CN106935411A - A kind of preparation of Graphene/mesoporous carbon spheres/array polyaniline material - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 31
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 title abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 239000002131 composite material Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 9
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000012265 solid product Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 2
- 239000011206 ternary composite Substances 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
本发明涉及一种石墨烯/介孔碳球/阵列聚苯胺材料的制备方法。包括以下步骤：介孔二氧化硅的制备，介孔碳球的制备，石墨烯/介孔碳球/聚苯胺的制备。本发明的有益效果是石墨烯/介孔碳球/聚苯胺三元复合材料的制备方法新颖独特。The invention relates to a preparation method of graphene/mesoporous carbon sphere/array polyaniline material. The method comprises the following steps: preparation of mesoporous silicon dioxide, preparation of mesoporous carbon spheres, and preparation of graphene/mesoporous carbon spheres/polyaniline. The beneficial effect of the invention is that the preparation method of the graphene/mesoporous carbon sphere/polyaniline ternary composite material is novel and unique.
Description
技术领域technical field
本发明涉及一种石墨烯/介孔碳球/阵列聚苯胺复合材料的制备方法，属于材料合成和电化学研究领域。The invention relates to a preparation method of a graphene/mesoporous carbon sphere/array polyaniline composite material, which belongs to the field of material synthesis and electrochemical research.
技术背景technical background
以石墨烯为基质的电极材料在最近几年一直是研究的热点，石墨烯具有较高的电导率和比表面积使得石墨烯具有很好的电化学性能，石墨烯易团聚的缺点限制了其电容性能，石墨烯与导电高分子的复合防止石墨烯团聚的同时还增加了电极材料的比表面积。聚苯胺酸掺杂后具有较高的导电率，增加了充放电过程中的电子传导速率，聚苯胺产生的是法拉第电容，有利于提高整个电容器的电容，对于聚苯胺而言，石墨烯的加入起到了很好的固定作用，改善了聚苯胺在充放电过程中因为肿胀和收缩造成的易坍塌、易溶解、稳定性和充放电循环性差等缺陷。独特有序结构的聚苯胺可以提供相对较短的离子扩散路径，在超级电容器中可以显示更好的电容性能，使苯胺在介孔碳球上聚合生长形成阵列聚苯胺的同时与石墨烯复合，防止石墨烯团聚的同时有序结构的聚苯胺还可以提高电容性能。因此我们提供了一个成功的路线合成石墨烯/介孔碳球/阵列聚苯胺。Graphene-based electrode materials have been a research hotspot in recent years. Graphene has high electrical conductivity and specific surface area, which makes graphene have good electrochemical performance. The disadvantage of graphene's easy agglomeration limits its capacitance. Performance, the combination of graphene and conductive polymers prevents graphene from agglomerating and increases the specific surface area of the electrode material. Polyaniline acid has higher conductivity after doping, which increases the electron conduction rate during charge and discharge. Polyaniline produces Faraday capacitance, which is beneficial to improve the capacitance of the entire capacitor. For polyaniline, the addition of graphene It plays a very good fixing role and improves the defects of polyaniline, such as easy collapse, easy dissolution, poor stability and poor charge-discharge cycle, caused by swelling and shrinkage during the charging and discharging process. The polyaniline with a unique ordered structure can provide a relatively short ion diffusion path, and it can show better capacitance performance in supercapacitors, so that aniline can be polymerized and grown on mesoporous carbon spheres to form an array of polyaniline and composite with graphene at the same time, The polyaniline ordered structure can also improve the capacitive performance while preventing graphene agglomeration. We thus provide a successful route to synthesize graphene/mesoporous carbon spheres/arrays of polyaniline.
发明内容Contents of the invention
本发明的目的是在于提供一种石墨烯/介孔碳球/阵列聚苯胺复合材料的制备方法。The purpose of the present invention is to provide a preparation method of graphene/mesoporous carbon sphere/array polyaniline composite material.
