CN113617303A - Preparation method of chitosan/reduced graphene oxide aerogel - Google Patents
Preparation method of chitosan/reduced graphene oxide aerogel Download PDFInfo
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- CN113617303A CN113617303A CN202110994421.0A CN202110994421A CN113617303A CN 113617303 A CN113617303 A CN 113617303A CN 202110994421 A CN202110994421 A CN 202110994421A CN 113617303 A CN113617303 A CN 113617303A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 128
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 106
- 239000004964 aerogel Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000007710 freezing Methods 0.000 claims abstract description 22
- 230000008014 freezing Effects 0.000 claims abstract description 22
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000004108 freeze drying Methods 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- -1 polytetrafluoroethylene Polymers 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000012520 frozen sample Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 2
- 230000009467 reduction Effects 0.000 abstract description 24
- 239000002131 composite material Substances 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 4
- 235000010086 Setaria viridis var. viridis Nutrition 0.000 description 3
- 244000304962 green bristle grass Species 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 230000021615 conjugation Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002211 L-ascorbic acid Substances 0.000 description 1
- 235000000069 L-ascorbic acid Nutrition 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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Abstract
The invention discloses a preparation method of chitosan/reduced graphene oxide aerogel, and relates to the technical field of preparation of graphene oxide aerogel. The invention comprises the following steps: preparing a graphene oxide/chitosan high-viscosity solution by using graphene oxide and chitosan; preparing a chitosan/reduced graphene oxide solution through a hydrothermal reaction, pre-freezing the solution through a refrigerator, and then freezing and drying the solution to obtain a finished product. Graphene oxide is reduced by using a mode of combining hydrothermal reduction with chitosan reduction, no additional reducing agent is added, the harm to experimenters and the pollution to the environment are avoided, and the preparation cost of the reduced graphene oxide composite aerogel can be saved; by adopting a hydrothermal reaction and freeze drying method, the preparation process is short, the operation is simple, and the chitosan/reduced graphene oxide aerogel is rapidly and efficiently prepared in a large scale; the aerogel shape is controllable, controls the shape of aerogel through chooseing for use different moulds, and the aerogel of preparation has higher intensity and can not take place the shrink.
Description
Technical Field
The invention belongs to the technical field of preparation of graphene oxide aerogel, and particularly relates to a preparation method of chitosan/reduced graphene oxide aerogel.
Background
With the rapid development of aerogels, unitary aerogels gradually fail to meet the requirements of various fields. Particularly in high-end fields such as aerospace, electronic communication, and the like, high strength is required along with good properties such as light weight, conductivity, and the like.
Graphene is sp2The two-dimensional honeycomb crystal formed by hybridized carbon atoms has the thickness of only one atom size (about 0.34nm), forms stable chemical bonds with surrounding carbon atoms, and the rest electrons on each carbon atom form large pi bonds in which electrons can freely move, so that the structure endows the graphene with good electrical conductivity.
Therefore, more and more researchers begin to aim at the direction of the composite aerogel material, and the aerogel has more unique properties through the compounding of the aerogel and other materials, so that the application of the aerogel in different fields is widened. However, the reduced graphene oxide aerogel is prepared by high-temperature hydrothermal reduction or high-temperature reduction self-assembly of L-ascorbic acid, the morphology of the aerogel prepared by the method is uncontrollable, graphene lamellar structures are mutually stacked under the action of pi-pi conjugation, the aperture is small, the morphology is not easy to control, and the application field is greatly limited.
Therefore, a technical scheme for preparing the reduced graphene oxide aerogel which is simple and controllable is urgently needed at present.
Disclosure of Invention
The invention aims to provide a preparation method of chitosan/reduced graphene oxide aerogel, which is a method for preparing the chitosan/reduced graphene oxide aerogel by reducing graphene oxide in situ through a hydrothermal method and solves the problems that the appearance of the aerogel prepared by the existing method is uncontrollable, graphene lamellar structures are mutually stacked under the action of pi-pi conjugation, the aperture is small, and the appearance is difficult to control.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a preparation method of chitosan/reduced graphene oxide aerogel, which comprises the following steps:
step S001: mixing graphene oxide and chitosan to prepare a chitosan/graphene oxide solution;
step S002: placing the chitosan/graphene oxide solution in a hydrothermal reaction kettle, and carrying out hydrothermal reaction at high temperature to obtain a chitosan/reduced graphene oxide solution;
step S003: and pre-freezing the chitosan/reduced graphene oxide solution in a refrigerator, and then freezing and drying to obtain the chitosan/reduced graphene oxide aerogel.
