CN113621167A - Cellulose-graphene porous composite aerogel and preparation method thereof - Google Patents
Cellulose-graphene porous composite aerogel and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of composite materials, and particularly relates to a cellulose-graphene porous composite aerogel and a preparation method thereof. When the product is prepared, according to parts by weight, 80-100 parts of cellulose, 0.5-1.5 parts of graphene oxide with the particle size distribution range of 5-20nm and 2-5 parts of reduced graphene with the particle size distribution range of 100-500nm are taken in sequence; dissolving cellulose in ionic liquid to obtain ionic liquid solution of the cellulose; adding oxidized graphene and reduced graphene into the ionic liquid solution of cellulose, carrying out ultrasonic dispersion uniformly, and dialyzing by using deionized water to remove the ionic liquid to obtain composite hydrogel; and (4) freeze-drying the obtained composite hydrogel to obtain the product. In the product obtained by the invention, the graphene material is uniformly dispersed, and a better reinforcing effect can be achieved by a smaller addition amount.
Description
Technical Field
The invention belongs to the technical field of composite materials. More particularly, relates to a cellulose-graphene porous composite aerogel and a preparation method thereof.
Background
The cellulose aerogel is a novel high polymer material prepared by taking cellulose as a matrix. As a biomass-based aerogel material, the cellulose aerogel has the characteristics of high specific area and high porosity of the traditional aerogel materials, and has the special advantages of the cellulose aerogel, such as excellent biocompatibility and degradability. The advantages enable the cellulose aerogel to have wide research value and application prospect in the field of reinforcing and adsorbing materials. The pure cellulose aerogel has the advantages that the porosity of the pure cellulose aerogel cannot be further improved due to the hydrogen bond combination between cellulose molecular chains and the mechanical interweaving acting force, and an internal microporous structure is easily damaged when external pressure is applied to the pure cellulose aerogel, so that the stress hardening phenomenon is caused. Therefore, the cellulose is compounded with the material with special properties, so that the mechanical property of the cellulose aerogel can be enhanced, and a new function can be endowed to the cellulose aerogel, such as a selectively adsorbed cellulose ultra-light material.
Graphene is a single-layer graphite material, the crystal lattice of the graphene material is a two-dimensional honeycomb structure formed by carbon atoms, and the graphene material has super-strong mechanical properties, and the special single-layer structure enables the graphene to have unique physical and chemical properties.
At present, scholars at home and abroad prepare cellulose/graphene composite aerogel, hydrogel and film in different systems by using different cellulose and cellulose derivative materials, and the cellulose/graphene composite aerogel, hydrogel and film are applied to functional materials such as electric conduction, adsorption, reinforcement and the like. At present, the problems of weak physical strength and non-uniform dispersion of graphene still exist in the development and application of cellulose/graphene composite functional materials.
Disclosure of Invention
The invention aims to overcome the defect and deficiency that the overall physical strength of a product cannot be further improved because graphene cannot be uniformly distributed in a matrix in the actual preparation process of the existing cellulose-graphene composite functional material, and provides a cellulose-graphene porous composite aerogel and a preparation method thereof.
The invention aims to provide a cellulose-graphene porous composite aerogel.
The invention also aims to provide a preparation method of the cellulose-graphene porous composite aerogel.
The above purpose of the invention is realized by the following technical scheme:
the cellulose-graphene porous composite aerogel comprises the following raw materials in parts by weight:
80-100 parts of cellulose, 0.5-1.5 parts of graphene oxide with the particle size distribution range of 5-20nm and 2-5 parts of reduced graphene with the particle size distribution range of 100-500 nm;
at least a portion of the cellulose and at least a portion of the graphene oxide are intercalated between adjacent lamellar structures of the reduced graphene to form a sandwich structure.
