CN110964266A - Novel graphene aerogel material and preparation method thereof - Google Patents
Novel graphene aerogel material and preparation method thereof Download PDFInfo
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Abstract
The embodiment of the invention discloses a novel graphene aerogel material and a preparation method thereof, and particularly relates to the field of aerogel materials, which comprises 60-80 parts of graphene oxide, 20-40 parts of poly-4-methyl-1-pentene, 10-20 parts of polytetrafluoroethylene, 5-15 parts of resorcinol-formaldehyde adhesive, 40-60 parts of deionized water, 10-20 parts of polymethyl methacrylate, 10-20 parts of polycarbonate and 2-6 parts of catalyst, wherein the prepared graphene aerogel has good heat resistance and flame retardance in the using process, is suitable for being used at high temperature, has high finished product light transmittance, is more attractive in appearance, improves the water resistance of the graphene aerogel and prolongs the service life of the graphene aerogel, and meanwhile, the molded graphene aerogel has low shrinkage, so that the prepared graphene aerogel has good size stability.
Description
Technical Field
The embodiment of the invention relates to the field of aerogel materials, and particularly relates to a novel graphene aerogel material and a preparation method thereof.
Background
The aerogel is a porous foam-like fixing material, and has an extremely light density and a very high specific surface area, and due to its special porous structure, the aerogel is widely researched in catalytic substrates, absorption materials, conductive and insulating materials, and the like, and the graphene aerogel has characteristics of graphene and aerogel, including high porosity, ultra-light density, high mechanical strength, and good thermal and electrical conductivity, so that the graphene aerogel is widely applied in the fields of energy storage, catalysis, environmental protection, electronic devices, and the like.
When the existing graphene aerogel material is prepared, due to improper treatment of raw materials, the graphene aerogel material is poor in heat resistance and flame retardance in the using process, and the formed graphene aerogel is high in shrinkage rate, so that the prepared graphene aerogel is poor in size stability.
Disclosure of Invention
Therefore, the embodiment of the invention provides a novel graphene aerogel material and a preparation method thereof, and the prepared graphene aerogel has good heat resistance and flame retardance in the use process, is suitable for being used at high temperature, has high finished product light transmittance, is more attractive in appearance, improves the water resistance of the graphene aerogel, prolongs the service life of the graphene aerogel, improves the mechanical strength and the oxidation resistance of the graphene aerogel, and is low in shrinkage rate after molding, so that the prepared graphene aerogel is good in size stability, and the problem in the background art is solved.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions: the novel graphene aerogel material comprises the following main materials in parts by weight: 60-80 parts of graphene oxide, 20-40 parts of poly-4-methyl-1-pentene, 10-20 parts of polytetrafluoroethylene, 5-15 parts of resorcinol-formaldehyde adhesive, 40-60 parts of deionized water, 10-20 parts of polymethyl methacrylate, 10-20 parts of polycarbonate and 2-6 parts of catalyst.
Further, the used main materials comprise the following raw materials in parts by weight: 65-75 parts of graphene oxide, 25-35 parts of poly 4-methyl-1-pentene, 13-17 parts of polytetrafluoroethylene, 8-12 parts of resorcinol-formaldehyde adhesive, 45-55 parts of deionized water, 13-17 parts of polymethyl methacrylate, 13-17 parts of polycarbonate and 3-5 parts of catalyst.
Further, the used main materials comprise the following raw materials in parts by weight: 70 parts of graphene oxide, 30 parts of poly-4-methyl-1-pentene, 15 parts of polytetrafluoroethylene, 10 parts of resorcinol-formaldehyde adhesive, 50 parts of deionized water, 15 parts of polymethyl methacrylate, 15 parts of polycarbonate and 4 parts of catalyst.
Further, the catalyst is any one of hydrazine hydrate, lithium aluminum hydride, p-phenylenediamine, diethylenetriamine, triethylene tetramine and tetraethylene pentamine or a combination of two of the two.
