CN112094481A - Preparation method of graphene/carbon nanotube/epoxy resin composite material - Google Patents
Preparation method of graphene/carbon nanotube/epoxy resin composite material Download PDFInfo
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- CN112094481A CN112094481A CN202011000378.3A CN202011000378A CN112094481A CN 112094481 A CN112094481 A CN 112094481A CN 202011000378 A CN202011000378 A CN 202011000378A CN 112094481 A CN112094481 A CN 112094481A
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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
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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/0083—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive non-fibrous particles embedded in an electrically insulating supporting structure, e.g. powder, flakes, whiskers
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Abstract
A preparation method of a graphene/carbon nano tube/epoxy resin composite material relates to a preparation method of an epoxy resin composite material. The invention aims to solve the problem of poor mechanical property of the existing epoxy resin. The method comprises the following steps: firstly, preparing graphene; secondly, preparing graphene/carbon nano tube mixed powder; and thirdly, mixing and curing. According to the invention, the graphene/carbon nano tube/epoxy resin composite material is prepared by taking the graphene and the carbon nano tube as fillers, and the tensile strength of the prepared graphene/carbon nano tube/epoxy resin composite material can reach 85.37 MPa. The graphene/carbon nanotube/epoxy resin composite material can be obtained.
Description
Technical Field
The invention relates to a preparation method of an epoxy resin composite material.
Background
Epoxy resin is excellent thermosetting resin, has more excellent physical property, electrical insulation property, chemical resistance, heat resistance and adhesion property compared with unsaturated polyester resin which is widely applied at present, and is the most common and important matrix material and structural material at present.
However, epoxy materials can also be damaged during use. Since epoxy is a thermosetting material, once the epoxy material is damaged, it cannot be repaired by a heated reshaping method as with thermoplastics.
Therefore, the epoxy resin is modified to improve its mechanical properties.
Disclosure of Invention
The invention aims to solve the problem of poor mechanical property of the existing epoxy resin, and provides a preparation method of a graphene/carbon nano tube/epoxy resin composite material.
The preparation method of the graphene/carbon nanotube/epoxy resin composite material is completed according to the following steps:
firstly, preparing graphene:
firstly, adding graphite into concentrated sulfuric acid with the mass fraction of 98% under the stirring condition, and then adding NaNO3Mechanically stirring for 1-3 h at room temperature, and adding KMnO under stirring4Continuing mechanically stirring at room temperature for 70-80 h, stopping stirring, adding deionized water, dripping 30% hydrogen peroxide until the solution turns yellow from brown red, and finally drying at 70 ℃ to obtain graphene oxide;
the volume ratio of the mass of the graphite to the mass fraction of 98% concentrated sulfuric acid in the first step is (1 g-3 g) 250 mL;
NaNO described in step one3The volume ratio of the mass of the concentrated sulfuric acid with the mass fraction of 98 percent is (4 g-6 g) 250 mL;
KMnO described in step one4The volume ratio of the concentrated sulfuric acid with the mass fraction of 98 percent (8 g-12 g) is 250 mL;
the volume ratio of the mass of the deionized water to the mass fraction of 98% concentrated sulfuric acid in the first step is (100-200 g) 250;
secondly, putting the graphene oxide obtained in the first step into a muffle furnace at 1000-1050 ℃ for heat treatment for 10-15 s to obtain graphene;
secondly, preparing graphene/carbon nanotube mixed powder:
mixing graphene and carbon nanotube powder, and then carrying out differential mixing ball milling under the protection of argon gas to obtain mixed powder; the mass of the carbon nanotube powder is 20-30% of the total mass of the mixed powder;
the differential speed mixing ball milling process comprises the following steps: firstly, ball milling is carried out for 2 h-3 h clockwise under the condition that the ball milling speed is 300 r/min-400 r/min, then ball milling is carried out for 2 h-3 h anticlockwise under the condition that the ball milling speed is 300 r/min-400 r/min, and differential speed mixing ball milling is completed, wherein the speed of the clockwise ball milling is greater than that of the anticlockwise ball milling;
mixing the epoxy resin and the mixed powder, standing for 13-16 h, stirring for 2-4 h, finally mixing the obtained mixed material with a curing agent at the temperature of 60-90 ℃, stirring for 7-10 h, and curing for 0.5-1 h at the temperature of 100-150 ℃ to obtain the epoxy resin-based electromagnetic shielding nanocomposite;
the mass ratio of the epoxy resin to the mixed powder in the third step is (48-60) to (15-20);
the mass ratio of the epoxy resin to the curing agent in the third step is (48-60) to (2-6).
