CN108711522B - Boron-doped graphene/polyaniline composite aerogel and preparation method thereof - Google Patents
Boron-doped graphene/polyaniline composite aerogel and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 78
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 51
- 239000004964 aerogel Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 33
- 229910021538 borax Inorganic materials 0.000 claims abstract description 20
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000017 hydrogel Substances 0.000 claims abstract description 20
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 20
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- 238000007710 freezing Methods 0.000 claims abstract description 14
- 230000008014 freezing Effects 0.000 claims abstract description 14
- 230000006835 compression Effects 0.000 claims abstract description 13
- 238000007906 compression Methods 0.000 claims abstract description 13
- 239000000499 gel Substances 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000011084 recovery Methods 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000007605 air drying Methods 0.000 claims description 7
- 238000000502 dialysis Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 9
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052796 boron Inorganic materials 0.000 abstract description 3
- 230000003993 interaction Effects 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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Abstract
The invention discloses a boron-doped graphene/polyaniline composite aerogel and a preparation method thereof. The boron-doped graphene/polyaniline composite aerogel is prepared by the following steps: 1) respectively adding aniline and sodium tetraborate solution into graphene oxide solution; 2) carrying out hydrothermal reaction on the mixed solution to obtain composite hydrogel; 3) soaking the obtained composite hydrogel in dialysate and freezing; 4) and naturally drying the freeze-dried composite gel to obtain the boron-doped graphene/polyaniline composite aerogel. According to the invention, the boron-doped graphene/polyaniline composite aerogel is prepared by one step under a hydrothermal condition by utilizing the interaction between aniline and graphene oxide and combining the doping of boron to graphene; the related preparation method is simple, the reaction condition is mild, and the method is suitable for large-scale production; the obtained composite aerogel has good compression recovery performance and is expected to be used in the fields of constructing compressible supercapacitors and the like.
Description
Technical Field
The invention belongs to the technical field of new materials and supercapacitors, and particularly relates to a boron-doped graphene/polyaniline composite aerogel and a preparation method thereof.
Background
Polyaniline is one of the most common conductive polymers, has easily available synthetic raw materials, simple synthetic method and low cost compared with polypyrrole, polythiophene and the like, has the characteristics of high conductivity and good environmental stability, and is widely applied to the fields of chemical sensors, high-efficiency electrode materials, supercapacitors, anticorrosive materials and the like. But the polyaniline has poor mechanical properties, is insoluble and infusible, has poor processability, and limits the further application of the polyaniline.
The graphene is a thin-layer material with a two-dimensional nano structure and has excellent electrical and mechanical properties. The graphene nanosheets with the two-dimensional structures can be assembled into graphene aerogel in a three-dimensional space. However, pure graphene materials only have double-layer capacitance, and graphene nanosheets are easy to agglomerate, which are disadvantageous to the application of graphene in the field of supercapacitors.
The compounding process of graphene and polyaniline is generally realized by a chemical method or an electrochemical method, and a graphene/polyaniline composite powder material, or a composite film, or a composite aerogel can be obtained. However, these graphene/polyaniline composite aerogels do not have compression recovery properties and cannot be applied to the construction of compressible supercapacitors.
Disclosure of Invention
The invention aims to provide a boron-doped graphene/polyaniline composite aerogel aiming at the defects in the prior art, the boron-doped graphene/polyaniline composite aerogel is prepared by taking graphene oxide, aniline and sodium tetraborate as raw materials and adopting a one-step hydrothermal method, the obtained boron-doped graphene/polyaniline composite aerogel has compression resilience, and the related preparation method is simple and is suitable for popularization and application.
In order to achieve the purpose, the invention adopts the technical scheme that:
the boron-doped graphene/polyaniline composite aerogel is prepared by taking graphene oxide, aniline and sodium tetraborate as raw materials and adopting a one-step hydrothermal method, and the boron-doped graphene/polyaniline composite aerogel with compression resilience is obtained.
In the scheme, the reaction temperature of the one-step hydrothermal method is 80-220 ℃, and the reaction time is 8-24 hours.
The preparation method of the boron-doped graphene/polyaniline composite aerogel comprises the following steps:
1) respectively adding aniline and sodium tetraborate solution into graphene oxide solution;
2) carrying out hydrothermal reaction on the mixed solution obtained in the step 1) to obtain composite hydrogel;
3) soaking the obtained composite hydrogel in dialysate and freezing;
4) and naturally air-drying the composite gel obtained after freeze-drying to obtain the boron-doped graphene/polyaniline composite aerogel.
In the scheme, the concentration of the graphene oxide is 1-10 mg/mL, the dosage of the graphene oxide solution is 10-50 mL, the concentration of the sodium tetraborate solution is 5-50 mg/mL, the dosage of the sodium tetraborate solution is 10-250 mu L, and the dosage of the aniline is 10-200 mu L.
In the scheme, the hydrothermal reaction temperature is 80-220 ℃, and the reaction time is 8-24 h.
In the scheme, the dialysate is an ethanol water solution, wherein the mixing volume ratio of ethanol to water is 1: 5-800.
In the scheme, the dialysis time is 4-48 h.