Further, in step S001, the method for preparing the chitosan/graphene oxide solution includes:
step S011: adding 0.04g of graphene oxide into 10ml of distilled water, and carrying out ultrasonic treatment at room temperature for 30 minutes to obtain a graphene oxide suspension;
step S012: adding 0.375g of chitosan into the stirred graphene oxide suspension in batches, and stirring for 2 hours at room temperature to obtain graphene oxide/chitosan suspension;
step S013: 0.3ml of acetic acid is added into the graphene oxide/chitosan suspension dropwise to dissolve the chitosan, so that the system becomes a high-viscosity solution.
Further, in step S002, the method for preparing the chitosan/reduced graphene oxide solution comprises:
step S021: transferring the chitosan/graphene oxide solution into a polytetrafluoroethylene lining;
step S022: and (3) putting the polytetrafluoroethylene lining into a reaction kettle, and carrying out hydrothermal reaction for 9 hours to obtain a chitosan/reduced graphene oxide solution.
Further, the step of preparing the chitosan/reduced graphene oxide aerogel in the step S003 is as follows:
step S031: cooling the chitosan/reduced graphene oxide solution to normal temperature, and pre-freezing in a refrigerator;
step S032: and (3) freeze-drying the pre-frozen sample in a freeze dryer to obtain the chitosan/reduced graphene oxide aerogel.
Further, the temperature of the hydrothermal reaction is 90-150 ℃.
Further, the pre-freezing conditions of the chitosan/reduced graphene oxide solution in the refrigerator in the step S003 are as follows: pre-freezing for 12h in a refrigerator at-18 deg.C, and fixing the filler to prevent the freeze-dried solution from boiling under negative pressure.
Further, the stirring speed of the graphene oxide suspension in the step S012 is 700-800 r/min.
Further, the obtaining criteria of the high-viscosity solution in the step S013 are:
and (3) uniformly dripping 0.3ml of acetic acid into the graphene oxide/chitosan suspension within 1min, completely dissolving chitosan within 30s, and continuously stirring for 2h to ensure that the chitosan is fully dissolved and the graphene oxide is uniformly dispersed.
The invention has the following beneficial effects:
according to the invention, graphene oxide is reduced by using a mode of combining hydrothermal reduction and chitosan reduction, and the experimental result shows that the reduction mode has a very good reduction effect on the graphene oxide; according to the invention, no additional reducing agent is added, and chitosan is a deacetylated product of natural polysaccharide chitin and is a nontoxic polymer with good biocompatibility, so that the harm to experimenters and the pollution to the environment are avoided, and the preparation cost of the reduced graphene oxide composite aerogel can be saved; by adopting a hydrothermal reaction and freeze drying method, the preparation process is short, the operation is simple, and the chitosan/reduced graphene oxide aerogel can be quickly and efficiently prepared in large quantities; the aerogel shape is controllable, can control the shape of aerogel through chooseing for use different moulds, and the aerogel of preparation has higher intensity and can not take place the shrink.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of the analysis of the physical properties of the chitosan/reduced graphene oxide aerogel CS-rGOA2 according to the present invention;
FIG. 2 is a SEM scanning electron microscope of CS-rGOA 2;
FIG. 3 is a Raman spectrum of different samples;
figure 4 is an XRD diffractogram of the different samples.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Step 1, adding 0.04g of graphene oxide into 10ml of distilled water, and performing ultrasonic treatment at room temperature for 30 minutes to obtain a graphene oxide suspension A1;
step 2, adding 0.375g of chitosan into the graphene oxide suspension A1 stirred at 700r/min in batches, and stirring for 2 hours at room temperature to obtain graphene oxide/chitosan suspension B1;
step 3, gradually dripping 0.3ml of acetic acid into the graphene oxide/chitosan suspension B1, quickly dissolving chitosan, and changing the system into a high-viscosity solution C1;
step 4, transferring the high-viscosity solution C1 into a polytetrafluoroethylene lining;
and 5, putting the polytetrafluoroethylene lining into a reaction kettle, and carrying out hydrothermal reaction at 90 ℃ for 9 hours to obtain a chitosan/reduced graphene oxide solution D1.
Step 6, cooling the chitosan/reduced graphene oxide solution D1 to normal temperature, and pre-freezing in a refrigerator;
and 7, freezing and drying the pre-frozen sample in a freezing dryer to obtain the chitosan/reduced graphene oxide aerogel CS-rGOA 1.
Example 2
Step 1, adding 0.04g of graphene oxide into 10ml of distilled water, and performing ultrasonic treatment at room temperature for 30 minutes to obtain a graphene oxide suspension A2;
step 2, adding 0.375g of chitosan into the graphene oxide suspension A2 stirred at the speed of 800r/min in batches, and stirring for 2 hours at room temperature to obtain graphene oxide/chitosan suspension B2;
and 3, gradually dripping 0.3ml of acetic acid into the graphene oxide/chitosan suspension B2, quickly dissolving chitosan, and changing the system into a high-viscosity solution C2.