The principle and the advantages of the invention are as follows:
the graphene is paid much attention to the scientific community by virtue of excellent mechanical properties, thermal properties, electrochemical properties and the like, and particularly, the graphene has very high mechanical properties, so that the mechanical properties of a polymer material can be greatly improved if the graphene is added into a polymer matrix as a filling material;
secondly, the graphene/carbon nano tube/epoxy resin composite material is prepared by taking the graphene and the carbon nano tube as fillers, and the tensile strength of the prepared graphene/carbon nano tube/epoxy resin composite material can reach 85.37 MPa.
The graphene/carbon nanotube/epoxy resin composite material can be obtained.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a graphene/carbon nanotube/epoxy resin composite material, which is completed according to the following steps:
firstly, preparing graphene:
firstly, adding graphite into concentrated sulfuric acid with the mass fraction of 98% under the stirring condition, and then adding NaNO3Mechanically stirring for 1-3 h at room temperature, and adding KMnO under stirring4Continuing mechanically stirring at room temperature for 70-80 h, stopping stirring, adding deionized water, dripping 30% hydrogen peroxide until the solution turns yellow from brown red, and finally drying at 70 ℃ to obtain graphene oxide;
the volume ratio of the mass of the graphite to the mass fraction of 98% concentrated sulfuric acid in the first step is (1 g-3 g) 250 mL;
NaNO described in step one3The volume ratio of the mass of the concentrated sulfuric acid with the mass fraction of 98 percent is (4 g-6 g) 250 mL;
KMnO described in step one4The volume ratio of the concentrated sulfuric acid with the mass fraction of 98 percent (8 g-12 g) is 250 mL;
the volume ratio of the mass of the deionized water to the mass fraction of 98% concentrated sulfuric acid in the first step is (100-200 g) 250;
secondly, putting the graphene oxide obtained in the first step into a muffle furnace at 1000-1050 ℃ for heat treatment for 10-15 s to obtain graphene;
secondly, preparing graphene/carbon nanotube mixed powder:
mixing graphene and carbon nanotube powder, and then carrying out differential mixing ball milling under the protection of argon gas to obtain mixed powder; the mass of the carbon nanotube powder is 20-30% of the total mass of the mixed powder;
the differential speed mixing ball milling process comprises the following steps: firstly, ball milling is carried out for 2 h-3 h clockwise under the condition that the ball milling speed is 300 r/min-400 r/min, then ball milling is carried out for 2 h-3 h anticlockwise under the condition that the ball milling speed is 300 r/min-400 r/min, and differential speed mixing ball milling is completed, wherein the speed of the clockwise ball milling is greater than that of the anticlockwise ball milling;
mixing the epoxy resin and the mixed powder, standing for 13-16 h, stirring for 2-4 h, finally mixing the obtained mixed material with a curing agent at the temperature of 60-90 ℃, stirring for 7-10 h, and curing for 0.5-1 h at the temperature of 100-150 ℃ to obtain the epoxy resin-based electromagnetic shielding nanocomposite;
the mass ratio of the epoxy resin to the mixed powder in the third step is (48-60) to (15-20);
the mass ratio of the epoxy resin to the curing agent in the third step is (48-60) to (2-6).
The principle and advantages of the embodiment are as follows:
the graphene is paid much attention to the scientific community by virtue of excellent mechanical properties, thermal properties, electrochemical properties and the like, and particularly, the graphene has very high mechanical properties, so that the mechanical properties of a polymer material can be greatly improved if the graphene is added into a polymer matrix as a filling material;
secondly, in the embodiment, the graphene/carbon nanotube/epoxy resin composite material is prepared by taking the graphene and the carbon nanotube as fillers, and the tensile strength of the prepared graphene/carbon nanotube/epoxy resin composite material can reach 85.37 MPa.