According to the technical scheme, the graphene oxide with small particle size and the reduced graphene with relatively large particle size are introduced into the cellulose aerogel matrix, wherein the number of hydroxyl and carboxyl in the molecular structure of the reduced graphene is relatively small, the number of the groups in the graphene oxide is relatively large, and the conjugated region of the graphene can be influenced by pi-pi accumulation action force, so that the graphene oxide with small particle size is influenced by the pi-pi accumulation action force of the reduced graphene with large particle size to be dispersed among the reduced graphene layers, the hydroxyl on the surface of the cellulose and the hydroxyl and carboxyl on the surface of the graphene oxide form hydrogen bonds, thus a continuous lamellar structure can be constructed by the reduced graphene with large particle size, the adjacent large lamellar reduced graphene is connected by utilizing the interaction between the graphene oxide with small particle size and the cellulose, and a three-dimensional continuous network structure is formed, therefore, the problem of dispersion of the graphene oxide in the matrix is solved by using the graphene oxide and the reduced graphene with different sizes and different properties, and the mechanical property of the product is considered.
Further, the cellulose molecular structure comprises aldehyde functional groups.
Aldehyde functional groups are introduced into a cellulose molecular structure, and the activity of the aldehyde functional groups is utilized to generate aldol condensation reaction with hydroxyl in a system at a certain probability, so that chemical bonding is formed, the cohesive strength of an aerogel product is further improved, and the structural stability of the product is guaranteed.
Further, the graphene oxide is obtained by spray drying of a graphene oxide aqueous solution.
Furthermore, the graphene oxide aqueous solution comprises 0.3-0.5% of glycerol and 0.3-0.5% of ethylene glycol.
According to the technical scheme, the graphene oxide is subjected to spray drying treatment, in the spray drying process, moisture evaporation caused by the mechanical action force of spraying and the instantaneous temperature is received, the graphene lamellar structure is wrinkled to a certain degree, so that the specific surface area of the graphene oxide is improved, and meanwhile, as the surface becomes wrinkled and rough, the fibrous structure of cellulose is more easily intertwined on the surface, so that physical winding is formed, and the mechanical property of an aerogel product is further improved;
and the introduction of glycerol and glycol can adjust the evaporation rate of water molecules in the spray drying process, so that the wrinkle degree of the graphene oxide can be adjusted, and agglomeration caused by overlarge interaction force of small-particle graphene after the specific surface area of the small-particle graphene is excessively increased is avoided.
A preparation method of cellulose-graphene porous composite aerogel comprises the following specific preparation steps:
according to the weight portion, 80-100 portions of cellulose, 0.5-1.5 portions of oxidized graphene with the particle size distribution range of 5-20nm and 2-5 portions of reduced graphene with the particle size distribution range of 100-500nm are taken in sequence;
dissolving cellulose in ionic liquid to obtain ionic liquid solution of the cellulose;
adding oxidized graphene and reduced graphene into the ionic liquid solution of cellulose, carrying out ultrasonic dispersion uniformly, and dialyzing by using deionized water to remove the ionic liquid to obtain composite hydrogel;
and (4) freeze-drying the obtained composite hydrogel to obtain the product.
Further, the specific preparation steps further comprise:
pretreating cellulose: mixing cellulose and sodium periodate solution, heating and stirring for reaction, filtering, washing and drying to obtain pretreated cellulose;
and after the obtained composite hydrogel is freeze-dried, heating and dehydrating for 25-30min at the temperature of 85-90 ℃ to obtain the product.
