CN112791697B - Elastic super-hydrophobic graphene gel ball and preparation method and application thereof - Google Patents
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Abstract
The invention provides an elastic super-hydrophobic graphene gel ball and a preparation method and application thereof, belonging to the field of organic matter and oil spill cleaning. The method comprises the following steps: and dripping the graphene oxide aqueous dispersion liquid into a coagulating bath containing a hydrophobic gelling agent to obtain a hydrophobically modified graphene oxide gel sphere, and drying and annealing at a proper temperature to obtain the super-hydrophobic graphene aerogel sphere with good elasticity. The method provided by the invention obtains the elastic super-hydrophobic graphene gel ball by a one-step crosslinking gel method. The method has the advantages of simple preparation process and excellent performance, can realize continuous large-scale production, has folds and porous structures in the gel spheres, and has wide application prospect in the field of organic pollutant adsorption.
Description
Technical Field
The invention relates to the technical field of graphene and the field of organic matter and oil spill cleaning, in particular to an elastic super-hydrophobic graphene gel ball and a preparation method and application thereof.
Background
Leakage of petroleum and organic solvents is detrimental to marine and freshwater environments, and efficient spill clean-up typically requires a light adsorbent with a high specific surface area and lipophilicity. The graphene is a carbon material constructed by a monoatomic layer, and has excellent characteristics such as high specific surface area and mechanical strength, so that the graphene has a wide application prospect in the field of environmental protection. The graphene has extremely low adsorption energy to water, is easy to bend in water body to form a micron-nanometer coexisting rough interface structure, sp 2 Due to the existence of a monoatomic layer structure formed by connecting hybrid structures and pi-pi conjugation, graphene has good affinity to oil products and strong physical adsorption capacity to organic molecules, so that the graphene has oleophylic and hydrophobic characteristics.
The graphene porous material has the advantages of extremely low density, high porosity, large surface area and the like, and various pollutants are easy to enter and diffuse into the three-dimensional graphene network. In addition, its excellent adsorption properties, high hydrophobicity and recyclability make it an ideal oil-absorbing material. At present, the preparation method of the graphene aerogel material mainly comprises a CVD method, a template method, a reduction self-assembly method, a cross-linked gel method and the like. The former two methods are limited by the size of the template and the reaction vessel, and have high equipment cost, and the reaction needs to be carried out at high temperature, so that the method is not suitable for industrial preparation. The reduction self-assembly and cross-linking gel method has simple preparation process, does not need expensive equipment, and has more practical application significance (ZHao X, Yao W, Gao W, et al, Wet-round super elastic graphene aerogel milestones with group effect [ J ]. Advanced Materials,2017,29(35): 1701482.). And the preparation of the super-hydrophobic graphene aerogel generally needs a two-step method, and after a graphene three-dimensional assembly is obtained, surface hydrophobic modification is carried out (Wu J, Li H, Lai X, et al. connecting and super-hydrophobic F-rGO @ CNTs/chitosan aerogels for interfacial resistance sensor [ J ]. Chemical Engineering Journal,2020,386:123998.), the grafting temperature and the equipment limitation are high, and the process is complex. Therefore, a simple and scalable preparation method is crucial for practical applications.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide an elastic super-hydrophobic graphene gel sphere and a preparation method and application thereof.
The invention provides a method for preparing super-hydrophobic graphene aerogel through one-step crosslinking, and aims to solve the problem of adsorption and recovery of ocean oil spill and other organic pollutants.
The purpose of the invention is realized by at least one of the following technical solutions.
The preparation method of the elastic super-hydrophobic graphene gel ball provided by the invention comprises the following steps:
(1) dispersing graphene oxide in water to obtain a graphene oxide aqueous dispersion;
(2) dispersing hydrophobic amine in ethanol to obtain a gel bath;
(3) extruding the graphene oxide aqueous dispersion liquid obtained in the step (1) into the gel bath obtained in the step (2) to obtain graphene oxide gel spheres;
(4) and (3) heating the graphene oxide gel spheres obtained in the step (3) to perform heating treatment (heating to promote the internal gelation process), then performing drying treatment and annealing treatment to obtain the elastic super-hydrophobic graphene gel spheres.
Further, the dispersing mode in the step (1) is ultrasonic dispersing; the ultrasonic dispersion frequency is 45-55kHz, and the ultrasonic dispersion time is 5-10 min.
Further, in the graphene oxide aqueous dispersion liquid in the step (1), the concentration of the graphene oxide is 2-10 g/L.
Further, the graphene oxide in the step (1) may be prepared by a Hummers method, a Modified Hummers method, or an Improved Hummers method.