The graphene/carbon nanotube/epoxy resin composite material can be obtained by the embodiment.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the mechanical stirring speed in the first step is 500 r/min-1000 r/min. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the volume ratio of the mass of the graphite to the mass fraction of 98% concentrated sulfuric acid in the first step is 2g:250 mL; NaNO described in step one3The volume ratio of the mass of the concentrated sulfuric acid to the mass fraction of 98 percent is 5g:250 mL; KMnO described in step one4Is 98% by mass or mass fractionThe volume ratio of concentrated sulfuric acid is 10g:250 mL; the volume ratio of the mass of the deionized water to the mass fraction of 98% concentrated sulfuric acid in the first step is 150g: 250. The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: and in the first step, the graphene oxide obtained in the first step is put into a muffle furnace at 1030-1050 ℃ for heat treatment for 13-15 s to obtain the graphene. The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the differential speed mixing ball milling process in the step two comprises the following steps: firstly, ball milling is carried out for 2.5h clockwise under the condition that the ball milling speed is 400r/min, then ball milling is carried out for 2.5h anticlockwise under the condition that the ball milling speed is 400r/min, and differential mixing ball milling is completed, wherein the speed of the clockwise ball milling is greater than that of the anticlockwise ball milling. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the length of the carbon nano tube in the second step is 20-40 μm, and the diameter is 40-50 nm. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the epoxy resin in the third step is bisphenol F epoxy resin. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: the curing agent in the third step is 2-methylimidazole. The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: and in the third step, the epoxy resin and the mixed powder are mixed and then stand for 14 to 16 hours, then are stirred for 3 to 4 hours, finally the obtained mixed material is mixed with a curing agent at the temperature of between 80 and 90 ℃, are stirred for 9 to 10 hours, and are cured for 0.8 to 1 hour at the temperature of between 130 and 140 ℃, so as to obtain the epoxy resin-based electromagnetic shielding nano composite material. The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: the mass ratio of the epoxy resin to the mixed powder in the third step is (50-60): 15; the mass ratio of the epoxy resin to the curing agent in the third step is (50-60): 4. The other steps are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows: the preparation method of the graphene/carbon nanotube/epoxy resin composite material is completed according to the following steps:
firstly, preparing graphene:
firstly, adding graphite into concentrated sulfuric acid with the mass fraction of 98% under the stirring condition, and then adding NaNO3Mechanically stirring at room temperature for 2h, and adding KMnO under stirring4Continuing mechanically stirring for 75 hours at room temperature, stopping stirring, adding deionized water, dripping 30% hydrogen peroxide by mass until the solution turns yellow from brownish red, and finally drying at 70 ℃ to obtain graphene oxide;
the speed of mechanical stirring in the first step is 500 r/min;
the volume ratio of the mass of the graphite to the mass fraction of 98% concentrated sulfuric acid in the first step is 2g:250 mL;
NaNO described in step one3The volume ratio of the mass of the concentrated sulfuric acid to the mass fraction of 98 percent is 5g:250 mL;
KMnO described in step one4The volume ratio of the mass of the concentrated sulfuric acid to the mass fraction of 98 percent is 10g:250 mL;
the volume ratio of the mass of the deionized water to the mass fraction of 98% concentrated sulfuric acid in the first step is 150g: 250;
secondly, putting the graphene oxide obtained in the first step into a muffle furnace at 1030 ℃ for heat treatment for 13s to obtain graphene;
secondly, preparing graphene/carbon nanotube mixed powder:
mixing graphene and carbon nanotube powder, and then carrying out differential mixing ball milling under the protection of argon gas to obtain mixed powder; the mass of the carbon nanotube powder is 25% of the total mass of the mixed powder;
the differential speed mixing ball milling process comprises the following steps: firstly, ball-milling clockwise for 2.5h under the condition that the ball-milling speed is 400r/min, then ball-milling anticlockwise for 2.5h under the condition that the ball-milling speed is 400r/min, and completing differential mixing ball-milling, wherein the speed of the clockwise ball-milling is greater than that of the anticlockwise ball-milling;
the length of the carbon nano tube in the second step is 20-40 μm, and the diameter is 40-50 nm;
thirdly, mixing the epoxy resin and the mixed powder, standing for 14 hours, stirring for 3 hours, finally mixing the obtained mixed material with a curing agent at the temperature of 80 ℃, stirring for 9 hours, and curing for 0.8 hour at the temperature of 130 ℃ to obtain the epoxy resin-based electromagnetic shielding nano composite material;
the epoxy resin in the third step is bisphenol F epoxy resin;
the curing agent in the third step is 2-methylimidazole;
the mass ratio of the epoxy resin to the mixed powder in the third step is 50: 15;
the mass ratio of the epoxy resin to the curing agent in the third step is 50: 4.
In the embodiment, the tensile strength of the graphene/carbon nanotube/epoxy resin composite material prepared in the first embodiment can reach 85.37 MPa.
