CN112138631B - Preparation method of graphene oxide/activated carbon composite material - Google Patents
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- CN112138631B CN112138631B CN202010707283.9A CN202010707283A CN112138631B CN 112138631 B CN112138631 B CN 112138631B CN 202010707283 A CN202010707283 A CN 202010707283A CN 112138631 B CN112138631 B CN 112138631B
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Abstract
The invention relates to a preparation method of a graphene oxide/activated carbon composite material, which comprises the following steps: s1, preparing graphene oxide solution; s2, dropwise adding a polyvinyl alcohol solution to the graphene oxide solution, and stirring for a first preset time to obtain a first mixed solution; s3, adding coconut shell carbon into the first mixed solution, stirring for a second preset time, and standing to obtain a second mixed solution; s4, adding soluble starch, formaldehyde and pentane into the second mixed solution, and fully stirring to obtain a third mixed solution; s5, dropwise adding concentrated sulfuric acid into the third mixed solution, then sending the solution into an oven to solidify the solution at a first preset temperature for a third preset time, and washing the solidified product for a plurality of times by deionized water to obtain the graphene oxide/activated carbon composite material. The process of the foam graphene oxide can avoid stacking of the graphene oxide sheets and maintain the characteristics of the graphene oxide single sheets.
Description
Technical Field
The invention relates to the field of composite material preparation, in particular to a preparation method of a graphene oxide/activated carbon composite material.
Background
The active carbon has ultrahigh specific surface area, but the oxygen-containing functional groups on the surface of the active carbon are limited, and the available active sites are limited; and the macropores of the activated carbon provide limited specific surface area.
Graphene has good electrical and mechanical properties, but the characteristics of a two-dimensional structure of graphene lead to the fact that graphene is difficult to stably exist, and agglomeration usually occurs. Specifically, graphene oxide obtained after grafting an oxygen-containing functional group on a graphene sheet layer can be stably dispersed in an aqueous solution. However, solid graphene oxide is difficult to maintain the characteristics of a monolithic layer.
Therefore, how to realize the combination of activated carbon and graphene oxide is a problem to be solved.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene oxide/activated carbon composite material, which can obtain a stable graphene oxide/activated carbon composite material.
In order to achieve the above object, the present invention provides a preparation method of a graphene oxide/activated carbon composite material, comprising the following steps:
s1, preparing graphene oxide solution;
s2, dropwise adding a polyvinyl alcohol solution to the graphene oxide solution, and stirring for a first preset time to obtain a first mixed solution;
s3, adding coconut shell carbon into the first mixed solution, stirring for a second preset time, and standing to obtain a second mixed solution;
s4, adding soluble starch, formaldehyde and pentane into the second mixed solution, and fully stirring to obtain a third mixed solution;
s5, dropwise adding concentrated sulfuric acid into the third mixed solution, then sending the solution into an oven to solidify the solution at a first preset temperature for a third preset time, and washing the solidified product for a plurality of times by deionized water to obtain the graphene oxide/activated carbon composite material.
According to one aspect of the present invention, in step S1, the concentration of the graphene oxide in the graphene oxide solution is 1-3mg/ml.
According to one aspect of the invention, the polyvinyl alcohol solution is prepared by dissolving polyvinyl alcohol in deionized water, and the concentration of the polyvinyl alcohol is 0.03-0.1g/ml.
According to one aspect of the invention, the first preset time is 0.5-1.5h.
According to one aspect of the invention, in step S3. And the second preset time is 4 hours, and the second mixed solution is obtained after stirring for the second preset time and then standing for at least 12 hours.
According to one aspect of the invention, in step S4. The amount of soluble starch added to the second mixed solution is 5-9g, the amount of formaldehyde is 10-12ml, and the amount of pentane is 5-8ml.
According to one aspect of the present invention, in step S5, the amount of concentrated sulfuric acid added dropwise to the third mixed solution is 5-10ml.
According to one aspect of the invention, the first preset temperature is 50-70 ℃ and the third preset time is 1-2h.
According to one aspect of the present invention, in step S1, it includes:
s11, preparing a first solution by using crystalline flake graphite, concentrated sulfuric acid and potassium permanganate, heating the first solution to a second preset temperature, performing an oxidation reaction for a fourth preset time to obtain a second solution, and dropwise adding deionized water into the second solution according to a first preset adding amount. Heating to a third preset temperature after the dripping is completed, carrying out a reaction for a fifth preset time, adding deionized water again to terminate the reaction, cooling the reacted solution to room temperature, and dropwise adding hydrogen peroxide until no bubbles are generated and a third solution is obtained;
s12, filtering and washing the third solution until the solution is neutral to obtain a graphite oxide solution, and performing mechanical ultrasonic treatment on the graphite oxide solution to obtain the graphene oxide solution.