A preparation method of a novel graphene aerogel material comprises the following specific operation steps:
firstly, crushing a proper amount of graphene oxide, pouring the crushed graphene oxide into a metal container after the treatment is finished, adding poly 4-methyl-1-pentene, polytetrafluoroethylene, a resorcinol-formaldehyde adhesive and deionized water into the metal container, and stirring for 1-2 hours to prepare a solution with the concentration of 1-10 mg/ml;
step two, heating the metal container with the solution prepared inside in warm water at 60 ℃ in a water bath, and vibrating for 2-4h by using an ultrasonic generator to obtain a graphene oxide aqueous solution;
step three, taking out a proper amount of polymethyl methacrylate and polycarbonate, mixing and stirring for 1h at the high temperature of 200-300 ℃, taking out and cooling to normal temperature for later use;
taking out the prepared graphene oxide aqueous solution, putting the graphene oxide aqueous solution into a reaction kettle, adding a catalyst, stirring for 20-30min, then adding a mixture of polymethyl methacrylate and polycarbonate into the reaction kettle, heating, and treating at the temperature of 100-300 ℃ for 2-6h to prepare graphene oxide hydrogel;
placing the prepared graphene oxide hydrogel in an acetone solution for solvent replacement to obtain a graphene oxide gel;
and step six, taking out the prepared graphene oxide hydrogel, naturally cooling for 2 hours at normal temperature, then putting the graphene oxide hydrogel into a refrigeration house at the temperature of minus 5 ℃, and freeze-drying the graphene oxide hydrogel, and taking out the graphene oxide hydrogel to obtain the high-strength graphene oxide aerogel.
Further, the metal container in the first step and the second step is a stainless steel member.
Further, the freeze drying time in the sixth step is 4-6h, and the obtained product is taken out and placed at normal temperature for 2 h.
The embodiment of the invention has the following advantages: the raw materials of the prepared graphene aerogel are easy to obtain, the preparation method is simple, and the prepared graphene aerogel has good heat resistance and flame retardance in the using process, is suitable for being used at high temperature, has high finished product light transmittance and is more attractive in appearance, wherein the water resistance of the graphene aerogel is improved and the service life of the graphene aerogel is prolonged due to the matching of the resorcinol-formaldehyde adhesive and other raw materials, the mechanical strength and the oxidation resistance of the graphene aerogel are improved, and meanwhile, the formed graphene aerogel is low in shrinkage rate, so that the prepared graphene aerogel is good in size stability and is suitable for popularization and use.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the novel graphene aerogel material of this embodiment, wherein the main material used comprises the following components: graphene oxide, poly-4-methyl-1-pentene, polytetrafluoroethylene, a resorcinol-formaldehyde adhesive, deionization, polymethyl methacrylate, polycarbonate and a catalyst;
specifically, the composition comprises the following components in parts by weight: 60 parts of graphene oxide, 20 parts of poly-4-methyl-1-pentene, 10 parts of polytetrafluoroethylene, 5 parts of resorcinol-formaldehyde adhesive, 40 parts of deionized water, 10 parts of polymethyl methacrylate, 10 parts of polycarbonate and 2 parts of catalyst.
Furthermore, the catalyst is any one or a combination of more than two of hydrazine hydrate, lithium aluminum hydride, p-phenylenediamine, diethylenetriamine, triethylene tetramine and tetraethylene pentamine.
A preparation method of a novel graphene aerogel material comprises the following specific operation steps:
firstly, crushing a proper amount of graphene oxide, pouring the crushed graphene oxide into a metal container after the treatment is finished, adding poly 4-methyl-1-pentene, polytetrafluoroethylene, a resorcinol-formaldehyde adhesive and deionized water into the metal container, and stirring for 1h to prepare a solution with the concentration of 1-10 mg/ml;
step two, heating the metal container with the solution prepared inside in warm water at 60 ℃ in a water bath, and vibrating for 2 hours by using an ultrasonic generator to obtain a graphene oxide aqueous solution;
step three, taking out a proper amount of polymethyl methacrylate and polycarbonate, mixing and stirring for 1h at the high temperature of 200-300 ℃, taking out and cooling to normal temperature for later use;
taking out the prepared graphene oxide aqueous solution, putting the graphene oxide aqueous solution into a reaction kettle, adding a catalyst, stirring for 20min, then putting a mixture of polymethyl methacrylate and polycarbonate into the reaction kettle, heating and treating at the temperature of 100 ℃ for 2-6h to prepare graphene oxide hydrogel;
placing the prepared graphene oxide hydrogel in an acetone solution for solvent replacement to obtain a graphene oxide gel;
and step six, taking out the prepared graphene oxide hydrogel, naturally cooling for 2 hours at normal temperature, then putting the graphene oxide hydrogel into a refrigeration house at the temperature of minus 5 ℃, and freeze-drying the graphene oxide hydrogel, and taking out the graphene oxide hydrogel to obtain the high-strength graphene oxide aerogel.
