CN112430450B - Modified graphene nanosheet composite powder and preparation method thereof - Google Patents
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Abstract
The invention relates to a modified graphene nanosheet composite powder and a preparation method thereof. Soaking a certain amount of graphene nanosheets in a nitric acid solution, mechanically stirring, washing the graphene nanosheets, mixing the washed graphene nanosheets with an organic ligand, cobalt salt and deionized water, uniformly dispersing the graphene nanosheets into the solution under the combined action of ultrasonic oscillation and mechanical stirring to form slurry, pouring the slurry into a reaction kettle, and reacting under a certain condition, wherein Co-MOFs (cobalt metal organic framework complex) can be attached to the surface of the graphene nanosheets in the process. And (3) taking out the reaction kettle after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the Co-MOFs modified graphene composite powder after the reaction, and drying in a vacuum drying oven to obtain the composite material powder with the Co-MOFs particles compounded on the surfaces of the graphene nanosheets.
Description
Technical Field
The invention relates to a surface modification process of a graphene nanosheet, in particular to modified graphene nanosheet composite powder and a preparation method thereof.
Background
Since the discovery of graphene, graphene has been widely used in various fields, such as batteries, electrical components, microwave absorption, biomaterials, and the like, due to its unique good mechanical properties, electrical properties, and chemical stability. However, in many fields, it is difficult for single graphene to meet the required performance requirements, so that surface modification of graphene is increasingly important to research methods capable of updating and improving the performance of graphene. Compared with a single-layer or double-layer graphene lamellar structure, the graphite nanosheet prepared by the physical vapor phase stripping method is a lamellar nanomaterial with the thickness of about 3 nanometers and the number of layers of a graphite structure of about 10 layers. This material cost is much lower than single or double layer graphene materials. On the other hand, MOF (metal organic framework) materials have been widely paid attention and used in recent years due to their unique characteristics of high porosity structure and controllable morphology. Particularly in the field of wave absorption, the MOF is used for carrying out surface modification on the graphene which mainly comprises dielectric loss, so that the wave absorption performance can be effectively improved, and the method is a good modification method.
The invention aims to provide a novel preparation method for modifying a cobalt metal organic framework complex on the surface of a graphene (alkene) nanosheet, which is used for improving the wave-absorbing characteristic of graphene (alkene) powder.
Disclosure of Invention
The invention aims to provide a novel preparation method of modified graphite nanosheet wave-absorbing composite powder and the modified graphite (alkene) nanosheet composite powder, which are used for improving the wave-absorbing property of the graphite (alkene) powder.
The technical effects of the invention can be obtained by the following technical scheme:
a preparation method of modified graphene (alkene) nanosheet wave-absorbing composite powder and the modified graphene (alkene) nanosheet composite powder comprise the following steps:
step one, activation pretreatment: soaking the graphene nanosheets in a nitric acid solution, mechanically stirring for not less than 12 hours, taking out the graphene nanosheets, washing, and filtering for later use to obtain etched and activated graphene nanosheets A;
step two: placing the graphene nanosheet A obtained in the step one in an organic ligand, cobalt salt and deionized water according to the proportion of 2g/L, fully stirring and mixing to enable the graphene nanosheet A, the organic ligand and the cobalt salt to be uniformly dispersed in the deionized water to form slurry A,
step three: pouring the slurry A obtained in the second step into a reaction kettle, reacting the slurry A and the reaction kettle together at 120-200 ℃ for 48-72 hours to generate Co-MOFs (cobalt metal organic framework complex), wherein the Co-MOFs can be attached to the surface of the graphene (alkene) nanosheet A at the same time to obtain modified graphene (alkene) composite powder B;
step four: and (3) taking out the reaction kettle in the third step, after the reaction kettle is naturally cooled to room temperature, carrying out suction filtration to take out the modified graphene composite powder B obtained in the third step, and drying the modified graphene composite powder B in a vacuum drying oven at 65 ℃ for 12 hours to obtain modified graphene composite powder C.
Further, the graphene nanoplatelets a of step one are taken out for washing, requiring multiple measurements with deionized water until the nitric acid solution in which the graphene nanoplatelets are soaked is diluted to a pH >5.
Further, the volume ratio of the graphene nanosheets to the nitric acid solution in the first step is 1,
and further, in the step two, the full stirring is realized by simultaneously stirring ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power of the ultrasonic oscillation is 300W, and the mechanical stirring speed is 2000r/min.