10. The method according to claim 9, wherein the preparing of the first solution from the flake graphite, the concentrated sulfuric acid and the potassium permanganate in the step S1 comprises:
s111, stirring the crystalline flake graphite under an ice water bath and adding the concentrated sulfuric acid into the crystalline flake graphite;
and S112, adding the potassium permanganate into the solution in the step S111, and stirring under ice water bath to obtain the first solution.
According to one aspect of the invention, in step S111, the flake graphite has a flake diameter of 5000-325 mesh, and the mass ratio of the flake graphite to the concentrated sulfuric acid is 1:45-1:55.
According to one aspect of the present invention, in step S111, the concentrated sulfuric acid is stirred for 10 to 30 minutes after the addition is completed.
According to one aspect of the invention, in step S112, the potassium permanganate is added at a rate of 1g/min, and the mass ratio of the crystalline flake graphite to the potassium permanganate is 1:1 to 1:4.
According to one aspect of the invention, step S112, stirring for 30-60min after the potassium permanganate addition is completed.
According to one aspect of the invention, the second preset temperature is 30-40 ℃, and the fourth preset time is 1-3 hours;
the third preset temperature is 70-85 ℃, and the fifth preset time is 30-60min.
According to one aspect of the invention, the first preset addition amount is 100-400ml.
According to one aspect of the invention, in step S4. And in the step of adding the soluble starch, formaldehyde and pentane into the second mixed solution and fully stirring to obtain a third mixed solution, the stirring speed is 350-600r/min.
According to one aspect of the present invention, in the step of stopping the reaction by adding deionized water again in the step S11, the amount of deionized water added is 1 to 1.5L.
According to the scheme of the invention, the process of the foam graphene oxide can avoid stacking of the graphene oxide sheets and maintain the characteristics of the graphene oxide single sheets.
According to the scheme provided by the invention, the graphene oxide foam fills the gaps of the active carbon, so that the specific surface area of the active carbon is increased.
According to one scheme of the invention, the graphene oxide sheet layer has rich oxygen-containing functional groups, and more reactive sites are provided for the graphene oxide/activated carbon composite material.
According to the scheme, stacking of the sheets can occur in the drying process of the graphene oxide, the specific surface area of the material is reduced, the problem can be avoided due to the foam structure, and the graphene oxide with the loose three-dimensional structure can provide a larger specific surface area and rich reactive sites.
According to the scheme of the invention, the activated carbon has limited oxygen-containing functional groups, is mainly porous and physically adsorbed in the adsorption application process, is unstable in adsorption, is easy to desorb, and the addition of graphene oxide with rich oxygen-containing functional groups enables the proportion of chemical adsorption to be increased, so that the adsorption effect is more stable.
According to the scheme of the invention, the difference of the sheet diameters of the graphite in the oxidation process can influence the structure of the three-dimensional foam, the sheet diameters are large, and the three-dimensional foam structure is loose; the sheet diameter is small, and the three-dimensional foam structure is compact. The tight porosity of the structure influences the transmission resistance (transmission speed) of a gas phase or a liquid phase in the subsequent adsorption process, the transmission speed can influence the contact time of substances to be adsorbed and the graphene oxide/activated carbon composite material, and the chip diameter of the crystalline flake graphite realizes the optimization adjustment of the structure compactness and the adsorption efficiency by adopting the arrangement, so that the adsorption performance of the product is further improved.
In addition, the adjustment of the graphite sheet diameter has a certain influence on the process, and the concentration and the reaction time of the potassium permanganate have a small influence on the sheet diameter of the graphene oxide. The larger the sheet diameter is, the milder the oxidation reaction is needed and the longer the reaction time is; the sheet diameter is small, and no obvious requirements are imposed on the oxidation degree and the reaction time. Furthermore, the adoption of the arrangement of the sheet diameter of the crystalline flake graphite not only improves the production efficiency, but also effectively reduces the consumption of potassium permanganate and saves the production cost.
According to the scheme of the invention, the graphene oxide/activated carbon composite material has a compact foam structure, the resistance of the target adsorbate passing through the composite material is large, the time of passing through the adsorption path is long, the contact time is long, the adsorption is thorough, and the adsorption effect is good.
