CN114149619A - Preparation method of graphene/cellulose composite material - Google Patents
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
Abstract
The invention relates to a preparation method of a graphene/cellulose composite material, which is characterized in that a graphene/cellulose composite material is prepared by partially reducing graphene oxide by ascorbic acid (VC) at a certain temperature, a cell crusher is used for crushing cells of a graphene oxide dispersion liquid prepared by the graphene oxide composite material, so that a uniformly dispersed graphene oxide dispersion liquid with a certain concentration is obtained, then the prepared cellulose is added to enable the graphene oxide dispersion liquid to be uniformly compounded with the graphene oxide, the uniformly compounded solution is preheated to remove bubbles and reach the reaction temperature in advance, the ascorbic acid (VC) is added to be heated and reduced, and the uniform graphene/cellulose composite material is obtained through hydrophobic association. The preparation method is simple in process and convenient to operate, the environment-friendly reducing agent is adopted, byproducts polluting the environment are not generated, the macroscopic preparation can be realized, and the dialyzed graphene/cellulose composite material can be directly used for photothermal conversion, heat conduction, electromagnetic shielding and the like.
Description
Technical Field
The invention belongs to the field of preparation of composite materials, and particularly relates to a preparation method of a graphene/cellulose composite material.
Background
The earth's surface is covered in 71% of its volume by the ocean, but seawater cannot be drunk directly. At present, the earth faces serious problems of water resource shortage, energy shortage, environmental deterioration and the like, so that the solar energy with clean and high efficiency is used for carrying out the photothermal evaporation seawater desalination and is of great interest.
Graphene as a new two-dimensional carbon nanomaterial consists of sp hybridized orbitals of carbon atoms, and has a unique nanosheet structure, so that the graphene has a plurality of excellent properties such as tensile strength, Young modulus, electrical conductivity, thermal conductivity, specific surface area, high barrier property and the like. With the gradual breakthrough of mass production and large-size problems, the industrial application of graphene is accelerating, and the application of graphene in the aspects of biology, composite materials, photosensitive elements, aerospace, hydrogen storage materials, seawater desalination, new energy and the like is more and more extensive. The research and application development of graphene is continuously increasing, and researchers with excellent performance and potential application value of materials related to graphite and graphene are dedicated to trying different methods in different fields to prepare high-quality large-area graphene materials. In interfacial solar evaporation, graphene can be an excellent absorber, absorbing sunlight and converting it into thermal energy by photoexcitation-electron scattering, thereby heating and evaporating water. An additional benefit of graphene with nanochannels is that it provides a path for water and steam to escape. Seawater desalination is achieved through a phase change process, and fresh water is collected through condensation. This technique has several major features: (1) it is completely made of solar energy (2) has extremely high ion removal efficiency; (3) the capital investment is low. All of this makes the technology very suitable as a portable device for use in developing countries and remote areas where infrastructure is scarce.
Cellulose nanocrystals are regions of cellulose fibers that are preferentially cut out of order by acid hydrolysis by mechanical and chemical treatments separated from the native cellulose. The cellulose nanocrystal exhibits excellent mechanical properties (e.g., young's modulus and tensile strength), high hydrophilicity and low thermal conductivity, and it is easy to surface-functionalize. At the time of acid hydrolysis, the initial degradation rate of disordered cellulose is fast, and the reaction is almost stopped when there is only a highly crystalline portion, reaching a so-called stationary polymerization stage. The obtained cellulose nanocrystal is in a rod-like shape, the diameter is 2-20 nm, and the length is 50-500 nm. CNC has a small aspect ratio (aspect ratio: 1-100) to CNF (aspect ratio: 15-300).
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a simple, easy, green and environment-friendly method for preparing the graphene/cellulose composite material, and expands the way for preparing the graphene composite material. The method adopts an ascorbic acid (VC) partial reduction method to prepare the graphene/cellulose composite material, has simple process, convenient operation and little pollution to the environment, and can realize macro preparation.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
a method for preparing a graphene/cellulose composite material is characterized in that a method for partially reducing graphene oxide by using a reducing agent at a certain temperature is used for preparing the graphene/cellulose composite material.