In the scheme, the freezing time is 4-48 h, and the freezing temperature is-5 to-20 ℃.
In the scheme, the air drying temperature is 10-40 ℃, and the air drying time is 24-48 h.
The boron-doped graphene/polyaniline composite aerogel obtained according to the scheme can show good compression recovery performance, and is expected to be applied to the fields of constructing compressible supercapacitors and the like.
Compared with the prior art, the invention has the beneficial effects that:
1) under the hydrothermal condition, electrons obtained by aniline are oxidized and polymerized into polyaniline, oxidized graphene loses electrons and is reduced into graphene, doping of boron into graphene is realized, and boron-doped graphene/polyaniline composite aerogel with compressive resilience is prepared by a one-step method;
2) the boron provided by the sodium tetraborate can perform heteroatom doping on the graphene to improve the performance (electrical property and the like) of the graphene on the one hand, and can play a role in structure enhancement on the other hand, so that the mechanical property (especially the elastic property) of the composite aerogel is improved, and the obtained composite aerogel can still basically recover the original shape under the repeated compression condition;
3) the natural wind drying method is adopted, and a freeze drying method or supercritical CO with higher equipment requirement is not required2The drying method is beneficial to reducing the production cost.
Drawings
Fig. 1 is a schematic view of the boron-doped graphene/polyaniline composite aerogel prepared in example 1 before (a) bearing a 500g weight, (b) bearing a 500g weight, and (c) after removing the 500g weight.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
A boron-doped graphene/polyaniline composite aerogel comprises the following steps:
1) respectively adding 20 mu L of aniline and 20 mu L of sodium tetraborate solution with the concentration of 20mg/mL into 25mL of graphene oxide solution with the concentration of 2 mg/mL;
2) carrying out hydrothermal reaction on the mixed solution at 80 ℃ for 15h to obtain composite hydrogel;
3) soaking the obtained composite hydrogel in ethanol/deionized water solution with the volume ratio of 1:5 for dialysis for 8h, and then freezing for 8h at-15 ℃;
4) and naturally drying the freeze-dried composite gel at 15 ℃ for 48 hours to obtain the boron-doped graphene/polyaniline composite aerogel.
Fig. 1 is a schematic view of a state of the boron-doped graphene/polyaniline composite aerogel obtained in this embodiment before bearing a 500g weight, while bearing a 500g weight, and after removing the 500g weight; it can be seen that the product obtained in this example can be substantially restored to its original state (see fig. 1) after being compressed by a 500g weight; in addition, after the obtained boron-doped graphene/polyaniline composite aerogel is repeatedly compressed for 20 times, the original state can still be basically recovered; the method is expected to be applied to the fields of constructing compressible supercapacitors and the like.
Example 2
A boron-doped graphene/polyaniline composite aerogel comprises the following steps:
1) respectively adding 110 mu L of aniline and 50 mu L of sodium tetraborate solution with the concentration of 50mg/mL into 30mL of graphene oxide solution with the concentration of 4 mg/mL;
2) carrying out hydrothermal reaction on the mixed solution at 120 ℃ for 14h to obtain composite hydrogel;
3) soaking the obtained composite hydrogel in ethanol/deionized water solution with the volume ratio of 1:200 for dialysis for 9h, and then freezing for 9h at-10 ℃;
4) and naturally drying the freeze-dried composite gel at 25 ℃ for 24h to obtain the boron-doped graphene/polyaniline composite aerogel.
Through tests, the boron-doped graphene/polyaniline composite aerogel obtained in the embodiment can show good compression recovery performance.
Example 3
A boron-doped graphene/polyaniline composite aerogel comprises the following steps:
1) respectively adding 80 mu L of aniline and 60 mu L of sodium tetraborate solution with the concentration of 40mg/mL into 30mL of graphene oxide solution with the concentration of 4 mg/mL;
2) carrying out hydrothermal reaction on the mixed solution at 100 ℃ for 15h to obtain composite hydrogel;
3) soaking the obtained composite hydrogel in ethanol/deionized water solution with the volume ratio of 1:80 for dialysis for 4h, and then freezing for 24h at-10 ℃;
4) and naturally drying the freeze-dried composite gel at 40 ℃ for 24h to obtain the boron-doped graphene/polyaniline composite aerogel.
Through tests, the boron-doped graphene/polyaniline composite aerogel obtained in the embodiment can show good compression recovery performance.
Example 4
A boron-doped graphene/polyaniline composite aerogel comprises the following steps:
1) respectively adding 60 mu L of aniline and 200 mu L of sodium tetraborate solution with the concentration of 50mg/mL into 50mL of graphene oxide solution with the concentration of 2 mg/mL;
2) carrying out hydrothermal reaction on the mixed solution at 180 ℃ for 10h to obtain composite hydrogel;
3) soaking the obtained composite hydrogel in ethanol/deionized water solution with the volume ratio of 1:10 for dialysis for 24h, and then freezing for 16h at-15 ℃;
4) and naturally drying the freeze-dried composite gel at 10 ℃ for 36 hours to obtain the boron-doped graphene/polyaniline composite aerogel.