Furthermore, the metal container in the first step and the second step is a component made of stainless steel;
further, the freeze drying time in the sixth step is 4-6h, and the obtained product is taken out and placed at the normal temperature for 2 h.
Example 2:
the novel graphene aerogel material of this embodiment, wherein the main material used comprises the following components: graphene oxide, poly-4-methyl-1-pentene, polytetrafluoroethylene, a resorcinol-formaldehyde adhesive, deionized water, polymethyl methacrylate, polycarbonate and a catalyst;
specifically, the composition comprises the following components in parts by weight: 65 parts of graphene oxide, 25 parts of poly-4-methyl-1-pentene, 14 parts of polytetrafluoroethylene, 8 parts of resorcinol-formaldehyde adhesive, 45 parts of deionized water, 14 parts of polymethyl methacrylate, 14 parts of polycarbonate and 4 parts of catalyst.
Furthermore, the catalyst is any one or a combination of more than two of hydrazine hydrate, lithium aluminum hydride, p-phenylenediamine, diethylenetriamine, triethylene tetramine and tetraethylene pentamine.
A preparation method of a novel graphene aerogel material comprises the following specific operation steps:
firstly, crushing a proper amount of graphene oxide, pouring the crushed graphene oxide into a metal container after the treatment is finished, adding poly 4-methyl-1-pentene, polytetrafluoroethylene, a resorcinol-formaldehyde adhesive and deionized water into the metal container, and stirring for 1h to prepare a solution with the concentration of 1-10 mg/ml;
step two, heating the metal container with the solution prepared inside in warm water at 60 ℃ in a water bath, and vibrating for 3 hours by using an ultrasonic generator to obtain a graphene oxide aqueous solution;
step three, taking out a proper amount of polymethyl methacrylate and polycarbonate, mixing and stirring for 1h at the high temperature of 200-300 ℃, taking out and cooling to normal temperature for later use;
taking out the prepared graphene oxide aqueous solution, putting the graphene oxide aqueous solution into a reaction kettle, adding a catalyst, stirring for 30min, then putting a mixture of polymethyl methacrylate and polycarbonate into the reaction kettle, heating and treating at the temperature of 300 ℃ for 2-6h to prepare graphene oxide hydrogel;
placing the prepared graphene oxide hydrogel in an acetone solution for solvent replacement to obtain a graphene oxide gel;
and step six, taking out the prepared graphene oxide hydrogel, naturally cooling for 2 hours at normal temperature, then putting the graphene oxide hydrogel into a refrigeration house at the temperature of minus 5 ℃, and freeze-drying the graphene oxide hydrogel, and taking out the graphene oxide hydrogel to obtain the high-strength graphene oxide aerogel.
Furthermore, the metal container in the first step and the second step is a component made of stainless steel;
further, the freeze drying time in the sixth step is 4-6h, and the obtained product is taken out and placed at the normal temperature for 2 h.
Example 3:
the novel graphene aerogel material of this embodiment, wherein the main material used comprises the following components: graphene oxide, poly-4-methyl-1-pentene, polytetrafluoroethylene, a resorcinol-formaldehyde adhesive, deionized water, polymethyl methacrylate, polycarbonate and a catalyst;
specifically, the composition comprises the following components in parts by weight: 70 parts of graphene oxide, 30 parts of poly-4-methyl-1-pentene, 17 parts of polytetrafluoroethylene, 12 parts of resorcinol-formaldehyde adhesive, 50 parts of deionized water, 17 parts of polymethyl methacrylate, 17 parts of polycarbonate and 5 parts of catalyst.
Furthermore, the catalyst is any one or a combination of more than two of hydrazine hydrate, lithium aluminum hydride, p-phenylenediamine, diethylenetriamine, triethylene tetramine and tetraethylene pentamine.