Claims (10)
1. A preparation method of a graphene/carbon nanotube/epoxy resin composite material is characterized in that the preparation method of the graphene/carbon nanotube/epoxy resin composite material is completed according to the following steps:
firstly, preparing graphene:
firstly, adding graphite into concentrated sulfuric acid with the mass fraction of 98% under the stirring condition, and then adding NaNO3Mechanically stirring for 1-3 h at room temperature, and adding KMnO under stirring4Continuously mechanically stirring for 70-80 h at room temperature, stopping stirring, and adding deionized waterAdding water, then dropping hydrogen peroxide with the mass fraction of 30% until the solution turns yellow from brownish red, and finally drying at 70 ℃ to obtain graphene oxide;
the volume ratio of the mass of the graphite to the mass fraction of 98% concentrated sulfuric acid in the first step is (1 g-3 g) 250 mL;
NaNO described in step one3The volume ratio of the mass of the concentrated sulfuric acid with the mass fraction of 98 percent is (4 g-6 g) 250 mL;
KMnO described in step one4The volume ratio of the concentrated sulfuric acid with the mass fraction of 98 percent (8 g-12 g) is 250 mL;
the volume ratio of the mass of the deionized water to the mass fraction of 98% concentrated sulfuric acid in the first step is (100-200 g) 250;
secondly, putting the graphene oxide obtained in the first step into a muffle furnace at 1000-1050 ℃ for heat treatment for 10-15 s to obtain graphene;
secondly, preparing graphene/carbon nanotube mixed powder:
mixing graphene and carbon nanotube powder, and then carrying out differential mixing ball milling under the protection of argon gas to obtain mixed powder; the mass of the carbon nanotube powder is 20-30% of the total mass of the mixed powder;
the differential speed mixing ball milling process comprises the following steps: firstly, ball milling is carried out for 2 h-3 h clockwise under the condition that the ball milling speed is 300 r/min-400 r/min, then ball milling is carried out for 2 h-3 h anticlockwise under the condition that the ball milling speed is 300 r/min-400 r/min, and differential speed mixing ball milling is completed, wherein the speed of the clockwise ball milling is greater than that of the anticlockwise ball milling;
mixing the epoxy resin and the mixed powder, standing for 13-16 h, stirring for 2-4 h, finally mixing the obtained mixed material with a curing agent at the temperature of 60-90 ℃, stirring for 7-10 h, and curing for 0.5-1 h at the temperature of 100-150 ℃ to obtain the epoxy resin-based electromagnetic shielding nanocomposite;
the mass ratio of the epoxy resin to the mixed powder in the third step is (48-60) to (15-20);
the mass ratio of the epoxy resin to the curing agent in the third step is (48-60) to (2-6).
2. The method for preparing the graphene/carbon nanotube/epoxy resin composite material according to claim 1, wherein the mechanical stirring speed in the first step is 500r/min to 1000 r/min.
3. The preparation method of the graphene/carbon nanotube/epoxy resin composite material according to claim 1, wherein the volume ratio of the mass of the graphite to the mass fraction of 98% concentrated sulfuric acid in the first step is 2g:250 mL; NaNO described in step one3The volume ratio of the mass of the concentrated sulfuric acid to the mass fraction of 98 percent is 5g:250 mL; KMnO described in step one4The volume ratio of the mass of the concentrated sulfuric acid to the mass fraction of 98 percent is 10g:250 mL; the volume ratio of the mass of the deionized water to the mass fraction of 98% concentrated sulfuric acid in the first step is 150g: 250.
4. The preparation method of the graphene/carbon nanotube/epoxy resin composite material according to claim 1, wherein the graphene oxide obtained in the first step is placed in a muffle furnace at 1030-1050 ℃ for heat treatment for 13-15 s to obtain the graphene.
5. The method for preparing graphene/carbon nanotube/epoxy resin composite material according to claim 1, wherein the differential speed mixing ball milling process in the second step comprises: firstly, ball milling is carried out for 2.5h clockwise under the condition that the ball milling speed is 400r/min, then ball milling is carried out for 2.5h anticlockwise under the condition that the ball milling speed is 400r/min, and differential mixing ball milling is completed, wherein the speed of the clockwise ball milling is greater than that of the anticlockwise ball milling.
6. The method according to claim 1, wherein the carbon nanotubes in step two have a length of 20 μm to 40 μm and a diameter of 40nm to 50 nm.
7. The method according to claim 1, wherein the epoxy resin in step three is bisphenol F epoxy resin.
8. The method for preparing graphene/carbon nanotube/epoxy resin composite material according to claim 1, wherein the curing agent in step three is 2-methylimidazole.
9. The preparation method of the graphene/carbon nanotube/epoxy resin composite material according to claim 1, wherein the epoxy resin and the mixed powder are mixed and then are kept stand for 14 to 16 hours, then are stirred for 3 to 4 hours, finally the obtained mixed material is mixed with a curing agent at 80 to 90 ℃, and are stirred for 9 to 10 hours, and are cured for 0.8 to 1 hour at 130 to 140 ℃ to obtain the epoxy resin-based electromagnetic shielding nanocomposite material.
10. The preparation method of the graphene/carbon nanotube/epoxy resin composite material according to claim 1, wherein the mass ratio of the epoxy resin to the mixed powder in the step three is (50-60): 15; the mass ratio of the epoxy resin to the curing agent in the third step is (50-60): 4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113717583A (en) * | 2021-09-24 | 2021-11-30 | 肇庆市海特复合材料技术研究院 | Preparation method of blue-green heat-insulating refrigeration coating |
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Application publication date: 20201218 |