Through tests, the boron-doped graphene/polyaniline composite aerogel obtained in the embodiment can show good compression recovery performance.
Example 5
A boron-doped graphene/polyaniline composite aerogel comprises the following steps:
1) respectively adding 20 mu L of aniline and 30 mu L of sodium tetraborate solution with the concentration of 20mg/mL into 30mL of graphene oxide solution with the concentration of 2 mg/mL;
2) carrying out hydrothermal reaction on the mixed solution at 190 ℃ for 15h to obtain composite hydrogel;
3) soaking the obtained composite hydrogel in ethanol/deionized water solution with the volume ratio of 1:500 for dialysis for 5h, and then freezing at-10 ℃ for 8 h;
4) and naturally drying the freeze-dried composite gel at 30 ℃ for 48h to obtain the boron-doped graphene/polyaniline composite aerogel.
Through tests, the boron-doped graphene/polyaniline composite aerogel obtained in the embodiment can show good compression recovery performance.
Example 6
A boron-doped graphene/polyaniline composite aerogel comprises the following steps:
1) respectively adding 20 mu L of aniline and 20 mu L of sodium tetraborate solution with the concentration of 10mg/mL into 10mL of graphene oxide solution with the concentration of 4 mg/mL;
2) carrying out hydrothermal reaction on the mixed solution at 100 ℃ for 18h to obtain composite hydrogel;
3) soaking the obtained composite hydrogel in ethanol/deionized water solution with volume ratio of 1:5, dialyzing for 4h, and freezing at-20 deg.C for 24 h;
4) and naturally drying the freeze-dried composite gel at 10 ℃ for 36 hours to obtain the boron-doped graphene/polyaniline composite aerogel.
Through tests, the boron-doped graphene/polyaniline composite aerogel obtained in the embodiment can show good compression recovery performance.
Comparative example 1
The preparation method of the boron-doped graphene/polyaniline composite aerogel is substantially the same as that of the embodiment 1, except that boric acid is used for replacing sodium tetraborate.
Tests prove that the obtained boron-doped graphene/polyaniline composite aerogel has no compression recovery performance.
It is apparent that the above embodiments are only examples for clearly illustrating and do not limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are therefore intended to be included within the scope of the invention as claimed.
Claims (8)
1. The boron-doped graphene/polyaniline composite aerogel is characterized in that graphene oxide, aniline and sodium tetraborate are used as raw materials, and a one-step hydrothermal method is adopted to prepare the boron-doped graphene/polyaniline composite aerogel with compressive recovery; the method specifically comprises the following steps:
1) respectively adding aniline and sodium tetraborate solution into graphene oxide solution;
2) carrying out hydrothermal reaction on the mixed solution obtained in the step 1) to obtain composite hydrogel;
3) soaking the obtained composite hydrogel in dialysate and freezing;
4) and naturally air-drying the composite gel obtained after freeze-drying to obtain the boron-doped graphene/polyaniline composite aerogel.
2. A preparation method of boron-doped graphene/polyaniline composite aerogel is characterized in that graphene oxide, aniline and sodium tetraborate are used as raw materials, and a one-step hydrothermal method is adopted to prepare the boron-doped graphene/polyaniline composite aerogel with compression resilience; the method comprises the following steps:
1) respectively adding aniline and sodium tetraborate solution into graphene oxide solution;
2) carrying out hydrothermal reaction on the mixed solution obtained in the step 1) to obtain composite hydrogel;
3) soaking the obtained composite hydrogel in dialysate and freezing;
4) and naturally air-drying the composite gel obtained after freeze-drying to obtain the boron-doped graphene/polyaniline composite aerogel.
3. The preparation method according to claim 2, wherein the concentration of the graphene oxide in the step 1) is 1-10 mg/mL, the dosage of the graphene oxide solution is 10-50 mL, the concentration of the sodium tetraborate solution is 5-50 mg/mL, the dosage of the sodium tetraborate solution is 10-250 μ L, and the dosage of the aniline is 10-500 μ L.
4. The preparation method according to claim 2, wherein the hydrothermal reaction temperature in the step 2) is 80-220 ℃ and the reaction time is 8-24 hours.
5. The preparation method according to claim 2, wherein the dialysate is an ethanol aqueous solution, and the volume ratio of ethanol to water is 1: 5-800.
6. The method according to claim 2, wherein the dialysis time is 4 to 48 hours.
7. The preparation method according to claim 2, wherein the freezing time is 4-48 h, and the freezing temperature is-5 to-20 ℃.
8. The preparation method of claim 2, wherein the air drying temperature in the step 4) is 10-40 ℃ and the air drying time is 24-48 h.
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| CN109801793A (en) * | 2018-12-26 | 2019-05-24 | 中国电子科技集团公司第十八研究所 | Preparation method of graphene/polypyrrole composite material for lithium ion capacitor cathode material |
| CN113121871B (en) * | 2021-04-21 | 2021-10-26 | 吉林省陆柒肆伍贰科技有限公司 | Preparation method of polyaniline/straw silicon aerogel and heat-insulating anticorrosive coating |
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