst is triphenylphosphine and derivatives thereof, the molecular weight of the prepared graphene/epoxy resin composite material is 910, and the graphene content is 7%.
5. The graphene/epoxy resin composite material according to claim 1, comprising the following components in parts by weight:
300 parts of bisphenol A type liquid epoxy resin;
32 parts of graphene nanoplatelets;
151.2 parts of bisphenol A;
0.25 part of catalyst;
wherein, the epoxy equivalent of the bisphenol A liquid epoxy resin is 184, the catalyst is triphenylphosphine and derivatives thereof, the molecular weight of the prepared graphene/epoxy resin composite material is 3000, and the graphene content is 6.60%.
6. The preparation method of the graphene/epoxy resin composite material according to claim 1, comprising the following steps:
(1) adding the low molecular weight bisphenol A type liquid epoxy resin with the formula amount into a reaction kettle, starting a stirrer for stirring, and starting steam to heat to 40 ℃;
(2) adding the graphene nanoplatelets with the formula amount under the low-speed stirring of 20-30 r/min, heating to 80 ℃ after adding, increasing the rotating speed to 150 r/min at the temperature, and quickly stirring for 40 min;
(3) adjusting the stirring speed to 20-30 r/min, adding bisphenol A with the formula amount, stirring and melting at 80 ℃ for 30min, adding catalyst with the formula amount, slowly increasing the rotating speed to 150 r/min, heating to 120 ℃, closing steam, and allowing the steam to automatically heat by virtue of reaction heat;
(4) and when the temperature reaches 130 ℃, opening a vacuum pump to ensure that the vacuum degree is gradually increased from 0 to more than-0.095 MPa, keeping the temperature between 130 and 200 ℃ for reaction for 60min, closing the vacuum pump, filling high-purity nitrogen, discharging and dishing, and cooling to room temperature to obtain the graphene/epoxy resin composite material.
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| CN102516512A (en) * | 2011-11-23 | 2012-06-27 | 安徽神剑新材料股份有限公司 | Preparation method of 70/30 high-Tg mixed type polyester resin |
| CN103627139A (en) * | 2013-09-25 | 2014-03-12 | 杭州师范大学 | Preparation method of functionalized graphene oxide/epoxy resin nanocomposite |
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| US9951436B2 (en) * | 2011-10-27 | 2018-04-24 | Garmor Inc. | Composite graphene structures |
| JP6199889B2 (en) * | 2011-12-20 | 2017-09-20 | ダウ グローバル テクノロジーズ エルエルシー | Epoxy resin composite material |
| WO2015171429A1 (en) * | 2014-05-07 | 2015-11-12 | Wichita State University | Nanocomposite microcapsules for self-healing of composite articles |
| CN107353587A (en) * | 2017-06-21 | 2017-11-17 | 江苏兴盛化工有限公司 | High concentration graphene/epoxy resin composite material and preparation method thereof |
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| CN102516512A (en) * | 2011-11-23 | 2012-06-27 | 安徽神剑新材料股份有限公司 | Preparation method of 70/30 high-Tg mixed type polyester resin |
| CN103627139A (en) * | 2013-09-25 | 2014-03-12 | 杭州师范大学 | Preparation method of functionalized graphene oxide/epoxy resin nanocomposite |
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