Further, the hydrophobic amine in the step (2) is one or more of alkylamine such as 1, 12-diaminododecane, undecamine, dodecylamine, tridecylamine, tetradecylamine, hexadecylamine, heptadecylamine, octadecylamine, etc.; the concentration of hydrophobic amine in the gelling bath is 0.5mM to 100 mM.
Further, in the step (3), the diameter of an extrusion opening for extruding the graphene oxide aqueous dispersion is 0.5-10 mm.
Preferably, in the step (3), the container for extruding the graphene oxide aqueous dispersion is a container with a dropping hole, a spraying hole and the like which can enable the graphene oxide aqueous dispersion to drop; the container for extruding the graphene oxide aqueous dispersion is equipment such as an injector, a spray head and a dropper, and the size and the shape of the gel ball can be controlled by adjusting the diameter of a dropping hole, the height of a pipe orifice and the dropping rate.
Further, the volume ratio of the graphene oxide aqueous dispersion liquid to the gel bath in the step (3) is 0.1-2: 1.
Further, the temperature of the heating treatment in the step (4) is 40-100 ℃, and the time of the heating treatment is 0.5-10 h.
Further, the annealing treatment in the step (4) is carried out under a protective atmosphere, wherein the protective atmosphere is a nitrogen atmosphere or an inert atmosphere; the temperature of the annealing treatment is 100-400 ℃, and the time of the annealing treatment is 30-120 min.
Preferably, the drying treatment in the step (4) comprises one of atmospheric drying, freeze drying and supercritical drying;
the invention provides an elastic super-hydrophobic graphene gel ball prepared by the preparation method.
The invention provides application of elastic super-hydrophobic graphene gel spheres in adsorption of organic pollutants.
According to the invention, graphene oxide aqueous dispersion is dripped into a coagulation bath containing a hydrophobic gelling agent to obtain a hydrophobically modified graphene oxide gel sphere, and the superhydrophobic graphene oxide gel sphere with good elasticity is obtained after drying treatment and annealing at a proper temperature. The elastic super-hydrophobic graphene gel spheres are obtained by a one-step crosslinking gel method.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the preparation method provided by the invention, specific graphene oxide precursor dispersion liquid and gel bath are preferably selected, and bonding and electrostatic interaction of amino, carboxyl and epoxy groups are utilized to form gel, so that the problem of the conventional two-step method for preparing the super-hydrophobic graphene aerogel is solved, the gel condition is simple and mild, the graphene oxide can be crosslinked to form gel at relatively low temperature, the preparation can be realized by means of conventional common equipment, the cost is low, and the industrial production can be realized; the data of the embodiment shows that the surface water contact angle of the elastic super-hydrophobic graphene gel sphere prepared by the invention reaches 153 degrees, the inner part of the elastic super-hydrophobic graphene gel sphere has a folded and porous structure, the structure provides a specific surface area for adsorbing organic matters, and the adsorption quantity of the elastic super-hydrophobic graphene gel sphere on the organic matters reaches 179g/g at most.
Drawings
FIG. 1 is an SEM micrograph of the interior of elastic superhydrophobic graphene gel spheres prepared in example 1;
FIG. 2 is a water contact angle of the elastic superhydrophobic graphene gel spheres prepared in example 1;
FIG. 3 is a graph showing the results of the adsorption amounts of organic solvents and oils by the elastic superhydrophobic graphene gel spheres prepared in example 1;
FIG. 4 is a stress-strain curve of the elastic superhydrophobic graphene gel spheres prepared in example 1.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
A preparation method of elastic super-hydrophobic graphene gel balls comprises the following steps:
(1) uniformly dispersing 120mg of graphene oxide in 24mL of deionized water by ultrasonic treatment, wherein the ultrasonic dispersion frequency is 53kHz, and the ultrasonic dispersion time is 10min, so as to obtain a graphene oxide water dispersion liquid with the concentration of 5 g/L;
(2) ultrasonic dispersing 240mg of octadecylamine in 60ml of absolute ethanol to obtain 14.84mM of hydrophobic amine gel bath;
(3) adding the graphene oxide aqueous dispersion obtained in the step (1) into a container capable of enabling the dispersion to be extruded and dripped, wherein the diameter of an extrusion opening is 8 mm;
(4) extruding and dripping the graphene oxide aqueous dispersion in the container in the step (3) into the gel bath of the hydrophobic amine in the step (2), wherein the volume ratio of the graphene oxide aqueous dispersion to the gel bath is 0.4: 1, heating at 70 ℃ for 8 hours, and completely replacing alcohol in the gel spheres with water to obtain graphene oxide gel spheres;
(5) placing the graphene oxide gel spheres in a refrigerator at the temperature of-20 ℃ for freezing, and then placing the graphene oxide gel spheres in a freeze dryer for drying to obtain dried graphene oxide gel spheres;
(6) and carrying out thermal annealing treatment on the dried graphene oxide gel spheres for 1h at 150 ℃ in a nitrogen atmosphere to obtain the elastic super-hydrophobic graphene gel spheres.