Further, the specific preparation steps further comprise:
pretreating graphene oxide: dispersing graphene oxide with the particle size distribution range of 5-20nm in deionized water to form a graphene oxide aqueous solution, adding glycerol accounting for 0.3-0.5% of the mass of the graphene oxide aqueous solution and ethylene glycol accounting for 0.3-0.5% of the mass of the graphene oxide aqueous solution into the graphene oxide aqueous solution, uniformly dispersing, and performing spray drying to obtain the pretreated graphene oxide.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1
Mixing graphene oxide with the particle size distribution range of 5-20nm and deionized water according to the mass ratio of 1: 8, performing ultrasonic dispersion for 10min under the ultrasonic frequency of 55kHz to form a graphene oxide aqueous solution, adding glycerol accounting for 0.3% of the mass of the graphene oxide aqueous solution and ethylene glycol accounting for 0.3% of the mass of the graphene oxide aqueous solution into the graphene oxide aqueous solution, continuing performing ultrasonic dispersion for 10min to obtain a dispersion liquid, transferring the dispersion liquid into a spray dryer, and performing spray drying at the air inlet temperature of 120 ℃ and the air outlet temperature of 90 ℃ to obtain pretreated graphene oxide;
reducing graphene oxide and an ascorbic acid solution, and screening reduced graphene with the particle size distribution range of 100-500 nm;
pretreating cellulose: mixing cellulose and sodium periodate solution with the mass fraction of 5%, heating and stirring for reaction for 2 hours at the temperature of 75 ℃ and the rotating speed of 300r/min, and then filtering, washing and drying to obtain pretreated cellulose;
according to the weight portion, sequentially taking 80 portions of pretreated cellulose, 0.5 portion of pretreated graphene oxide with the particle size distribution range of 5-20nm and 2 portions of reduced graphene with the particle size distribution range of 100-500 nm;
firstly, pretreating cellulose and ionic liquid according to a mass ratio of 1: 10, mixing and dissolving to obtain an ionic liquid solution of cellulose, adding pretreated graphene oxide and reduced graphene into the ionic liquid solution of cellulose, ultrasonically dispersing for 20min at the frequency of 60kHz, and dialyzing by using deionized water to remove the ionic liquid to obtain the composite hydrogel;
and (3) carrying out vacuum freeze drying on the obtained composite hydrogel under the conditions that the vacuum degree is 80Pa and the temperature is-60 ℃ to obtain dry aerogel, transferring the obtained dry aerogel into an oven, and carrying out heating dehydration for 25min under the condition that the temperature is 85 ℃ to obtain the product.
Example 2
Mixing graphene oxide with the particle size distribution range of 10-20nm and deionized water according to the mass ratio of 1: 9, after mixing, performing ultrasonic dispersion for 20min under the condition that the ultrasonic frequency is 60kHz to form a graphene oxide aqueous solution, adding glycerol accounting for 0.4% of the mass of the graphene oxide aqueous solution and ethylene glycol accounting for 0.4% of the mass of the graphene oxide aqueous solution into the graphene oxide aqueous solution, continuing performing ultrasonic dispersion for 15min to obtain a dispersion liquid, transferring the dispersion liquid into a spray dryer, and performing spray drying at the air inlet temperature of 125 ℃ and the air outlet temperature of 95 ℃ to obtain pretreated graphene oxide;
reducing graphene oxide and an ascorbic acid solution, and screening reduced graphene with the particle size distribution range of 400-500 nm;
pretreating cellulose: mixing cellulose and 8% sodium periodate solution, heating and stirring for reaction for 3 hours at the temperature of 78 ℃ and the rotating speed of 400r/min, filtering, washing and drying to obtain pretreated cellulose;
according to the weight portion, sequentially taking 90 portions of pretreated cellulose, 0.8 portion of pretreated graphene oxide with the particle size distribution range of 10-20nm and 3 portions of reduced graphene with the particle size distribution range of 400-500 nm;
firstly, pretreating cellulose and ionic liquid according to a mass ratio of 1: 15, mixing and dissolving to obtain an ionic liquid solution of cellulose, adding pretreated graphene oxide and reduced graphene into the ionic liquid solution of cellulose, ultrasonically dispersing for 30min at the frequency of 70kHz, and dialyzing by using deionized water to remove the ionic liquid to obtain the composite hydrogel;
and (3) carrying out vacuum freeze drying on the obtained composite hydrogel under the conditions that the vacuum degree is 100Pa and the temperature is-70 ℃ to obtain dry aerogel, transferring the obtained dry aerogel into an oven, and carrying out heating dehydration for 26min under the condition that the temperature is 88 ℃ to obtain the product.