More specifically, the preparation method of the graphene/cellulose composite material comprises the following steps:
1) preparing a uniformly dispersed graphene oxide dispersion liquid with a certain concentration;
2) preparing cellulose nanocrystalline dispersion liquid with certain concentration by a sulfuric acid hydrolysis method;
3) uniformly mixing the graphene oxide dispersion liquid with the cellulose nanocrystal solution to obtain a mixed solution;
4) preheating the mixed solution;
5) adding a reducing agent for reduction reaction, and dialyzing in deionized water to obtain the graphene/cellulose composite material.
In a preferred embodiment of the present invention, in the step (1), the graphene oxide is prepared by a Hummers method, and the thickness of the graphene oxide is controlled to be 0.1-10 nm; preferably, a cell crusher is used for carrying out cell crushing on the prepared graphene oxide, and the graphene oxide is diluted to obtain a graphene oxide dispersion liquid with the concentration of 0.1-50 mg/ml, preferably 2-8 mg/ml; more preferably 5 mg/ml.
In a preferred embodiment of the invention, in the step (1), the preparation is carried out by a Hummer method, firstly, 10g of natural graphite and 10g of ground sodium nitrate are weighed and placed in a flask, a reaction device is placed in an ice-water bath, 300ml of concentrated sulfuric acid is added while stirring, 30g of potassium permanganate is added in 5 times, the ice bath is removed after stirring for half an hour, the temperature is raised to 35 ℃, the stirring is carried out for 6 hours, 400ml of deionized water is added dropwise, the temperature is raised, the system is kept at more than 95 ℃ for reaction for 15 minutes, the mixed solution in the flask is introduced into the flask filled with 1400ml of deionized water, 100ml of hydrogen peroxide is added dropwise to remove unreacted potassium permanganate until the solution is bright yellow, and the reaction is terminated; and standing the mixed suspension for a period of time, pouring out supernatant, adding hydrochloric acid for replacement twice, finally washing with a large amount of deionized water, and washing with a centrifugal machine for several times until the supernatant is neutral to obtain the graphene oxide solution.
In a preferred embodiment of the invention, in the step (2), the concentration of the cellulose nanocrystal solution is 1-20 mg/ml, preferably 4-10 mg/ml.
In the preferred embodiment of the invention, in the step (2), the cellulose nanocrystals are prepared by a sulfuric acid hydrolysis method, 4 parts of 10g of MCC are weighed, 4 parts of 100ml of 56% concentrated sulfuric acid is weighed, the MCC is slowly put into sulfuric acid, the sulfuric acid in a conical flask is continuously vibrated while the MCC is added, the MCC is prevented from caking in the conical flask, the subsequent hydrolysis is not easy, then hot water bath treatment is carried out, the water bath temperature is set to be 45 ℃, and the water bath time is 50min-60min until the MCC is completely hydrolyzed; washing the acid-treated sample with distilled water, centrifuging at 6000r/min for 5min, repeating twice, centrifuging at 14000r/min for 5min, repeating twice, and collecting supernatant; putting the sample obtained by the centrifugation in the previous step into a dialysis bag, soaking the sample in distilled water, changing water for 3 times every day, and dialyzing for 3 days; and (3) breaking cells of the dialyzed sample for 15min under 50% of power to obtain the cellulose nanocrystal dispersion.
In a preferred embodiment of the invention, in the step (3), the mass ratio of the graphene oxide to the cellulose nanocrystal is 2: 1-30: 1, and the mixture is stirred for 5-120 min, preferably 20-60 min.
In a preferred embodiment of the invention, in the step (4), the temperature of the preheating treatment is 30-100 ℃, preferably 60-90 ℃, and the preheating time is 20-120 min, preferably 30-60 min.