Further, in the second step, the organic ligand is one or more of bipyridyl, triphenylamine tricarboxylate, terephthalic acid, pyrazine or organic ligands with the same properties as the materials.
Further, the cobalt salt in the second step is common cobalt compounds such as cobalt acetate, cobalt sulfate, cobalt chloride, cobalt nitrate and the like.
Further, the graphene (alkene) nanosheet in the step one can be prepared from a graphite nanosheet obtained by a physical gas phase stripping method or reduced graphene oxide obtained by a chemical oxidation-reduction method.
Further, in the second step, the ratio of the organic ligand, the cobalt salt and the deionized water is 1.
According to the modified graphene (alkene) nanosheet composite powder obtained by the preparation method, co-MOFs particles are uniformly loaded on the surface of the modified graphene (alkene) composite powder C.
Has the advantages that:
the invention discloses a preparation method of modified graphite nanosheet wave-absorbing composite powder and modified graphite (graphene) nanosheet composite powder. Stirring and fusing the acidified and ultrasonically treated graphene nanosheets, cobalt salt and an organic ligand in water, then placing the obtained slurry in a reaction kettle, and carrying out adhesion and combination on the graphene nanosheets and Co-MOFs (cobalt metal organic framework complexes) generated in the reaction process through a hydrothermal method so as to obtain the composite powder of the graphene nanosheets and the Co-MOFs. According to the invention, a hydrothermal method is adopted to compound the graphene (alkene) nanosheets and the Co-MOFs, so that the complex step of preparing the MOF precursor and compounding is omitted, the complex is generated and compounded with the graphene (alkene) nanosheets simultaneously in the hydrothermal process, and the process flow is simplified; in the process of carrying out ultrasonic and stirring on the slurry, the dispersion degree of the graphene nanosheets in the slurry can be effectively improved, the specific surface area of the graphene nanosheets is increased, and Co-MOFs particles can be more uniformly loaded on the surfaces of the graphene nanosheets. The preparation process is simple and easy to operate, and can be put into industrial production.
Compared with the existing preparation process, the product of the graphene surface modified composite wave-absorbing material has a single structure; in the prior art, the raw material is chemically prepared Graphene Oxide (GO) or a product rGO reduced by the Graphene Oxide (GO), and the preparation steps of the modification of the Co-MOFs particles attached to the surfaces of the graphene (alkene) nanosheets are complicated; and the graphite (alkene) nanosheet is too fine to be dispersed in a solution, and the process operation is difficult. Therefore, the invention provides a preparation method which is simple and convenient to prepare, low in equipment requirement and wide in preparation conditions. By using the hydrothermal temperature difference as a driving force, organic metal ligands are synthesized in a single reaction and are simultaneously attached to the surface of the graphene (alkene) to complete the modification of the cobalt metal organic framework complex on the surface of the graphene (alkene), so that the three-dimensional structure composite wave-absorbing material with high porosity is obtained, the complex morphology of the three-dimensional structure composite wave-absorbing material is favorable for the refraction and absorption of electromagnetic waves, the natural disadvantage that a single graphene (alkene) nanosheet only has dielectric microwave loss can be effectively overcome, and various absorption mechanisms are introduced on the premise that the excellent mechanical properties of the graphene (alkene) material are retained, so that the comprehensive wave-absorbing performance of the graphene (alkene) material is improved. The obtained cobalt metal organic framework complex modified graphene powder has composite wave-absorbing effects of electric loss, magnetic loss and the like, and is obviously superior to the wave-absorbing powder using graphite nanosheets or cobalt alone.
Detailed Description
The present invention will be further described below based on preferred embodiments.
The terminology used in the description is for the purpose of describing the embodiments of the invention and is not intended to be limiting of the invention.
The invention relates to a preparation method of Co-MOFs composite graphene (alkene) nanosheet composite wave-absorbing powder, which is prepared by taking a graphene (alkene) nanosheet as a substrate, activating, dispersing in metal cobalt salt, an organic ligand and deionized water, and carrying out hydrothermal synthesis.
A preparation method of modified graphene (alkene) nanosheet wave-absorbing composite powder and the modified graphene (alkene) nanosheet composite powder comprise the following steps:
the method comprises the following steps: soaking the graphene nanosheets in a nitric acid solution, mechanically stirring for not less than 12 hours, taking out the graphene nanosheets, washing, and filtering for later use to obtain etched and activated graphene nanosheets A;
preferably, the volume ratio of the graphene nanoplatelets to the nitric acid solution is 1;
preferably, the graphene (alkene) nanosheet can be prepared from graphene nanosheets obtained by a physical vapor phase stripping method or reduced graphene oxide prepared by a chemical oxidation-reduction method.