Drawings
FIG. 1 schematically shows a block diagram of steps of a preparation method according to an embodiment of the invention;
Detailed Description
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments will be briefly described below. It is apparent that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
In describing embodiments of the present invention, the terms "longitudinal," "transverse," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in terms of orientation or positional relationship shown in the drawings for convenience of description and simplicity of description only, and do not denote or imply that the devices or elements in question must have a particular orientation, be constructed and operated in a particular orientation, so that the above terms are not to be construed as limiting the invention.
The present invention will be described in detail below with reference to the drawings and the specific embodiments, which are not described in detail herein, but the embodiments of the present invention are not limited to the following embodiments.
As shown in fig. 1, according to an embodiment of the present invention, a preparation method of a graphene oxide/activated carbon composite material of the present invention includes the steps of:
s1, preparing graphene oxide solution;
s2, dropwise adding a polyvinyl alcohol solution into the graphene oxide solution, and stirring for a first preset time to obtain a first mixed solution;
s3, adding coconut shell carbon into the first mixed solution, stirring for a second preset time, and standing to obtain a second mixed solution;
s4, adding soluble starch, formaldehyde and pentane into the second mixed solution, and fully stirring to obtain a third mixed solution;
s5, dropwise adding concentrated sulfuric acid into the third mixed solution, then sending the third mixed solution into an oven to cure the third mixed solution at a first preset temperature for a third preset time, and washing the cured product for a plurality of times by adopting deionized water to obtain the graphene oxide/activated carbon composite material.
According to one embodiment of the present invention, in the graphene oxide solution prepared in step S1, the concentration of graphene oxide is 1-3mg/ml. By the arrangement, the performance and quality of the final finished product are ensured and improved, and if the conditions are exceeded or fallen below, the defect that the finished product is invalid is easily caused.
According to one embodiment of the present invention, in step S2, a polyvinyl alcohol (PVA) solution is prepared by dissolving polyvinyl alcohol in deionized water, and the concentration of polyvinyl alcohol is 0.03-0.1g/ml. Through the arrangement, the internal bonding strength of the materials is ensured, and micro cracks in the finished product in the subsequent production process are effectively reduced or avoided, so that the performance and quality of the final finished product are guaranteed and improved, and if the conditions are exceeded or lower than the conditions, the cracks of the finished product are easily excessive and broken.
According to one embodiment of the present invention, in step S1, in the case of stirring the graphene oxide solution obtained in step S1, a polyvinyl alcohol solution is added, and stirring is continued for a first preset time after the addition is completed. In this embodiment, the first preset time is 0.5 to 1.5 hours. Through the arrangement, the materials can be fully mixed, which is beneficial to ensuring and improving the performance and quality of the final finished product,
according to one embodiment of the invention, in step S3. Adding coconut shell charcoal into the first mixed solution, uniformly stirring for a second preset time, and standing for at least 12 hours after stirring for the second preset time to obtain a second mixed solution. In this embodiment, the second preset time is 4h. By setting the stirring time and the standing time long enough, the sufficient contact between the solution and the coconut shell carbon is ensured, the good performance of the prepared second mixed solution is ensured,
according to one embodiment of the invention, in step S4. The amount of the soluble starch added to the second mixed solution is 5-9g per 100ml of graphene oxide solution, the amount of formaldehyde is 10-12ml per 100ml of graphene oxide solution, and the amount of pentane is 5-8ml per 100ml of graphene oxide solution. In this embodiment, after adding starch, formaldehyde and pentane, vigorous stirring is carried out at a rotational speed of 350-600r/min, so that it can be reacted sufficiently. Through the arrangement, the added materials can be stirred uniformly in a short time, and the method is beneficial to ensuring and improving the performance and quality of the final finished product.
According to one embodiment of the present invention, in step S5, the amount of concentrated sulfuric acid added dropwise to the third mixed solution is 5 to 10ml. In the embodiment, after the addition of the concentrated sulfuric acid is completed, the obtained product is dried and solidified in an oven at a first preset temperature of 50-70 ℃ and a third preset time of 1-2h. By the arrangement, the added materials can be fully reacted, and the method is beneficial to ensuring and improving the performance and quality of the final finished product.
According to an embodiment of the present invention, in step S1, it includes:
s11, preparing a first solution by using crystalline flake graphite, concentrated sulfuric acid and potassium permanganate, heating the first solution to a second preset temperature, performing an oxidation reaction for a fourth preset time to obtain a second solution, and dropwise adding deionized water into the second solution according to the first preset adding amount. Heating to a third preset temperature after the dripping is completed, reacting for a fifth preset time, adding deionized water again to terminate the reaction, cooling the reacted solution to room temperature, dropwise adding hydrogen peroxide until no bubbles are generated, and obtaining a third solution; in this embodiment, the first preset addition amount is 100-400ml.