And (3) testing the adsorption capacity:
the adsorption test of the elastic super-hydrophobic graphene gel spheres on oil and organic pollutants is calculated by the following formula:
in the adsorption experiment, the initial elastic super-hydrophobic graphene gel ball is weighed by a balance, and the recorded mass is m 0 Putting the small ball into a beaker filled with organic matters, taking out the small ball after the small ball reaches saturated adsorption, weighing the small ball by a balance, and recording the mass m 1 In order to reduce errors as much as possible, the adsorption of the same organic substance was tested in triplicate.
According to adsorption tests, the elastic super-hydrophobic graphene gel spheres prepared in example 1 have excellent elasticity, hydrophobicity and high adsorbability.
Fig. 1 is an SEM micrograph of the interior of graphene aerogel spheres of example 1; as shown in FIG. 1, the pore structure inside the gel sphere is micron-sized, is arranged in an ordered layer, and has a rich wrinkle structure on the surface.
Fig. 2 is a surface water contact angle graph of the graphene aerogel sphere of example 1, as shown in the figure, the water contact angle of the graphene aerogel sphere reaches 153 ° under the surface contact angle instrument test.
Fig. 3 is an adsorption test chart of example 1, and as shown in the chart, the adsorption amount of the prepared graphene aerogel spheres to organic solvents such as ethanol, acetone, chloroform, pump oil and the like is 52-179g/g, and the adsorption amount to carbon tetrachloride is the highest and reaches 179 g/g.
Fig. 4 is a compression rebound graph of example 1, and the graphene aerogel spheres still maintain the complete shape after being compressed for five times under 70% strain, which shows that the graphene aerogel spheres have good elastic performance.
Example 2
A preparation method of elastic super-hydrophobic graphene gel balls comprises the following steps:
(1) uniformly dispersing 120mg of graphene oxide in 60mL of deionized water by ultrasonic, wherein the ultrasonic dispersion frequency is 53kHz, and the ultrasonic dispersion time is 10min to obtain a graphene oxide water dispersion liquid with the concentration of 2 g/L;
(2) ultrasonic dispersing 240mg of octadecylamine in 60ml of absolute ethanol to obtain 14.84mM of hydrophobic amine gel bath;
(3) adding the graphene oxide aqueous dispersion obtained in the step (1) into a container capable of enabling the dispersion to be extruded and dripped, wherein the diameter of an extrusion opening is 8 mm;
(4) extruding and dripping the graphene oxide aqueous dispersion in the container in the step (3) into the gel bath of the hydrophobic amine in the step (2), wherein the volume ratio of the graphene oxide aqueous dispersion to the gel bath is 1: 1, heating at 70 ℃ for 4 hours, and completely replacing alcohol in the gel spheres with water to obtain graphene oxide gel spheres;
(5) placing the graphene oxide gel spheres in a refrigerator at the temperature of-20 ℃ for freezing, and then placing the graphene oxide gel spheres in a freeze dryer for drying to obtain dried graphene oxide gel spheres;
(6) and carrying out thermal annealing treatment on the dried graphene oxide gel spheres for 1h at 150 ℃ in a nitrogen atmosphere to obtain the elastic super-hydrophobic graphene gel spheres.
And (3) testing the adsorption capacity:
the adsorption test of the elastic super-hydrophobic graphene gel spheres on oil and organic pollutants is calculated by the following formula:
in the adsorption experiment, the initial elastic super-hydrophobic graphene gel ball is weighed by a balance, and the recorded mass is m 0 Putting the small ball into a beaker filled with organic matters, taking out the small ball after the small ball reaches saturated adsorption, weighing the small ball by a balance, and recording the mass m 1 In order to reduce errors as much as possible, the adsorption of the same organic substance was tested in triplicate.
Through an adsorption test, the adsorption capacity of the superhydrophobic graphene aerogel spheres prepared in example 2 on organic solvents such as ethanol, acetone, chloroform and pump oil is 18-73g/g, as shown in fig. 3.
The elastic superhydrophobic graphene gel spheres prepared in example 2 also have micron-sized hole structures inside and abundant wrinkle structures on the surfaces, and can be seen in fig. 1.
The elastic superhydrophobic graphene gel spheres prepared in example 2 remained in an intact shape after five cycles of compression at 50% strain, as shown in fig. 4.