Step two: fully stirring and mixing the graphene nanosheet A and the graphene nanosheet A in organic ligand, cobalt salt and deionized water, so that the graphene nanosheet A, the organic ligand and the cobalt salt are uniformly dispersed in the deionized water to form slurry A;
preferably, the sufficient stirring is realized by simultaneously stirring ultrasonic oscillation and mechanical stirring. The graphene nanosheets A can be uniformly dispersed in the slurry A as much as possible through ultrasonic oscillation and mechanical stirring, so that the subsequent full contact and compounding with Co-MOFs are facilitated.
Preferably, the graphene nanoplatelets a are removed for washing, requiring multiple washes with deionized water until the nitric acid solution in which the graphene nanoplatelets are immersed is diluted to a pH >5.
Preferably, the organic ligand is bipyridine, triphenylamine tricarboxylate, terephthalic acid, pyrazine or an organic ligand having the same properties as the aforementioned materials.
Preferably, the cobalt salt is a common cobalt compound such as cobalt acetate, cobalt sulfate, cobalt chloride, cobalt nitrate and the like.
In the process, the cobalt metal organic complex is generated in the aqueous solution and is attached to the surface of the graphene nanosheet, so that the complex treatment step of firstly generating the complex and then compounding the complex for the second time is omitted.
Step three: pouring the slurry A obtained in the second step into a reaction kettle, and reacting the slurry A and the reaction kettle together at 120-200 ℃ for 48-72 hours to generate Co-MOFs (cobalt metal organic framework complex) in the process, wherein the Co-MOFs can be attached to the surface of the graphene (alkene) nanosheet A at the same time to obtain modified graphene (alkene) composite powder B;
the reaction generates a binuclear cobalt metal-organic framework complex which has a unique three-dimensional porous structure and is attached to the surface of a graphene nanosheet during the reaction.
Step four: and (3) taking out the reaction kettle in the third step, naturally cooling the reaction kettle to room temperature, taking out the modified graphene composite powder B obtained in the third step, and drying the modified graphene composite powder B in a vacuum drying oven at 65 ℃ to obtain modified graphene composite powder C.
The following lists a plurality of methods for preparing the modified graphene (alkene) nanosheet wave-absorbing composite powder and the modified graphene (alkene) nanosheet composite powder prepared by the method.
Example one
The method comprises the following steps: soaking the graphene nanosheets in a nitric acid solution, mechanically stirring for not less than 12 hours, taking out the graphene nanosheets, washing, and filtering for later use to obtain etched and activated graphene nanosheets A;
step two: placing the graphene nanosheet A in a solution of deionized water, cobalt acetate 3.5g/L, bipyridine 1.5g/L and 4,4' -trimethylamine triphenylamine 3.8g/L according to the proportion of 2g/L in the first step, and fully stirring and mixing the graphene nanosheet A simultaneously through ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 300W, and the mechanical stirring speed is 2000r/min. Uniformly dispersing the graphene nanosheet A, 4' -triphenylamine tricarboxylate, bipyridine and cobalt acetate in deionized water to form slurry A;
step three: and (4) pouring the slurry A obtained in the second step into a reaction kettle, putting the reaction kettle into a 120 ℃ oven, and taking out the reaction kettle after 72 hours.
Step four: and (3) taking out the reaction kettle in the third step, after the reaction kettle is naturally cooled to room temperature, carrying out suction filtration to take out the modified graphene composite powder B obtained in the third step, and drying the modified graphene composite powder B in a vacuum drying oven at 65 ℃ for 12 hours to obtain modified graphene composite powder C.
The modified graphene composite powder obtained in the implementation has high performance, and shows that the minimum reflection loss value is-48.3 dB and the wave-absorbing bandwidth is 7.44GHz under the condition that the thickness is 5.7mm and 5.04GHz.