Step 4, transferring the high-viscosity solution C2 into a polytetrafluoroethylene lining;
and 5, putting the polytetrafluoroethylene lining into a reaction kettle, and carrying out hydrothermal reaction at 120 ℃ for 9 hours to obtain a chitosan/reduced graphene oxide solution D2.
Step 6, cooling the chitosan/reduced graphene oxide solution D2 to normal temperature, and pre-freezing in a refrigerator;
and 7, freezing and drying the pre-frozen sample in a freezing dryer to obtain the chitosan/reduced graphene oxide aerogel CS-rGOA 2.
Example 3
Step 1, adding 0.04g of graphene oxide into 10ml of distilled water, and performing ultrasonic treatment at room temperature for 30 minutes to obtain a graphene oxide suspension A3;
step 2, adding 0.375g of chitosan into the graphene oxide suspension A3 stirred at a high speed in batches, and keeping stirring at the high speed for 2 hours at room temperature to obtain graphene oxide/chitosan suspension B3;
and 3, gradually dripping 0.3ml of acetic acid into the graphene oxide/chitosan suspension B3, quickly dissolving chitosan, and changing the system into a high-viscosity solution C3.
Step 4, transferring the high-viscosity solution C3 into a polytetrafluoroethylene lining;
and 5, putting the polytetrafluoroethylene lining into a reaction kettle, and carrying out hydrothermal reaction at 150 ℃ for 9 hours to obtain a chitosan/reduced graphene oxide solution D3.
Step 6, cooling the chitosan/reduced graphene oxide solution D3 to normal temperature, and pre-freezing in a refrigerator;
and 7, freezing and drying the pre-frozen sample in a freezing dryer to obtain the chitosan/reduced graphene oxide aerogel CS-rGOA 3.
Control group 1
1. Adding 0.04g of graphene oxide into 10ml of distilled water, and carrying out ultrasonic treatment at room temperature for 30 minutes to obtain a graphene oxide suspension;
2. adding 0.375g of chitosan into the graphene oxide suspension liquid stirred at a high speed in batches, and keeping stirring at the high speed for 2 hours at room temperature to obtain a graphene oxide/chitosan suspension liquid B;
3. gradually dripping 0.3ml of acetic acid into the suspension B, quickly dissolving the chitosan, and changing the system into a high-viscosity solution C;
6. cooling the solution C to normal temperature, and pre-freezing in a refrigerator;
7. freeze-drying the pre-frozen sample in a freeze dryer to obtain chitosan/graphene oxide aerogel CS-GOA;
control group 2
Graphene oxide feedstock (GO) was used as control 2.
Experimental mode
1. Light weight and high strength characterization of chitosan/reduced graphene oxide aerogel
Gently placing the chitosan/reduced graphene oxide aerogel on green bristlegrass, and then placing 100g of weight on the chitosan/reduced graphene oxide aerogel to respectively take digital photos;
2. detection of reduction effect of chitosan/reduced graphene oxide aerogel through hydrothermal reaction
Cutting the chitosan/reduced graphene oxide aerogel into small blocks, and then respectively observing a control group 1, a control group 2, an embodiment 1, an embodiment 2 and an embodiment 3 by using a Raman spectrophotometer to perform reduction effect characterization on the obtained aerogel;
cutting the chitosan/reduced graphene oxide aerogel into small blocks, and then respectively observing a control group 1, a control group 2, an embodiment 1, an embodiment 2 and an embodiment 3 by using an X-ray diffractometer to characterize the reduction effect of the obtained aerogel;
results of the experiment
1. As can be seen from fig. 1(a), (b):
FIG. 1(a) is a digital photograph taken with CS-rGOA2 placed on green bristlegrass: the chitosan/reduced graphene oxide aerogel obtained by reduction at 120 ℃ has lower density and can be easily supported by green bristlegrass;
FIG. 1(b) is a digital photograph taken with a 200g weight placed on CS-rGOA2, the aerogel having a higher strength and being able to easily load the 200g weight.
2. As can be seen from fig. 2, the chitosan/reduced graphene oxide aerogel prepared by hydrothermal reduction at 120 ℃ has a better pore structure, the pore diameter is a micron-sized macropore, and the size is relatively uniform.
3. As can be seen from FIG. 3, the hydrothermal reduction can reduce graphene oxide, and I in the Raman spectrum is increased along with the increase of temperatureD/IGGradually decrease, indicating that the reduction effect is enhanced, and the reduction effect of the chitosan/reduced graphene oxide aerogel is significantly enhanced compared to the reduced graphene oxide aerogel without the addition of chitosan, which is a result of the synergistic effect of the hydrothermal reaction and the reduction of chitosan.