A preparation method of a novel graphene aerogel material comprises the following specific operation steps:
firstly, crushing a proper amount of graphene oxide, pouring the crushed graphene oxide into a metal container after the treatment is finished, adding poly 4-methyl-1-pentene, polytetrafluoroethylene, a resorcinol-formaldehyde adhesive and deionized water into the metal container, and stirring for 2 hours to prepare a solution with the concentration of 1-10 mg/ml;
step two, heating the metal container with the solution prepared inside in warm water at 60 ℃ in a water bath, and vibrating for 4 hours by using an ultrasonic generator to obtain a graphene oxide aqueous solution;
step three, taking out a proper amount of polymethyl methacrylate and polycarbonate, mixing and stirring for 1h at the high temperature of 200-300 ℃, taking out and cooling to normal temperature for later use;
taking out the prepared graphene oxide aqueous solution, putting the graphene oxide aqueous solution into a reaction kettle, adding a catalyst, stirring for 25min, then putting a mixture of polymethyl methacrylate and polycarbonate into the reaction kettle, heating, and treating at the temperature of 300 ℃ for 2-6h to prepare graphene oxide hydrogel;
placing the prepared graphene oxide hydrogel in an acetone solution for solvent replacement to obtain a graphene oxide gel;
and step six, taking out the prepared graphene oxide hydrogel, naturally cooling for 2 hours at normal temperature, then putting the graphene oxide hydrogel into a refrigeration house at the temperature of minus 5 ℃, and freeze-drying the graphene oxide hydrogel, and taking out the graphene oxide hydrogel to obtain the high-strength graphene oxide aerogel.
Furthermore, the metal container in the first step and the second step is a component made of stainless steel;
further, the freeze drying time in the sixth step is 4-6h, and the obtained product is taken out and placed at the normal temperature for 2 h.
Example 4:
the novel graphene aerogel material of this embodiment, wherein the main material used comprises the following components: graphene oxide, poly-4-methyl-1-pentene, polytetrafluoroethylene, a resorcinol-formaldehyde adhesive, deionized water, polymethyl methacrylate, polycarbonate and a catalyst;
specifically, the composition comprises the following components in parts by weight: 80 parts of graphene oxide, 40 parts of poly-4-methyl-1-pentene, 20 parts of polytetrafluoroethylene, 15 parts of resorcinol-formaldehyde adhesive, 60 parts of deionized water, 20 parts of polymethyl methacrylate, 20 parts of polycarbonate and 6 parts of catalyst.
Furthermore, the catalyst is any one or a combination of more than two of hydrazine hydrate, lithium aluminum hydride, p-phenylenediamine, diethylenetriamine, triethylene tetramine and tetraethylene pentamine.
A preparation method of a novel graphene aerogel material comprises the following specific operation steps:
firstly, crushing a proper amount of graphene oxide, pouring the crushed graphene oxide into a metal container after the treatment is finished, adding poly 4-methyl-1-pentene, polytetrafluoroethylene, a resorcinol-formaldehyde adhesive and deionized water into the metal container, and stirring for 1-2 hours to prepare a solution with the concentration of 1-10 mg/ml;
step two, heating the metal container with the solution prepared inside in warm water at 60 ℃ in a water bath, and vibrating for 3 hours by using an ultrasonic generator to obtain a graphene oxide aqueous solution;
step three, taking out a proper amount of polymethyl methacrylate and polycarbonate, mixing and stirring for 1h at the high temperature of 200-300 ℃, taking out and cooling to normal temperature for later use;
taking out the prepared graphene oxide aqueous solution, putting the graphene oxide aqueous solution into a reaction kettle, adding a catalyst, stirring for 30min, then putting a mixture of polymethyl methacrylate and polycarbonate into the reaction kettle, heating and treating at the temperature of 200 ℃ for 2-6h to prepare graphene oxide hydrogel;
placing the prepared graphene oxide hydrogel in an acetone solution for solvent replacement to obtain a graphene oxide gel;
and step six, taking out the prepared graphene oxide hydrogel, naturally cooling for 2 hours at normal temperature, then putting the graphene oxide hydrogel into a refrigeration house at the temperature of minus 5 ℃, and freeze-drying the graphene oxide hydrogel, and taking out the graphene oxide hydrogel to obtain the high-strength graphene oxide aerogel.
Furthermore, the metal container in the first step and the second step is a component made of stainless steel;
further, the freeze drying time in the sixth step is 4-6h, and the obtained product is taken out and placed at the normal temperature for 2 h.