Example 3
A preparation method of elastic super-hydrophobic graphene gel balls comprises the following steps:
(1) uniformly dispersing 120mg of graphene oxide in 12mL of deionized water by ultrasonic, wherein the ultrasonic dispersion frequency is 53kHz, and the ultrasonic dispersion time is 10min, so as to obtain a graphene oxide aqueous dispersion solution with the concentration of 10 g/L;
(2) ultrasonically dispersing 240mg of octadecylamine in 60ml of absolute ethyl alcohol to obtain 14.84mM of hydrophobic amine gel bath, wherein the volume ratio of the graphene oxide aqueous dispersion to the gel bath is 0.2;
(3) adding the graphene oxide aqueous dispersion obtained in the step (1) into a container capable of enabling the dispersion to be extruded and dropped, wherein the diameter of an extrusion opening is 8 mm;
(4) extruding and dripping the graphene oxide aqueous dispersion in the container in the step (3) into the gel bath of the hydrophobic amine in the step (2), heating for 4h at 70 ℃, and completely replacing alcohol in the gel spheres with water to obtain graphene oxide gel spheres;
(5) placing the graphene oxide gel spheres in a refrigerator at the temperature of-20 ℃ for freezing, and then placing the graphene oxide gel spheres in a freeze dryer for drying to obtain dried graphene oxide gel spheres;
(6) and carrying out thermal annealing treatment on the dried graphene oxide gel spheres for 1h at 150 ℃ in a nitrogen atmosphere to obtain the elastic super-hydrophobic graphene gel spheres.
And (3) testing the adsorption capacity:
the adsorption test of the elastic super-hydrophobic graphene gel spheres on oil and organic pollutants is calculated by the following formula:
in the adsorption experiment, the initial elastic super-hydrophobic graphene gel ball is weighed by a balance, and the recorded mass is m 0 Putting the small ball into a beaker containing organic matters, taking out the small ball after the small ball reaches saturated adsorption, weighing the small ball by a balance, and recording the mass m 1 For reducing errors as much as possible, adsorption of the same organic substanceThe test was repeated three times.
Through an adsorption test, the adsorption capacity of the superhydrophobic graphene aerogel spheres prepared in example 3 on organic solvents such as ethanol, acetone, chloroform and pump oil is 27-95g/g, as shown in fig. 3.
The elastic superhydrophobic graphene gel spheres prepared in example 3 also have micron-sized hole structures inside and abundant wrinkle structures on the surfaces, and can be seen in fig. 1.
The elastic superhydrophobic graphene gel sphere prepared in example 3 maintains the complete shape after being compressed for five times under 70% strain, which can be seen in fig. 4.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (5)
1. A preparation method of elastic super-hydrophobic graphene gel balls is characterized by comprising the following steps:
(1) dispersing graphene oxide in water to obtain a graphene oxide aqueous dispersion;
in the graphene oxide aqueous dispersion liquid in the step (1), the concentration of graphene oxide is 2-10 g/L;
(2) dispersing hydrophobic amine in ethanol to obtain a gel bath;
the hydrophobic amine in the step (2) is more than one alkylamine of 1, 12-diaminododecane, undecamine, dodecylamine, tridecylamine, tetradecylamine, hexadecylamine, heptadecylamine and octadecylamine; the concentration of hydrophobic amine in the gel bath is 0.5mM-100 mM;
(3) extruding the graphene oxide aqueous dispersion liquid obtained in the step (1) into the gel bath obtained in the step (2) to obtain a graphene oxide gel ball solution;
in the step (3), the diameter of an extrusion opening for extruding the graphene oxide aqueous dispersion is 0.5-10 mm;
the volume ratio of the graphene oxide aqueous dispersion liquid to the gel bath in the step (3) is 0.1-2: 1;
(4) heating the graphene oxide gel sphere solution obtained in the step (3) for heating, drying the obtained graphene oxide gel spheres, and annealing to obtain the elastic super-hydrophobic graphene gel spheres; the temperature of the heating treatment is 70-100 ℃, and the time of the heating treatment is 0.5-10 h; the temperature of the annealing treatment is 100-400 ℃.
2. The method for preparing elastic superhydrophobic graphene gel spheres of claim 1, wherein the dispersion manner of the step (1) is ultrasonic dispersion; the ultrasonic dispersion frequency is 45-55kHz, and the ultrasonic dispersion time is 5-10 min.
3. The method for preparing elastic superhydrophobic graphene gel spheres of claim 1, wherein the annealing treatment of the step (4) is performed under a protective atmosphere, the protective atmosphere being a nitrogen atmosphere or an inert atmosphere; the time of the annealing treatment is 30min-120 min.
4. An elastic superhydrophobic graphene gel pellet prepared by the preparation method of any one of claims 1-3.
5. Use of the elastic superhydrophobic graphene gel spheres of claim 4 for adsorbing organic contaminants.
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