CN115025754A - Preparation method of patterned nitrogen and sulfur co-doped graphene aerogel - Google Patents
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Abstract
The invention provides a preparation method of a patterned nitrogen and sulfur co-doped graphene aerogel, and belongs to the technical field of graphene aerogel preparation. The preparation method is simple, the clothianidin hydrochloride or the rhodanine is used as a nitrogen source and a sulfur source and added into the graphene oxide dispersion liquid, a formed solid mixture is obtained through drying, and finally the patterned nitrogen-sulfur co-doped graphene is obtained through high-temperature reaction. After the oxidized graphene adsorbing rhodanine or clothianidin hydrochloride molecules is subjected to high-temperature action, not only is the doping of nitrogen and sulfur atoms realized, but also the structure of the graphene is partially recovered, the rapid synthesis of nitrogen and sulfur co-doped graphene under the condition of no metal catalyst is realized, and the product has high purity, large specific surface area and excellent adsorption performance.
Description
Technical Field
The invention relates to the technical field of graphene aerogel preparation, in particular to a preparation method of a patterned nitrogen and sulfur co-doped graphene aerogel.
Background
Graphene has chemical properties similar to graphite, and can adsorb and desorb various atoms and molecules. When the atoms or molecules are used as donors or acceptors, the concentration of graphene carriers can be changed, and graphene can keep good conductivity.
The graphene oxide is a layered material obtained by oxidizing graphite, after bulk phase graphite is treated by fuming concentrated acid solution, a graphene layer is oxidized into hydrophilic graphene oxide, and the distance between graphite layers is from before oxidationIs increased toThe separated graphene oxide lamellar structure is easily formed through a heating or ultrasonic stripping process in water. After oxidation treatment, the graphite oxide still maintains the layered structure of graphite, but a plurality of oxygen-based functional groups are introduced on each layer of graphene single sheet. The introduction of these oxygen-based functional groups makes the single graphene structure very complex.
Adopt nitrogen sulfur atom to dope graphite alkene, prepare nitrogen sulfur codope graphite alkene aerogel, can further improve its ability such as absorption, catalysis.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a patterned nitrogen and sulfur co-doped graphene aerogel, and the prepared nitrogen and sulfur co-doped graphene product has a relatively high application prospect in the fields of adsorption (water treatment, oil-water separation, gas adsorption), catalyst carriers, composite materials and the like.
The invention aims to provide a preparation method of a patterned nitrogen and sulfur co-doped graphene aerogel, which comprises the following steps:
(1) ultrasonically dispersing graphene oxide into water to obtain a graphene oxide dispersion liquid;
(2) adding the thiamine hydrochloride or rhodanine into the graphene oxide dispersion liquid obtained in the step (1), performing ultrasonic treatment until the graphene oxide dispersion liquid is completely dissolved, pouring the ultrasonic dispersion liquid into a container, and performing freeze drying in a vacuum freeze drying device for 24 hours to obtain a molded solid mixture;
(3) and (3) placing the solid mixture obtained in the step (2) in a high-temperature tube furnace, sealing and introducing nitrogen, heating the tube furnace to 600-800 ℃ according to the heating rate of 5 ℃/min, keeping the temperature for 0.5-2 h, and slowly cooling to room temperature to obtain the patterned nitrogen-sulfur co-doped graphene aerogel.
Preferably, the mass-to-volume ratio of the graphene oxide to the water in the step (1) is 1-2: 1 to 2.
Preferably, the mass ratio of the clothianidin hydrochloride or rhodanine to the graphene oxide in the graphene oxide dispersion liquid in the step (2) is 1: 50.
Preferably, the container in step (2) includes a cylindrical container, a cube-shaped container, and a rectangular parallelepiped-shaped container.
The structure of the graphene oxide adopted by the invention is as shown in formula (I), the structure of the nitrogen and sulfur co-doped graphene is as shown in formula (II), and the synthetic route is as follows:
compared with the prior art, the invention has the following beneficial effects: according to the invention, clothianidin hydrochloride or rhodanine is used as a nitrogen source and a sulfur source, added into graphene oxide dispersion liquid, dried to obtain a formed solid mixture, and subjected to high-temperature reaction to prepare the patterned nitrogen-sulfur co-doped graphene. The micro-morphology of the nitrogen and sulfur co-doped graphene is a typical two-dimensional layered structure, the sheet layer is basically transparent, a large number of folds exist, a large number of holes are reserved after freeze-drying, and the sizes are different, so that the specific surface area of the graphene is greatly increased, and the application research in the aspects of adsorption, catalysis and the like is facilitated.