4. As can also be seen from fig. 4, the unreduced graphene oxide has a strong characteristic peak near 9 °, and the characteristic peak near 9 ° of the aerogel after reduction basically disappears corresponding to the (100) crystal plane of the graphene oxide, which indicates that the graphene oxide can be reduced by hydrothermal reduction, and the reduction effect increases with temperature.
According to the preparation method of the chitosan/reduced graphene oxide aerogel, graphene oxide is reduced in a manner of combining hydrothermal reduction and chitosan reduction, and the experimental result shows that the reduction manner has a very good reduction effect on the graphene oxide; according to the invention, no additional reducing agent is added, and chitosan is a deacetylated product of natural polysaccharide chitin and is a nontoxic polymer with good biocompatibility, so that the harm to experimenters and the pollution to the environment are avoided, and the preparation cost of the reduced graphene oxide composite aerogel can be saved; by adopting a hydrothermal reaction and freeze drying method, the preparation process is short, the operation is simple, and the chitosan/reduced graphene oxide aerogel can be quickly and efficiently prepared in large quantities; the aerogel shape is controllable, can control the shape of aerogel through chooseing for use different moulds, and the aerogel of preparation has higher intensity and can not take place the shrink.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. A preparation method of chitosan/reduced graphene oxide aerogel is characterized by comprising the following steps:
step S001: mixing graphene oxide and chitosan to prepare a chitosan/graphene oxide solution;
step S002: placing the chitosan/graphene oxide solution in a hydrothermal reaction kettle, and carrying out hydrothermal reaction at high temperature to obtain a chitosan/reduced graphene oxide solution;
step S003: and pre-freezing the chitosan/reduced graphene oxide solution in a refrigerator, and then freezing and drying to obtain the chitosan/reduced graphene oxide aerogel.
2. The method for preparing the chitosan/reduced graphene oxide aerogel according to claim 1, wherein in the step S001, the method for preparing the chitosan/reduced graphene oxide solution comprises:
step S011: adding 0.04g of graphene oxide into 10ml of distilled water, and carrying out ultrasonic treatment at room temperature for 30 minutes to obtain a graphene oxide suspension;
step S012: adding 0.375g of chitosan into the stirred graphene oxide suspension in batches, and stirring for 2 hours at room temperature to obtain graphene oxide/chitosan suspension;
step S013: 0.3ml of acetic acid is added into the graphene oxide/chitosan suspension dropwise to dissolve the chitosan, so that the system becomes a high-viscosity solution.
3. The preparation method of chitosan/reduced graphene oxide aerogel according to claim 2, wherein in step S002, the method for preparing the chitosan/reduced graphene oxide solution comprises:
step S021: transferring the chitosan/graphene oxide solution into a polytetrafluoroethylene lining;
step S022: and (3) putting the polytetrafluoroethylene lining into a reaction kettle, and carrying out hydrothermal reaction for 9 hours to obtain a chitosan/reduced graphene oxide solution.
4. The method for preparing chitosan/reduced graphene oxide aerogel according to claim 3, wherein the step of preparing the chitosan/reduced graphene oxide aerogel in step S003 is as follows:
step S031: cooling the chitosan/reduced graphene oxide solution to normal temperature, and pre-freezing in a refrigerator;
step S032: and (3) freeze-drying the pre-frozen sample in a freeze dryer to obtain the chitosan/reduced graphene oxide aerogel.
5. The preparation method of chitosan/reduced graphene oxide aerogel according to claim 1 or 3, wherein the temperature of the hydrothermal reaction is 90-150 ℃.
6. The method for preparing the chitosan/reduced graphene oxide aerogel according to claim 1, wherein the pre-freezing conditions of the chitosan/reduced graphene oxide solution in the refrigerator in the step S003 are as follows: pre-freezing for 12h in a refrigerator at-18 ℃.
7. The preparation method of the chitosan/reduced graphene oxide aerogel according to claim 1, wherein the stirring speed of the graphene oxide suspension in the step S012 is 700-800 r/min.
8. The method for preparing chitosan/reduced graphene oxide aerogel according to claim 1, wherein the obtaining criteria of the high-viscosity solution in step S013 are:
and (3) uniformly dripping 0.3ml of acetic acid into the graphene oxide/chitosan suspension within 1min, completely dissolving chitosan within 30s, and continuously stirring for 2h to ensure that the chitosan is fully dissolved and the graphene oxide is uniformly dispersed.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114984757A (en) * | 2022-06-21 | 2022-09-02 | 青岛大学 | Graphene oxide/chitosan composite nanofiltration membrane with controllable water flux or rejection rate and application thereof |
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