In a preferred embodiment of the present invention, in the step (5), the reducing agent is at least one of hydroiodic acid, hydrazine hydrate, citric acid, ascorbic acid, gluconic acid and ammonia water, preferably ascorbic acid (VC), and the mass ratio of the ascorbic acid to the graphene oxide is 4-7: 1; the temperature of the reduction reaction is 30-120 ℃, and preferably 60-90 ℃; the reduction time is 4h-11 h.
In a preferred embodiment of the present invention, in step (5), a dialysis treatment is performed in deionized water for 2 to 3 days to remove excess solvent and unreacted molecules.
Compared with the prior art, the graphene/cellulose composite material is prepared by a method of partially reducing graphene oxide by ascorbic acid (VC) at a certain temperature, firstly, a cell crusher is used for crushing cells of the prepared graphene oxide dispersion liquid to obtain uniformly dispersed graphene oxide dispersion liquid with a certain concentration, then, cellulose nanocrystals prepared by a sulfuric acid hydrolysis method are added to be uniformly compounded with graphene oxide, the uniformly compounded solution is preheated to remove bubbles and reach a reaction temperature in advance, ascorbic acid (VC) is added to be heated and reduced, and the uniform graphene/cellulose composite material is obtained through hydrophobic association. The preparation method is simple in process and convenient to operate, the environment-friendly reducing agent is adopted, byproducts polluting the environment are not generated, the macroscopic preparation can be realized, and the dialyzed graphene/cellulose composite material can be directly used for photothermal conversion, heat conduction, electromagnetic shielding and the like.
Drawings
The invention will be further described with reference to the accompanying drawings, which are only schematic illustrations and illustrations of the invention, and do not limit the scope of the invention.
Fig. 1 is a flow chart of the preparation of the graphene/cellulose composite material of the present invention;
FIG. 2 is a scanning electron microscope image of graphene/cellulose prepared by the method of the present invention;
FIG. 3 is a scanning electron microscope image of graphene/cellulose prepared by the method of the present invention;
FIG. 4 is an X-ray photoelectron spectrum of the graphene/cellulose composite material prepared by the method of the present invention;
FIG. 5 is a pictorial representation of a graphene/cellulose composite material prepared by the method of the present invention;
FIG. 6 is an infrared spectrum of a graphene/cellulose composite prepared by the method of the present invention;
FIG. 7 shows the intensity of sunlight (1 kW/m) of graphene/cellulose composite material prepared by the method of the present invention and pure water2) Graph of performance of the light evaporation test under.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
Example 1
Step 1: preparing graphene oxide dispersion liquid by a Hummers method, carrying out cell disruption on the prepared graphene oxide for 10min by using a cell disruptor, and diluting to obtain the graphene oxide dispersion liquid with the concentration of 4mg/ml and the thickness of 0.1-10 nm;
step 2: preparing cellulose nanocrystalline dispersion liquid by a sulfuric acid hydrolysis method, and performing cell disruption on the prepared cellulose nanocrystalline for 15min by using a cell disruptor, wherein the concentration of the cellulose nanocrystalline is prepared to be 6 mg/ml;
and step 3: mixing the graphene oxide and the cellulose nanocrystal in a mass ratio of 2:1, and stirring for 10min to obtain a uniformly dispersed mixed solution;
and 4, step 4: preheating the mixed solution in an oven at 70 ℃ for 30 min;
and 5: adding ascorbic acid for reduction reaction, adding ascorbic acid according to the mass ratio of the ascorbic acid to the graphene oxide of 5:1, reacting for 4 hours in a 70 ℃ oven, and dialyzing in deionized water for 2 days to obtain the graphene/cellulose composite material.