The preparation method is simple, the graphene oxide adsorbing the rhodanine or the clothianidin hydrochloride molecules not only realizes the doping of nitrogen and sulfur atoms, but also partially recovers the structure of the graphene after the high-temperature action, realizes the rapid synthesis of the nitrogen and sulfur co-doped graphene under the condition of no metal catalyst, and has high product purity, large specific surface area and excellent adsorption performance.
Drawings
Fig. 1 is an X-ray diffraction pattern of a nitrogen and sulfur co-doped graphene aerogel in example 1;
fig. 2 is a scanning electron microscope image of the nitrogen and sulfur co-doped graphene aerogel in example 1;
fig. 3 is an EDX energy spectrum of the nitrogen and sulfur co-doped graphene aerogel in example 1;
fig. 4 is a cylindrical nitrogen and sulfur co-doped graphene aerogel prepared in example 1;
fig. 5 is a cubic nitrogen and sulfur co-doped graphene aerogel prepared in example 2;
fig. 6 is a cuboid-shaped nitrogen and sulfur co-doped graphene aerogel prepared in example 3.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of a patterned nitrogen and sulfur co-doped graphene aerogel comprises the following steps:
(1) weighing 50mg of graphite oxide, adding 50mL of water, and performing ultrasonic dispersion for 2 hours to obtain a graphene oxide dispersion liquid;
(2) then weighing 1.0g of thiamine hydrochloride, adding the thiamine hydrochloride into the graphene oxide dispersion liquid obtained in the step (1), and continuing ultrasonic treatment until the thiamine hydrochloride is completely dissolved; pouring the ultrasonic dispersion liquid into a cylindrical container, and placing the container in a vacuum freeze drying device for freeze drying for 24 hours to obtain a cylindrical solid mixture;
(3) and (3) placing the solid mixture obtained in the step (2) in a high-temperature tube furnace, hermetically introducing nitrogen, heating the tube furnace to 800 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 2h, and slowly cooling the tube furnace to room temperature to obtain the cylindrical nitrogen-sulfur co-doped graphene aerogel.
Example 2
A preparation method of a patterned nitrogen and sulfur co-doped graphene aerogel comprises the following steps:
(1) weighing 50mg of graphite oxide, adding 50mL of water, and performing ultrasonic dispersion for 2 hours to obtain a graphene oxide dispersion liquid;
(2) then weighing 1.0g of thiamine hydrochloride, adding the thiamine hydrochloride into the graphene oxide dispersion liquid obtained in the step (1), and continuing ultrasonic treatment until the thiamine hydrochloride is completely dissolved; pouring the ultrasonic dispersion liquid into a cubic container, and freeze-drying in a vacuum freeze-drying device for 24 hours to obtain a cubic solid mixture;
(3) and (3) placing the solid mixture obtained in the step (2) in a high-temperature tubular furnace, hermetically introducing nitrogen, heating the tubular furnace to 700 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 2 hours, and slowly cooling the tubular furnace to room temperature to obtain the cubic nitrogen and sulfur co-doped graphene aerogel.
Example 3
A preparation method of a patterned nitrogen and sulfur co-doped graphene aerogel comprises the following steps:
(1) weighing 50mg of graphite oxide, adding 50mL of water, and performing ultrasonic dispersion for 2 hours to obtain a graphene oxide dispersion liquid;
(2) then weighing 1.0g of thiamine hydrochloride, adding the thiamine hydrochloride into the graphene oxide dispersion liquid obtained in the step (1), and continuing ultrasonic treatment until the thiamine hydrochloride is completely dissolved; pouring the ultrasonic dispersion liquid into a cuboid container, and freeze-drying in a vacuum freeze-drying device for 24 hours to obtain a cuboid solid mixture;
(3) and (3) placing the solid mixture obtained in the step (2) in a high-temperature tube furnace, introducing nitrogen in a sealed manner, heating the tube furnace to 600 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 0.5h, and then slowly cooling the tube furnace to room temperature to obtain the cuboid-shaped nitrogen-sulfur co-doped graphene aerogel.