本发明所述一种石墨烯/介孔碳球/阵列聚苯胺复合材料的制备方法包括以下步骤：The preparation method of a kind of graphene/mesoporous carbon sphere/array polyaniline composite material of the present invention comprises the following steps:
a、制备介孔二氧化硅纳米粒子：在60℃下将22.8mL乙醇和十六烷基三甲基溴化胺粉末加入到145.2mL去离子水中并搅拌，十六烷基三甲基溴化胺完全溶解后，加入氨水并保持60℃继续搅拌30min，滴加14.6mL正硅酸乙酯，在60℃继续搅拌2h，将悬浮液冷却至室温，在4000rpm下离心10min，回收固体产物并用去离子水和乙醇反复洗涤，干燥后的产物最后在空气中煅烧6h；a. Preparation of mesoporous silica nanoparticles: add 22.8mL of ethanol and cetyltrimethylammonium bromide powder to 145.2mL of deionized water at 60°C and stir, cetyltrimethylammonium bromide After the amine is completely dissolved, add ammonia water and keep stirring at 60°C for 30 minutes, add 14.6 mL of tetraethyl orthosilicate dropwise, continue stirring at 60°C for 2 hours, cool the suspension to room temperature, centrifuge at 4000 rpm for 10 minutes, recover the solid product and use it Ionized water and ethanol were washed repeatedly, and the dried product was finally calcined in air for 6 hours;
b、介孔碳球的制备：将葡萄糖溶于25mL去离子水中，将步骤a中制备出的二氧化硅加入上述溶液，剧烈搅拌15min，将混合溶液转移到30mL特氟隆衬里的不锈钢高压釜中并在180℃下加热4h，高压釜在空气中自然冷却后将产物过滤并在蒸馏水和乙醇中反复洗涤，60℃下干燥后，样品在管式炉中氮气氛围中煅烧4h，冷却后分散在10％的氢氟酸溶液中24h以除去二氧化硅模版，用蒸馏水和乙醇反复洗涤产物，最后冷冻干燥；b. Preparation of mesoporous carbon spheres: Dissolve glucose in 25 mL deionized water, add the silicon dioxide prepared in step a to the above solution, stir vigorously for 15 min, and transfer the mixed solution to a 30 mL Teflon-lined stainless steel autoclave and heated at 180°C for 4h, after the autoclave was naturally cooled in air, the product was filtered and washed repeatedly in distilled water and ethanol, after drying at 60°C, the sample was calcined in a nitrogen atmosphere in a tube furnace for 4h, and dispersed after cooling In 10% hydrofluoric acid solution for 24 hours to remove the silica template, the product was repeatedly washed with distilled water and ethanol, and finally freeze-dried;
c、石墨烯/介孔碳球/阵列聚苯胺复合材料的制备：将氧化石墨烯和b中制备出的介孔碳球加入到含有2.28g苯胺和盐酸的20mL 20％的乙醇中，剧烈搅拌1h，将20mL 20％的乙醇快速加入到上述溶液中，将0.644g过硫酸铵溶于1mL去离子水中并逐滴加入上述溶液中，在0℃下搅拌10h后加入锌粉，超声处理15min，加入5mL盐酸溶解过量锌粉，用过量水和乙醇冲洗后冷冻干燥。c. Preparation of graphene/mesoporous carbon spheres/array polyaniline composites: add graphene oxide and mesoporous carbon spheres prepared in b to 20mL of 20% ethanol containing 2.28g of aniline and hydrochloric acid, and stir vigorously 1h, quickly add 20mL of 20% ethanol to the above solution, dissolve 0.644g of ammonium persulfate in 1mL of deionized water and add it dropwise to the above solution, stir at 0°C for 10h, add zinc powder, and ultrasonically treat for 15min. Add 5mL of hydrochloric acid to dissolve excess zinc powder, rinse with excess water and ethanol, and freeze-dry.
进一步,步骤a中十六烷基三甲基溴化胺的量为3～6g，氨水为1～3mL，煅烧温度为400～600℃。Further, in step a, the amount of cetyltrimethylammonium bromide is 3-6g, the ammonia water is 1-3mL, and the calcination temperature is 400-600°C.
进一步，所述步骤b中葡萄糖的量为2～3g，二氧化硅的量为0.5～1.5g，管式炉中煅烧温度为700～900℃。Further, in the step b, the amount of glucose is 2-3g, the amount of silicon dioxide is 0.5-1.5g, and the calcination temperature in the tube furnace is 700-900°C.
进一步,所述步骤c中氧化石墨烯的量为3～6mg,介孔碳球为0.5～1.5g，盐酸为2～4mL,锌粉为300～600mg。Further, in the step c, the amount of graphene oxide is 3-6 mg, the amount of mesoporous carbon spheres is 0.5-1.5 g, the amount of hydrochloric acid is 2-4 mL, and the amount of zinc powder is 300-600 mg.
本发明的有益效果是：石墨烯/介孔碳球/阵列聚苯胺复合材料的制备方法新颖独特。The beneficial effect of the invention is that the preparation method of the graphene/mesoporous carbon sphere/array polyaniline composite material is novel and unique.