Example two
The method comprises the following steps: soaking the graphene nanosheets in a nitric acid solution, mechanically stirring for not less than 12 hours, taking out the graphene nanosheets, washing, and filtering for later use to obtain etched and activated graphene nanosheets A;
step two: placing the graphene nanosheet A in a solution of deionized water, 19.4g/L of cobalt nitrate, 1.5g/L of bipyridyl and 11g/L of 1, 4-terephthalic acid according to the proportion of 2g/L in the first step, fully stirring and mixing simultaneously through ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 300W, and the mechanical stirring speed is 2000r/min. Uniformly dispersing the graphene nanosheet A, 4-terephthalic acid, bipyridine and cobalt nitrate in deionized water to form slurry A;
step three: and (4) pouring the slurry A obtained in the second step into a reaction kettle, putting the reaction kettle into a 120 ℃ oven, and taking out the reaction kettle after 72 hours.
Step four: and (4) taking out the reaction kettle in the third step, after the reaction kettle is naturally cooled to room temperature, carrying out suction filtration to take out the modified graphene composite powder B obtained in the third step, and drying the modified graphene composite powder B in a vacuum drying oven at 65 ℃ for 12 hours to obtain modified graphene composite powder C.
The modified graphene composite powder obtained in the implementation has high performance, and shows that the minimum reflection loss value is-37.4 dB and the wave-absorbing bandwidth is 8.56GHz under the conditions that the thickness is 5.1mm and 5.44GHz.
EXAMPLE III
The method comprises the following steps: soaking the graphene nanosheets in a nitric acid solution, mechanically stirring for not less than 12 hours, taking out the graphene nanosheets, washing, and filtering for later use to obtain etched and activated graphene nanosheets A;
step two: and (2) placing the graphene nanosheet A in a solution of deionized water, 5.6g/L of cobalt sulfate, 1.6g/L of pyrazine and 11g/L of 1, 4-terephthalic acid according to the proportion of 2g/L in the first step, carrying out ultrasonic oscillation and mechanical stirring, and simultaneously fully stirring and mixing, wherein the ultrasonic power is 300W, and the mechanical stirring speed is 2000r/min. Uniformly dispersing the graphene nanosheet A, 4-terephthalic acid, pyrazine and cobalt sulfate in deionized water to form slurry A;
step three: and (4) pouring the slurry A obtained in the second step into a reaction kettle, putting the reaction kettle into a 120 ℃ oven, and taking out the reaction kettle after 72 hours.
Step four: and (3) taking out the reaction kettle in the third step, after the reaction kettle is naturally cooled to room temperature, carrying out suction filtration to take out the modified graphene composite powder B obtained in the third step, and drying the modified graphene composite powder B in a vacuum drying oven at 65 ℃ for 12 hours to obtain modified graphene composite powder C.
The modified graphene composite powder obtained in the implementation has high performance, and is shown in the fact that the minimum reflection loss value is-24.6 dB and the wave-absorbing bandwidth is 6.67GHz under the condition that the thickness is 4.7mm and 6.08GHz.
Example four
The method comprises the following steps: soaking the graphene nanosheets in a nitric acid solution, mechanically stirring for not less than 12 hours, taking out the graphene nanosheets, washing, and filtering for later use to obtain etched and activated graphene nanosheets A;
step two: placing the graphene nanosheet A in a solution of deionized water, cobalt chloride 4.7g/L, bipyridine 1.5g/L and 1, 4-terephthalic acid 11g/L according to the proportion of 2g/L in the first step, carrying out ultrasonic oscillation and mechanical stirring, and simultaneously fully stirring and mixing, wherein the ultrasonic power is 300W, and the mechanical stirring speed is 2000r/min. Uniformly dispersing the graphene nanosheet A, 4-terephthalic acid, bipyridine and cobalt chloride in deionized water to form slurry A;
step three: and (4) pouring the slurry A obtained in the second step into a reaction kettle, putting the reaction kettle into a 120 ℃ oven, and taking out the reaction kettle after 72 hours.
Step four: and (3) taking out the reaction kettle in the third step, after the reaction kettle is naturally cooled to room temperature, carrying out suction filtration to take out the modified graphene composite powder B obtained in the third step, and drying the modified graphene composite powder B in a vacuum drying oven at 65 ℃ for 12 hours to obtain modified graphene composite powder C.
The modified graphene composite powder obtained in the implementation has high performance, and is shown in the fact that the minimum reflection loss value is-39.5 dB and the wave-absorbing bandwidth is 6.43GHz under the conditions that the thickness is 5.1mm and 3.92GHz.