Example 2
Step 1: preparing graphene oxide dispersion liquid by a Hummers method; carrying out cell disruption on the prepared graphene oxide by using a cell disruptor for 10min, and diluting to obtain graphene oxide dispersion liquid with the concentration of 4mg/ml and the thickness of 0.1-10 nm;
step 2: preparing cellulose nanocrystalline dispersion liquid by a sulfuric acid hydrolysis method, and performing cell disruption on the prepared cellulose nanocrystalline for 15min by using a cell disruptor, wherein the concentration of the cellulose nanocrystalline is prepared to be 6 mg/ml;
and step 3: mixing the graphene oxide and the cellulose nanocrystal in a mass ratio of 5:1, and stirring for 10min to obtain a uniformly dispersed mixed solution;
and 4, step 4: preheating the mixed solution in an oven at 70 ℃ for 30 min;
and 5: adding ascorbic acid in a mass ratio of the ascorbic acid to the graphene oxide of 5:1, reacting for 4 hours in a drying oven at 70 ℃, and performing dialysis treatment in deionized water for 2 days to obtain the graphene/cellulose composite material.
Example 3
Step 1: preparing graphene oxide dispersion liquid by a Hummers method; carrying out cell disruption on the prepared graphene oxide by using a cell disruptor for 10min, and diluting to obtain graphene oxide dispersion liquid with the concentration of 4mg/ml and the thickness of 0.1-10 nm;
step 2: preparing cellulose nanocrystalline dispersion liquid by a sulfuric acid hydrolysis method, and performing cell disruption on the prepared cellulose nanocrystalline for 15min by using a cell disruptor, wherein the concentration of the cellulose nanocrystalline is prepared to be 6 mg/ml;
and step 3: mixing graphene oxide and cellulose nanocrystal in a mass ratio of 10:1, and stirring for 10min to obtain a uniformly dispersed mixed solution;
and 4, step 4: preheating the mixed solution in an oven at 70 ℃ for 30 min;
and 5: adding ascorbic acid in a mass ratio of the ascorbic acid to the graphene oxide of 5:1, reacting for 4 hours in a drying oven at 70 ℃, and performing dialysis treatment in deionized water for 2 days to obtain the graphene/cellulose composite material.
Example 4
Step 1: preparing graphene oxide dispersion liquid by a Hummers method; carrying out cell disruption on the prepared graphene oxide by using a cell disruptor for 10min, and diluting to obtain graphene oxide dispersion liquid with the concentration of 4mg/ml and the thickness of 0.1-10 nm;
step 2: preparing cellulose nanocrystalline dispersion liquid by a sulfuric acid hydrolysis method, and performing cell disruption on the prepared cellulose nanocrystalline for 15min by using a cell disruptor, wherein the concentration of the cellulose nanocrystalline is prepared to be 6 mg/ml;
and step 3: mixing the graphene oxide and the cellulose nanocrystal in a mass ratio of 20:1, and stirring for 10min to obtain a uniformly dispersed mixed solution;
and 4, step 4: preheating the mixed solution in an oven at 70 ℃ for 30 min;
and 5: adding ascorbic acid in a mass ratio of the ascorbic acid to the graphene oxide of 5:1, reacting for 4 hours in a drying oven at 70 ℃, and performing dialysis treatment in deionized water for 2 days to obtain the graphene/cellulose composite material.
Example 5
Step 1: preparing graphene oxide dispersion liquid by a Hummers method; carrying out cell disruption on the prepared graphene oxide by using a cell disruptor for 10min, and diluting to obtain graphene oxide dispersion liquid with the concentration of 4mg/ml and the thickness of 0.1-10 nm;
step 2: preparing cellulose nanocrystalline dispersion liquid by a sulfuric acid hydrolysis method, and performing cell disruption on the prepared cellulose nanocrystalline for 15min by using a cell disruptor, wherein the concentration of the cellulose nanocrystalline is prepared to be 6 mg/ml;
and step 3: mixing the graphene oxide and the cellulose nanocrystal in a mass ratio of 30:1, and stirring for 10min to obtain a uniformly dispersed mixed solution;
and 4, step 4: preheating the mixed solution in an oven at 70 ℃ for 30 min;
and 5: adding ascorbic acid in a mass ratio of the ascorbic acid to the graphene oxide of 5:1, reacting for 4 hours in a drying oven at 70 ℃, and performing dialysis treatment in deionized water for 2 days to obtain the graphene/cellulose composite material.