Example 3
Mixing graphene oxide with the particle size distribution range of 5-20nm and deionized water according to the mass ratio of 1: 10, performing ultrasonic dispersion for 40min under the condition that the ultrasonic frequency is 65kHz to form a graphene oxide aqueous solution, adding glycerol accounting for 0.5% of the mass of the graphene oxide aqueous solution and ethylene glycol accounting for 0.5% of the mass of the graphene oxide aqueous solution into the graphene oxide aqueous solution, continuing performing ultrasonic dispersion for 20min to obtain a dispersion liquid, transferring the dispersion liquid into a spray dryer, and performing spray drying at the air inlet temperature of 140 ℃ and the air outlet temperature of 100 ℃ to obtain pretreated graphene oxide;
reducing graphene oxide and an ascorbic acid solution, and screening reduced graphene with the particle size distribution range of 100-500 nm;
pretreating cellulose: mixing cellulose and a sodium periodate solution with the mass fraction of 10%, heating, stirring and reacting for 4 hours at the temperature of 85 ℃ and the rotating speed of 500r/min, and then filtering, washing and drying to obtain pretreated cellulose;
according to the weight portion, sequentially taking 100 portions of pretreated cellulose, 1.5 portions of pretreated graphene oxide with the particle size distribution range of 5-20nm and 5 portions of reduced graphene with the particle size distribution range of 100-500 nm;
firstly, pretreating cellulose and ionic liquid according to a mass ratio of 1: 20, mixing and dissolving to obtain an ionic liquid solution of cellulose, adding pretreated graphene oxide and reduced graphene into the ionic liquid solution of cellulose, ultrasonically dispersing for 40min at the frequency of 80kHz, and dialyzing by using deionized water to remove the ionic liquid to obtain the composite hydrogel;
and (3) carrying out vacuum freeze drying on the obtained composite hydrogel under the conditions that the vacuum degree is 120Pa and the temperature is-80 ℃ to obtain dry aerogel, transferring the obtained dry aerogel into an oven, and carrying out heating dehydration for 30min under the condition that the temperature is 90 ℃ to obtain the product.
Example 4
This example differs from example 1 in that: the sodium periodate solution is replaced by deionized water with equal mass, and the rest conditions are kept unchanged.
Example 5
This example differs from example 1 in that: glycerol and ethylene glycol were not added and the remaining conditions were kept constant.
Example 6
Reducing graphene oxide and an ascorbic acid solution, and screening reduced graphene with the particle size distribution range of 100-500 nm;
pretreating cellulose: mixing cellulose and sodium periodate solution with the mass fraction of 5%, heating and stirring for reaction for 2 hours at the temperature of 75 ℃ and the rotating speed of 300r/min, and then filtering, washing and drying to obtain pretreated cellulose;
according to the weight portion, 80 portions of pretreated cellulose, 0.5 portion of graphene oxide with the particle size distribution range of 5-20nm and 2 portions of reduced graphene with the particle size distribution range of 100-500nm are taken in sequence;
firstly, pretreating cellulose and ionic liquid according to a mass ratio of 1: 10, mixing and dissolving to obtain an ionic liquid solution of cellulose, adding graphene oxide and reduced graphene into the ionic liquid solution of cellulose, ultrasonically dispersing for 20min at the frequency of 60kHz, and dialyzing by using deionized water to remove the ionic liquid to obtain the composite hydrogel;
and (3) carrying out vacuum freeze drying on the obtained composite hydrogel under the conditions that the vacuum degree is 80Pa and the temperature is-60 ℃ to obtain dry aerogel, transferring the obtained dry aerogel into an oven, and carrying out heating dehydration for 25min under the condition that the temperature is 85 ℃ to obtain the product.
Comparative example 1
This comparative example differs from example 1 in that: reduced graphene is not added, and the rest conditions are kept unchanged.
Comparative example 2
This comparative example differs from example 1 in that: graphene oxide is not added, and the rest conditions are kept unchanged.