S12, filtering and washing the third solution until the solution is neutral to obtain a graphite oxide solution, and performing mechanical ultrasonic treatment on the graphite oxide solution to obtain the graphene oxide solution.
According to one embodiment of the invention, in the step of adding deionized water again to terminate the reaction, the amount of deionized water added is 1 to 1.5L.
According to one embodiment of the present invention, in the step S11, the step of preparing the first solution from the flake graphite, the concentrated sulfuric acid and the potassium permanganate includes:
s111, stirring the crystalline flake graphite under an ice water bath and adding concentrated sulfuric acid into the crystalline flake graphite. In the embodiment, the flake diameter of the crystalline flake graphite is 5000-325 meshes, and the mass ratio of the crystalline flake graphite to the concentrated sulfuric acid is 1:45-1:55. In this embodiment, the concentrated sulfuric acid is stirred for 10 to 30 minutes after the addition is completed. By the arrangement, the added materials can be fully reacted, and the method is beneficial to ensuring and improving the performance and quality of the final finished product.
And S112, adding potassium permanganate into the solution in the step S111, and stirring under an ice water bath to obtain a first solution. In the embodiment, the adding speed of the potassium permanganate is 1g/min, and the mass ratio of the crystalline flake graphite to the potassium permanganate is 1:1 to 1:4. In this embodiment, the stirring is performed for 30 to 60 minutes after the completion of the addition of potassium permanganate. By the arrangement, the added materials can be fully reacted, and the method is beneficial to ensuring and improving the performance and quality of the final finished product.
According to one embodiment of the present invention, in the step S11, in the step of heating the first solution to the second preset temperature and performing the oxidation reaction for the fourth preset time to obtain the second solution, the first solution is slowly heated to the second preset temperature, and the second preset temperature is 30-40 ℃. And after the temperature is raised, keeping the temperature for a fourth preset time which is 1-3h. In the embodiment, after the second solution is kept at a constant temperature, the deionized water with the first preset addition amount of 100-400ml is slowly added dropwise, after the water addition is completed, the temperature is raised to a third preset temperature, and constant-temperature stirring is carried out for a fifth preset time. In this embodiment, the third preset temperature is 70-85 ℃, and the fifth preset time is 30-60min. By the arrangement, the added materials can be fully reacted, and the method is beneficial to ensuring and improving the performance and quality of the final finished product.
To further illustrate the invention, an example is based on the above scheme.
Preparation of graphene oxide solution
9g of flake graphite with a flake diameter of 5000-325 meshes is selected as a raw material, 240ml of concentrated sulfuric acid is added into the graphite under the condition of stirring, the mass ratio of the flake graphite to the concentrated sulfuric acid is 1:45-1:55, and then the reaction equipment is placed in an ice-water bath for stirring for 10-30min, so that the graphite is uniformly dispersed in the concentrated sulfuric acid;
then slowly adding potassium permanganate under stirring of ice water bath, wherein the mass ratio of the crystalline flake graphite to the potassium permanganate d is=1:1-1:4. In the embodiment, the adding speed of the potassium permanganate is 1g/min, and after the adding is finished, stirring is carried out for 30-60min under an ice water bath, so that the potassium permanganate is completely dissolved;
then slowly heating to 30-40 ℃, keeping the constant temperature for 1-3 hours, slowly dropwise adding 100-400ml of deionized water, heating to 80 ℃ after water addition is completed, stirring at the constant temperature for 30 minutes, adding a large amount of deionized water to dilute the acid solution to terminate the reaction, and then slowly dropwise adding hydrogen peroxide until no bubbles are generated;
and filtering and washing the solution after the reaction is completed to be neutral to obtain a graphite oxide solution, and then performing mechanical ultrasonic treatment to obtain the graphene oxide solution. In this embodiment, the concentration of the graphene oxide solution is 1 to 3mg/ml.
Obtaining graphene oxide/activated carbon composite material
1-3g of PVA is completely dissolved in 30ml of deionized water, then 100ml of graphene oxide solution prepared in the previous step is dropwise added under stirring, the stirring is carried out for 0.5-1.5h, then the uniformly mixed solution is mixed with coconut shell carbon, the mixture is stirred for 4h and then is left to stand for a night so that the solution is fully contacted with the coconut shell carbon, then 5-8g of soluble starch is added, then 10-12ml of formaldehyde and 5-8ml of pentane are added into the solution, the stirring is violent, 5-10ml of concentrated sulfuric acid is added dropwise after full reaction, and then the product is solidified in an oven at 60 ℃ for 1.5h. And finally washing with deionized water for 3 times to obtain the graphene oxide/activated carbon composite material.