具体实施方式detailed description
现在结合具体实施例对本发明做进一步说明，以下实施例旨在说明本发明而不是对本发明的进一步限定。The present invention will now be further described in conjunction with specific examples, and the following examples are intended to illustrate the present invention rather than further limit the present invention.
实施例一：Embodiment one:
石墨烯/介孔碳球/阵列聚苯胺材料的制备方法，包括以下步骤：The preparation method of graphene/mesoporous carbon sphere/array polyaniline material comprises the following steps:
(1)在60℃下将22.8mL乙醇和5.73g十六烷基三甲基溴化胺粉末加入到145.2mL去离子水中并搅拌，在十六烷基三甲基溴化胺完全溶解后，将1.25mL氨水加入到混合物中，保持60℃继续搅拌30min后，滴加14.6mL正硅酸乙酯，在60℃继续搅拌2h，将悬浮液冷却至室温，在4000rpm下离心10min，回收固体产物并用去离子水和乙醇反复洗涤，干燥后的产物最后在550℃下在空气中煅烧6h，得到介孔二氧化硅。(1) Add 22.8mL of ethanol and 5.73g of cetyltrimethylammonium bromide powder into 145.2mL of deionized water at 60°C and stir. After the cetyltrimethylammonium bromide is completely dissolved, Add 1.25mL ammonia water to the mixture, keep stirring at 60°C for 30min, then add 14.6mL tetraethyl orthosilicate dropwise, continue stirring at 60°C for 2h, cool the suspension to room temperature, centrifuge at 4000rpm for 10min, and recover the solid product And washed repeatedly with deionized water and ethanol, the dried product was finally calcined in air at 550° C. for 6 hours to obtain mesoporous silica.
(2)将2.25g葡萄糖溶于25mL去离子水中，然后加入1g步骤(1)中制备出的二氧化硅，在剧烈搅拌15min后，将混合溶液转移到30mL特氟隆衬里的不锈钢高压釜中并在180℃下加热4h，高压釜在空气中自然冷却后将产物过滤并在蒸馏水和乙醇中反复洗涤，60℃下干燥后，样品在管式炉中氮气氛围中750℃下煅烧4h，冷却后取出浸在10％的氢氟酸溶液中24小时以除去二氧化硅模版，用蒸馏水和乙醇反复洗涤产物，最后冷冻干燥，制备出介孔碳球。(2) Dissolve 2.25 g of glucose in 25 mL of deionized water, then add 1 g of the silica prepared in step (1), and after stirring vigorously for 15 min, transfer the mixed solution to a 30 mL Teflon-lined stainless steel autoclave And heated at 180°C for 4h, after the autoclave was naturally cooled in the air, the product was filtered and washed repeatedly in distilled water and ethanol, after drying at 60°C, the sample was calcined in a tube furnace at 750°C for 4h in a nitrogen atmosphere, cooled Then take it out and immerse it in 10% hydrofluoric acid solution for 24 hours to remove the silica template, wash the product repeatedly with distilled water and ethanol, and finally freeze-dry to prepare mesoporous carbon spheres.
(3)将氧化石墨烯4mg和(2)中制备出的介孔碳球1g加入到含有2.8g苯胺和3.3mL盐酸的20mL 20％的乙醇中，剧烈搅拌1h，将20mL 20％的乙醇快速加入到上述溶液中，将0.644g过硫酸铵溶于3mL去离子水中并逐滴加入上述溶液中，在0℃下搅拌10h后加入500mg锌粉，超声处理15min，加入5mL盐酸溶解过量锌粉，用过量水和乙醇冲洗后冷冻干燥,制备出石墨烯/介孔碳球/阵列聚苯胺。(3) Add 4 mg of graphene oxide and 1 g of mesoporous carbon spheres prepared in (2) to 20 mL of 20% ethanol containing 2.8 g of aniline and 3.3 mL of hydrochloric acid, stir vigorously for 1 h, and quickly dissolve 20 mL of 20% ethanol Add to the above solution, dissolve 0.644g of ammonium persulfate in 3mL of deionized water and add dropwise to the above solution, stir at 0°C for 10h, add 500mg of zinc powder, ultrasonically treat for 15min, add 5mL of hydrochloric acid to dissolve the excess zinc powder, The graphene/mesoporous carbon sphere/array polyaniline was prepared by rinsing with excess water and ethanol and freeze-drying.
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| CN109065896A (en) * | 2018-08-15 | 2018-12-21 | 山东建筑大学 | The nanometer-material-modified anode of microbial fuel cell preparation method of mesoporous silicon oxide/polypyrrole |
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