Comparative example 3
This comparative example differs from example 1 in that: reduced graphene with the same mass and the particle size distribution range of 5-20nm is adopted to replace the oxidized graphene, and the rest conditions are kept unchanged.
Comparative example 4
This comparative example differs from example 1 in that: the reduced graphene is replaced by the oxidized graphene with the equal mass and the particle size distribution range of 100-500nm, and the rest conditions are kept unchanged.
The products obtained in examples 1 to 6 and comparative examples 1 to 4 were subjected to performance tests, the specific test methods and test results are as follows:
and (3) detecting the mechanical strength: placing a sample in the center of a pressure plate of a universal testing machine, adjusting the height of the pressure plate to ensure that an upper pressure plate is just contacted with the sample, setting the speed of the pressure plate to be 20mm/min for measurement, measuring and calculating the Young modulus, wherein the specific test result is shown in table 1;
table 1: product performance test results
| Young's modulus/MPa | |
| Example 1 | 92.5 |
| Example 2 | 92.6 |
| Example 3 | 92.7 |
| Example 4 | 88.6 |
| Example 5 | 89.2 |
| Example 6 | 86.5 |
| Comparative example 1 | 55.6 |
| Comparative example 2 | 50.1 |
| Comparative example 3 | 62.5 |
| Comparative example 4 | 65.5 |
The test results in table 1 show that the product obtained by the invention has excellent mechanical properties.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. The cellulose-graphene porous composite aerogel is characterized by comprising the following raw materials in parts by weight:
80-100 parts of cellulose, 0.5-1.5 parts of graphene oxide with the particle size distribution range of 5-20nm and 2-5 parts of reduced graphene with the particle size distribution range of 100-500 nm;
at least a portion of the cellulose and at least a portion of the graphene oxide are intercalated between adjacent lamellar structures of the reduced graphene to form a sandwich structure.
2. The cellulose-graphene porous composite aerogel according to claim 1, wherein the cellulose molecular structure contains aldehyde functional groups.
3. The cellulose-graphene porous composite aerogel according to claim 1, wherein the graphene oxide is obtained by spray drying of a graphene oxide aqueous solution.
4. The cellulose-graphene porous composite aerogel according to claim 3, wherein the graphene oxide aqueous solution comprises 0.3-0.5% by mass of glycerol and 0.3-0.5% by mass of ethylene glycol.
5. The preparation method of the cellulose-graphene porous composite aerogel is characterized by comprising the following specific preparation steps:
according to the weight portion, 80-100 portions of cellulose, 0.5-1.5 portions of oxidized graphene with the particle size distribution range of 5-20nm and 2-5 portions of reduced graphene with the particle size distribution range of 100-500nm are taken in sequence;
dissolving cellulose in ionic liquid to obtain ionic liquid solution of the cellulose;
adding oxidized graphene and reduced graphene into the ionic liquid solution of cellulose, carrying out ultrasonic dispersion uniformly, and dialyzing by using deionized water to remove the ionic liquid to obtain composite hydrogel;
and (4) freeze-drying the obtained composite hydrogel to obtain the product.
6. The preparation method of the cellulose-graphene porous composite aerogel according to claim 5, wherein the specific preparation steps further comprise:
pretreating cellulose: mixing cellulose and sodium periodate solution, heating and stirring for reaction, filtering, washing and drying to obtain pretreated cellulose;
and after the obtained composite hydrogel is freeze-dried, heating and dehydrating for 25-30min at the temperature of 85-90 ℃ to obtain the product.
7. The preparation method of the cellulose-graphene porous composite aerogel according to claim 5, wherein the specific preparation steps further comprise:
pretreating graphene oxide: dispersing graphene oxide with the particle size distribution range of 5-20nm in deionized water to form a graphene oxide aqueous solution, adding glycerol accounting for 0.3-0.5% of the mass of the graphene oxide aqueous solution and ethylene glycol accounting for 0.3-0.5% of the mass of the graphene oxide aqueous solution into the graphene oxide aqueous solution, uniformly dispersing, and performing spray drying to obtain the pretreated graphene oxide.
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