According to the invention, stacking of sheets can occur in the drying process of the graphene oxide, the specific surface area of the material is reduced, the foam structure can avoid the problem, and the graphene oxide with a loose three-dimensional structure can provide a larger specific surface area and rich reactive sites.
According to the invention, the activated carbon has limited oxygen-containing functional groups, and is mainly subjected to pore physical adsorption in the adsorption application process, so that the adsorption is unstable, desorption is easy to occur, the proportion of chemical adsorption is increased by adding the graphene oxide with rich oxygen-containing functional groups, and the adsorption effect is more stable.
According to the invention, the difference of the sheet diameters of the graphite in the oxidation process can influence the structure of the three-dimensional foam, the sheet diameters are large, and the three-dimensional foam structure is loose; the sheet diameter is small, and the three-dimensional foam structure is compact. The tight porosity of the structure influences the transmission resistance (transmission speed) of a gas phase or a liquid phase in the subsequent adsorption process, the transmission speed can influence the contact time of substances to be adsorbed and the graphene oxide/activated carbon composite material, and the chip diameter of the crystalline flake graphite realizes the optimization adjustment of the structure compactness and the adsorption efficiency by adopting the arrangement, so that the adsorption performance of the product is further improved.
In addition, the adjustment of the graphite sheet diameter has a certain influence on the process, and the concentration and the reaction time of the potassium permanganate have a small influence on the sheet diameter of the graphene oxide. The larger the sheet diameter is, the milder the oxidation reaction is needed and the longer the reaction time is; the sheet diameter is small, and no obvious requirements are imposed on the oxidation degree and the reaction time. Furthermore, the adoption of the arrangement of the sheet diameter of the crystalline flake graphite not only improves the production efficiency, but also effectively reduces the consumption of potassium permanganate and saves the production cost.
According to the graphene oxide/activated carbon composite material, the foam structure is compact, the resistance of a target adsorbate passing through the composite material is large, the time of passing through an adsorption path is long, the contact time is long, the adsorption is thorough, and the adsorption effect is good.
The foregoing is merely exemplary of embodiments of the invention and, as regards devices and arrangements not explicitly described in this disclosure, it should be understood that this can be done by general purpose devices and methods known in the art.
The above description is only one embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. The preparation method of the graphene oxide/activated carbon composite material comprises the following steps:
9g of flake graphite with a flake diameter of 5000-325 meshes is selected as a raw material, 240mL of concentrated sulfuric acid is added into the graphite under the condition of stirring, the mass ratio of the flake graphite to the concentrated sulfuric acid is 1:45-1:55, and then the reaction equipment is placed in an ice-water bath for stirring for 10-30min, so that the graphite is uniformly dispersed in the concentrated sulfuric acid;
slowly adding potassium permanganate under stirring of ice water bath, wherein the mass ratio of the crystalline flake graphite to the potassium permanganate is (1:1) - (1:4); the adding speed of the potassium permanganate is 1g/min, and after the adding is finished, stirring is carried out for 30-60min under an ice water bath, so that the potassium permanganate is completely dissolved;
then slowly heating to 30-40 ℃, keeping the constant temperature for 1-3 hours, slowly dropwise adding 100-400mL of deionized water, heating to 80 ℃ after water addition is completed, stirring at the constant temperature for 30 minutes, adding a large amount of deionized water to dilute the acid solution to terminate the reaction, and then slowly dropwise adding hydrogen peroxide until no bubbles are generated;
filtering and washing the solution after the reaction is completed to be neutral to obtain a graphite oxide solution, and then performing mechanical ultrasonic treatment to obtain a graphene oxide solution; the concentration of the graphene oxide solution is 1-3mg/mL;
completely dissolving 1-3g of PVA in 30mL of deionized water, dropwise adding 100mL of graphene oxide solution prepared in the previous step under stirring, stirring for 0.5-1.5h, mixing the uniformly mixed solution with coconut carbon, standing overnight after stirring for 4h to enable the solution to be fully contacted with the coconut carbon, adding 5-8g of soluble starch, adding 10-12mL of formaldehyde and 5-8mL of pentane into the solution, vigorously stirring, dropwise adding 5-10mL of concentrated sulfuric acid after full reaction, and curing the product in an oven at 60 ℃ for 1.5h; and finally washing with deionized water for 3 times to obtain the graphene oxide/activated carbon composite material.
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| CN112138631A (en) | 2020-12-29 |
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