The graphene aerogels prepared in the above embodiments 1 to 4 were subjected to performance tests, and the following data were obtained:
| flame retardant rating | Light transmittance | Short term heat resistance temperature | Degree of molding shrinkage | |
| Example 1 | Stage B1 | 56％ | 413 | Height of |
| Example 2 | Stage B1 | 63％ | 416 | Is low in |
| Example 3 | Stage B1 | 82％ | 438 | Is low in |
| Example 4 | Stage B1 | 75％ | 425 | Is low in |
Known from the table, raw materials cooperation proportion is moderate in embodiment 3, the graphite alkene aerogel that makes possesses good heat resistance and flame retardant property in the use, and the finished product luminousness that makes is higher, make the outward appearance more pleasing to the eye, the cooperation of resorcinol-formaldehyde adhesive and other raw materials, the water resistance that has improved graphite alkene aerogel and the life that has prolonged graphite alkene aerogel, and the mechanical strength and the antioxidant property of graphite alkene aerogel have been improved, and graphite alkene aerogel shrinkage factor after the shaping is lower, make the graphite alkene aerogel size stability of making good.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (7)
1. A novel graphene aerogel material is characterized in that: the used main materials comprise the following raw materials in parts by weight: 60-80 parts of graphene oxide, 20-40 parts of poly-4-methyl-1-pentene, 10-20 parts of polytetrafluoroethylene, 5-15 parts of resorcinol-formaldehyde adhesive, 40-60 parts of deionized water, 10-20 parts of polymethyl methacrylate, 10-20 parts of polycarbonate and 2-6 parts of catalyst.
2. The novel graphene aerogel material according to claim 1, wherein: the used main materials comprise the following raw materials in parts by weight: 65-75 parts of graphene oxide, 25-35 parts of poly 4-methyl-1-pentene, 13-17 parts of polytetrafluoroethylene, 8-12 parts of resorcinol-formaldehyde adhesive, 45-55 parts of deionized water, 13-17 parts of polymethyl methacrylate, 13-17 parts of polycarbonate and 3-5 parts of catalyst.
3. The novel graphene aerogel material according to claim 1, wherein: the used main materials comprise the following raw materials in parts by weight: 70 parts of graphene oxide, 30 parts of poly-4-methyl-1-pentene, 15 parts of polytetrafluoroethylene, 10 parts of resorcinol-formaldehyde adhesive, 50 parts of deionized water, 15 parts of polymethyl methacrylate, 15 parts of polycarbonate and 4 parts of catalyst.
4. The novel graphene aerogel material according to claim 1, wherein: the catalyst is any one or a combination of more than two of hydrazine hydrate, lithium aluminum hydride, p-phenylenediamine, diethylenetriamine, triethylene tetramine and tetraethylene pentamine.
5. The novel graphene aerogel material according to any one of claims 1 to 4, further comprising a preparation method of the novel graphene aerogel material, wherein the preparation method comprises the following specific operation steps:
firstly, crushing a proper amount of graphene oxide, pouring the crushed graphene oxide into a metal container after the treatment is finished, adding poly 4-methyl-1-pentene, polytetrafluoroethylene, a resorcinol-formaldehyde adhesive and deionized water into the metal container, and stirring for 30 minutes to prepare a solution with the concentration of 1-10 mg/ml;
step two, heating the metal container with the solution prepared inside in warm water at 60 ℃ in a water bath, and vibrating for 2-4h by using an ultrasonic generator to obtain a graphene oxide aqueous solution;
taking out a proper amount of polymethyl methacrylate and polycarbonate, mixing and stirring for 1h at the high temperature of 300 ℃, taking out and cooling to normal temperature for later use;
taking out the prepared graphene oxide aqueous solution, putting the graphene oxide aqueous solution into a reaction kettle, adding a catalyst, stirring for 20-30min, then adding a mixture of polymethyl methacrylate and polycarbonate into the reaction kettle, heating, and treating at the temperature of 100-300 ℃ for 2-6h to prepare graphene oxide hydrogel;
placing the prepared graphene oxide hydrogel in an acetone solution for solvent replacement to obtain a graphene oxide gel;
and step six, taking out the prepared graphene oxide hydrogel, naturally cooling for 2 hours at normal temperature, then putting the graphene oxide hydrogel into a refrigeration house at the temperature of minus 5 ℃, and freeze-drying the graphene oxide hydrogel, and taking out the graphene oxide hydrogel to obtain the high-strength graphene oxide aerogel.
6. The preparation method of the novel graphene aerogel material according to claim 5, wherein the preparation method comprises the following steps: the metal container in the first step and the second step is a stainless steel component.
7. The preparation method of the novel graphene aerogel material according to claim 5, wherein the preparation method comprises the following steps: and in the sixth step, the freeze drying time is 4-6h, and the mixture is taken out and placed at the normal temperature for 2 h.
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