Example 6
Step 1: preparing graphene oxide dispersion liquid by a Hummers method; carrying out cell disruption on the prepared graphene oxide by using a cell disruptor for 10min, and diluting to obtain graphene oxide dispersion liquid with the concentration of 4mg/ml and the thickness of 0.1-10 nm;
step 2: preparing cellulose nanocrystalline dispersion liquid by a sulfuric acid hydrolysis method, and performing cell disruption on the prepared cellulose nanocrystalline for 15min by using a cell disruptor, wherein the concentration of the cellulose nanocrystalline is prepared to be 6 mg/ml;
and step 3: mixing graphene oxide and cellulose nanocrystal in a mass ratio of 10:1, and stirring for 10min to obtain a uniformly dispersed mixed solution;
and 4, step 4: preheating the mixed solution in an oven at 70 ℃ for 30 min;
and 5: adding ascorbic acid in a mass ratio of 10:1 of ascorbic acid to graphene oxide, reacting for 9 hours in a 70 ℃ oven, and dialyzing in deionized water for 2 days to obtain the graphene/cellulose composite material.
The preparation flow chart of the graphene/cellulose composite material is shown in fig. 1. Fig. 2 and 3 are scanning electron micrographs of the prepared graphene/cellulose composite material, which can be seen to have countless randomly distributed micron-sized pores. Fig. 4 is an X-ray photoelectron spectrum of the graphene/cellulose composite material prepared by the method of the present invention, and characteristic absorption peaks C, O, N of graphene oxide, graphene and the graphene/cellulose composite material can be respectively seen. Fig. 5 is a physical diagram of the graphene/cellulose composite material prepared by the method of the present invention, which can bear the weight of 200 g. FIG. 6 shows an IR spectrum of a graphene/cellulose composite material prepared by the method of the present inventionIn the figure, compared with graphene oxide, the graphene/cellulose composite material has a red-shift of a hydroxyl stretching peak, which proves that hydrogen bonds are formed between oxygen-containing functional groups of graphene and cellulose, and the system is more stable. FIG. 7 shows the intensity of sunlight (1 kW/m) of graphene/cellulose composite material prepared by the method of the present invention and pure water2) The performance curve of the illumination evaporation test shows that the evaporation rate of the graphene/cellulose composite material is 5.3 times that of pure water.
The invention has been described in an illustrative manner, and it is to be understood that the invention is not limited in its implementation to the details of construction and to the arrangements of the components set forth in the description, but is capable of equivalent embodiments or modifications, such as combinations of features, divisions or repetitions, or application of the concepts and arrangements of the invention without modification in other applications, all without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a graphene/cellulose composite material is characterized in that the graphene/cellulose composite material is prepared by a method of partially reducing graphene oxide by using a reducing agent at a certain temperature.
2. The method of claim 1, comprising the steps of:
1) preparing a uniformly dispersed graphene oxide dispersion liquid with a certain concentration;
2) preparing cellulose nanocrystalline dispersion liquid with certain concentration by a sulfuric acid hydrolysis method;
3) uniformly mixing the graphene oxide dispersion liquid with the cellulose nanocrystal solution to obtain a mixed solution;
4) preheating the mixed solution;
5) adding a reducing agent for reduction reaction, and dialyzing in deionized water to obtain the graphene/cellulose composite material.
3. The preparation method according to claim 2, wherein in the step (1), the graphene oxide dispersion liquid is prepared by a Hummers method, and the thickness of the graphene oxide is controlled to be 0.4-10 nm; preferably, a cell crusher is used for carrying out cell crushing on the prepared graphene oxide, and the graphene oxide is diluted to obtain a graphene oxide dispersion liquid with the concentration of 0.1-50 mg/ml, preferably 2-8 mg/ml; more preferably 5 mg/ml.