EXAMPLE five
The method comprises the following steps: soaking the graphene nanosheets in a nitric acid solution, mechanically stirring for not less than 12 hours, taking out the graphene nanosheets, washing, and filtering for later use to obtain etched and activated graphene nanosheets A;
step two: placing the graphene nanosheet A in a solution of deionized water, 3.5g/L of cobalt acetate, 1.5g/L of bipyridine and 3.8g/L of 4,4' -triphenylamine tricarboxylate according to the proportion of 2g/L in the first step, fully stirring and mixing the solution simultaneously by ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power is 300W, and the mechanical stirring speed is 2000r/min. Dispersing the graphene nanosheet A, 4' -triphenylamine tricarboxylate, bipyridine and cobalt acetate in deionized water uniformly to form slurry A;
step three: and (3) pouring the slurry A obtained in the second step into a reaction kettle, putting the reaction kettle into a 200 ℃ oven, and taking out after 48 hours.
Step four: and (4) taking out the reaction kettle in the third step, after the reaction kettle is naturally cooled to room temperature, carrying out suction filtration to take out the modified graphene composite powder B obtained in the third step, and drying the modified graphene composite powder B in a vacuum drying oven at 65 ℃ for 12 hours to obtain modified graphene composite powder C.
The modified graphene composite powder obtained in the implementation has high performance, and shows that the minimum reflection loss value is-33.4 dB and the wave-absorbing bandwidth is 7.20GHz under the conditions that the thickness is 4.8mm and the thickness is 4.96GHz.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit of the invention, and it is intended to claim all such changes and modifications as fall within the scope of the appended claims.
Claims (7)
1. A preparation method of modified graphene nanosheet composite powder is characterized by comprising the following steps:
step one, activation pretreatment: soaking the graphene nanosheets in a nitric acid solution, mechanically stirring for not less than 12 hours, taking out the graphene nanosheets, washing, and filtering for later use to obtain etched and activated graphene nanosheets A;
step two: placing the graphene nanosheet A obtained in the first step into an organic ligand, a cobalt salt and deionized water according to the proportion of 2g/L, and fully stirring and mixing to uniformly disperse the graphene nanosheet A, the organic ligand and the cobalt salt in the deionized water to form slurry A;
step three: pouring the slurry A obtained in the second step into a reaction kettle, and reacting the slurry A and the reaction kettle together at the temperature of 120-200 ℃ for 48-72 hours to generate a cobalt metal organic framework complex in the process, wherein the cobalt metal organic framework complex is attached to the surface of the graphene nanosheet A at the same time to obtain a modified graphene composite powder B;
step four: taking out the reaction kettle in the third step, after the reaction kettle is naturally cooled to room temperature, carrying out suction filtration to take out the modified graphene composite powder B obtained in the third step, and drying the modified graphene composite powder B in a vacuum drying oven at 65 ℃ for 12 hours to obtain modified graphene composite powder C;
taking out and washing the graphene nanosheet A, and washing with deionized water for multiple times until the nitric acid solution for soaking the graphene nanosheet is diluted to a pH value of more than 5;
in the first step, the volume ratio of the graphene nanosheets to the nitric acid solution is 1.
2. The method for preparing modified graphene nano sheet composite powder according to claim 1,
and step two, fully stirring, namely stirring simultaneously by ultrasonic oscillation and mechanical stirring, wherein the ultrasonic power of the ultrasonic oscillation is 300W, and the mechanical stirring speed is 2000r/min.
3. The method for preparing modified graphene nano sheet composite powder according to claim 1,
and in the second step, the organic ligand is one or more of bipyridyl, triphenylamine tricarboxylate, terephthalic acid and pyrazine.
4. The preparation method of the modified graphene nanoplatelet composite powder of claim 1,
the cobalt salt in the second step is one or more of cobalt acetate, cobalt sulfate, cobalt chloride and cobalt nitrate.
5. The method for preparing modified graphene nano sheet composite powder according to claim 1,
the graphene nanosheet in the step one is the graphene nanosheet obtained by adopting a physical gas phase stripping method or the reduced graphene oxide prepared by adopting a chemical oxidation reduction method.
6. The method for preparing modified graphene nano sheet composite powder according to claim 1,
in the second step, the molar ratio of the organic ligand, the cobalt salt and the deionized water is 1.
7. The modified graphene nanoplatelet composite powder obtained by the preparation method of any one of claims 1 to 6, wherein the surface of the modified graphene composite powder C is uniformly loaded with cobalt metal organic framework complex particles.
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