An X-ray diffraction pattern of the nitrogen and sulfur co-doped graphene aerogel prepared in example 1 is shown in fig. 1, and a characteristic diffraction peak of the nitrogen and sulfur co-doped graphene in fig. 1 is located near 26 °, and the peak is a characteristic peak of a (002) crystal face of a graphene material, which indicates that graphene oxide is reduced after a high-temperature reaction, and a structure of graphene is partially recovered. In addition, other diffraction peaks do not appear in the spectrum, which indicates that the synthesized nitrogen-sulfur co-doped graphene is a pure graphene product, does not contain any impurity, and has high product purity.
The scanning electron microscope image of the nitrogen and sulfur co-doped graphene aerogel prepared in example 1 is shown in fig. 2, and fig. 2 can visually observe the microscopic morphology of the nitrogen and sulfur co-doped graphene, which is a typical two-dimensional layered structure, the lamellar layer is substantially transparent, a large number of folds exist, a large number of holes are reserved after freeze-drying, and the sizes are different, so that the specific surface area is greatly increased, and the BET specific surface area is 115.7m 2 The concentration is/g, which is beneficial to the application research in the aspects of adsorption, catalysis and the like.
The elemental composition of the nitrogen and sulfur co-doped graphene aerogel prepared in example 1 was analyzed by EDX spectroscopy, and the results are shown in fig. 3 and table 1. In fig. 3, significant characteristic peaks of four elements of carbon, nitrogen, oxygen, and sulfur appear, and other impurity elements do not appear, which indicates that nitrogen and sulfur atoms successfully enter the graphene lattice, but the product still mainly contains carbon element, accounting for 77.6% (mass percent), and the nitrogen and sulfur contents are 10.8% and 6.6%, respectively. Therefore, after the oxidized graphene adsorbing the rhodanine or the clothianidin hydrochloride molecules is subjected to high-temperature action, not only is the doping of nitrogen and sulfur atoms realized, but also the structure of the graphene is partially recovered, the rapid synthesis of the nitrogen and sulfur co-doped graphene under the condition of no metal catalyst is realized, and the product has high purity, large specific surface area and excellent adsorption performance.
TABLE 1
Element(s) | By weight% | Atom% |
CK | 77.59 | 82.94 |
NK | 10.8 | 9.89 |
OK | 6.55 | 5.25 |
SK | 5.06 | 2.02 |
The cylindrical nitrogen and sulfur co-doped graphene aerogel prepared in example 1 is shown in fig. 4; the cubic-shaped nitrogen and sulfur co-doped graphene aerogel prepared in example 2 is shown in fig. 5; the cuboid-shaped nitrogen and sulfur co-doped graphene aerogel prepared in example 3 is shown in fig. 6.
In the embodiment of the invention, the proportion of the raw material graphite oxide and the raw material of the hydrochloric acid is variable, the hydrochloric acid is replaced by rhodanine molecules, the reaction temperature and the reaction time are adjustable, and the shape can be determined according to the shape of the mould.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. The preparation method of the patterned nitrogen and sulfur co-doped graphene aerogel is characterized by comprising the following steps of:
(1) ultrasonically dispersing graphene oxide into water to obtain a graphene oxide dispersion liquid;
(2) adding the thiamine hydrochloride or rhodanine into the graphene oxide dispersion liquid obtained in the step (1), performing ultrasonic treatment until the graphene oxide dispersion liquid is completely dissolved, pouring the ultrasonic dispersion liquid into a container, and performing freeze drying in a vacuum freeze drying device for 24 hours to obtain a formed solid mixture;
(3) and (3) placing the solid mixture obtained in the step (2) in a high-temperature tubular furnace, hermetically introducing nitrogen, heating the tubular furnace to 600-800 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 0.5-2 h, and then slowly cooling to room temperature to obtain the patterned nitrogen-sulfur co-doped graphene aerogel.
2. The preparation method of the patterned nitrogen and sulfur co-doped graphene aerogel according to claim 1, wherein the mass-to-volume ratio of the graphene oxide and water in the step (1) is 1-2: 1 to 2.
3. The preparation method of the patterned nitrogen and sulfur co-doped graphene aerogel according to claim 1, wherein the mass ratio of the thiaamine hydrochloride or rhodanine to the graphene oxide in the graphene oxide dispersion liquid in the step (2) is 1: 50.
4. The method for preparing the patterned nitrogen and sulfur co-doped graphene aerogel according to claim 1, wherein the container in the step (2) comprises a cylindrical container, a square container and a rectangular parallelepiped container.
5. The patterned nitrogen and sulfur co-doped graphene aerogel is characterized by being prepared according to the preparation method of any one of claims 1 to 4.
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