4. The preparation method according to claim 3, characterized in that in step (1), the preparation is carried out by a Hummer method, wherein 10g of natural graphite and 10g of ground sodium nitrate are weighed and placed in a flask, a reaction device is placed in an ice-water bath, 300ml of concentrated sulfuric acid is added while stirring, 30g of potassium permanganate is added in 5 times, the ice bath is removed after stirring for half an hour, the temperature is raised to 35 ℃, the stirring is carried out for 6 hours, 400ml of deionized water is added dropwise, the temperature is raised, the final system is kept at more than 95 ℃ for reaction for 15 minutes, the mixed solution in the flask is introduced into the flask containing 1400ml of deionized water, 100ml of hydrogen peroxide is added dropwise to remove unreacted potassium permanganate until the solution is bright yellow, and the reaction is terminated; and standing the mixed suspension for a period of time, pouring out supernatant, adding hydrochloric acid for replacement twice, finally washing with a large amount of deionized water, and washing with a centrifugal machine for several times until the supernatant is neutral to obtain the graphene oxide solution.
5. The preparation method according to claim 2, wherein in the step (2), the concentration of the cellulose nanocrystal solution is 1-20 mg/ml, preferably 4-10 mg/ml.
6. The preparation method according to claim 5, wherein in the step (2), the cellulose nanocrystals are prepared by a sulfuric acid hydrolysis method, wherein 4 parts of 10g of MCC is weighed, 4 parts of 100ml of 56% concentrated sulfuric acid is weighed, the MCC is slowly added into the sulfuric acid, the sulfuric acid in the conical flask is continuously vibrated while the MCC is added, the MCC is prevented from caking in the MCC, so that the MCC is not easily hydrolyzed later, and then hot water bath treatment is performed, wherein the water bath temperature is set to be 45 ℃ and the water bath time is 50min to 60min until the MCC is completely hydrolyzed; washing the acid-treated sample with distilled water, centrifuging at 6000r/min for 5min, repeating twice, centrifuging at 14000r/min for 5min, repeating twice, and collecting supernatant; putting the sample obtained by the centrifugation in the previous step into a dialysis bag, soaking the sample in distilled water, changing water for 3 times every day, and dialyzing for 3 days; and (3) ultrasonically crushing the dialyzed sample for 15min under 50% of power to obtain the cellulose nanocrystal dispersion.
7. The preparation method according to claim 2, wherein in the step (3), the mass ratio of the graphene oxide to the cellulose nanocrystal is 2: 1-30: 1, and the mixture is stirred for 5-120 min, preferably 20-60 min.
8. The preparation method according to claim 2, wherein in the step (4), the temperature of the preheating treatment is 30 to 100 ℃, preferably 60 to 90 ℃, and the preheating time is 20 to 120min, preferably 30 to 60 min.
9. The preparation method according to claim 2, wherein in the step (5), the reducing agent is at least one of hydroiodic acid, hydrazine hydrate, citric acid, ascorbic acid, gluconic acid and ammonia water, preferably ascorbic acid (VC), and the mass ratio of the ascorbic acid to the graphene oxide is 4-7: 1; the temperature of the reduction reaction is 30-120 ℃, and preferably 60-90 ℃; the reduction time is 4h-11 h.
10. The method according to claim 2, wherein in the step (5), the dialysis treatment is performed in deionized water for 2 to 3 days to remove excess solvent and unreacted molecules.
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| CN116554556A (en) * | 2023-05-06 | 2023-08-08 | 华南理工大学 | Cellulose nanocrystalline-reduced graphene oxide composite membrane and preparation method and application thereof |
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Inventor after: Li Xiaofeng Inventor after: Ma Zaiyuan Inventor after: Li Wei Inventor after: Hu Chen Inventor after: Yu Zhongzhen Inventor before: Li Xiaofeng Inventor before: Li Wei Inventor before: Hu Chen Inventor before: Yu Zhongzhen |
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