CN110127660B - Method for Microwave Preparation of Porous Carbon Nanomaterials - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000376 reactant Substances 0.000 claims abstract description 23
- 229960002635 potassium citrate Drugs 0.000 claims abstract description 16
- 239000001508 potassium citrate Substances 0.000 claims abstract description 16
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims abstract description 16
- 235000011082 potassium citrates Nutrition 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 4
- 239000006230 acetylene black Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 21
- 238000002484 cyclic voltammetry Methods 0.000 description 10
- 238000010586 diagram Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 230000035484 reaction time Effects 0.000 description 7
- 239000003575 carbonaceous material Substances 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 4
- 238000001994 activation Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- -1 CO 2 Chemical compound 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
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Abstract
本发明公开了一种微波制备多孔碳纳米材料的方法。所述方法以质量比为1:1的碳粉与甲苯的混合物为微波反应剂,按质量比为1:10~200将微波反应剂和柠檬酸钾混合后研磨,再置于200~800W下微波加热,制备得到多孔碳纳米材料。本发明方法简便、高效且成本低,制得的多孔碳纳米材料具有较高比表面积和比电容,可作为高性能超级电容器材料。
The invention discloses a method for preparing porous carbon nanometer material by microwave. The method uses a mixture of carbon powder and toluene with a mass ratio of 1:1 as a microwave reactant, mixes the microwave reactant and potassium citrate at a mass ratio of 1:10-200, grinds them, and then places them under 200-800W Microwave heating is used to prepare porous carbon nanomaterials. The method of the invention is simple, efficient and low in cost, and the prepared porous carbon nanometer material has relatively high specific surface area and specific capacitance, and can be used as a high-performance supercapacitor material.
Description
技术领域technical field
本发明涉及碳材料制备技术领域,涉及一种微波制备多孔碳纳米材料的方法。The invention relates to the technical field of carbon material preparation, and relates to a method for preparing porous carbon nanomaterials by microwave.
背景技术Background technique
多孔碳材料具有尺寸可控的孔道结构、良好的导电和导热性、可调的表面组分等特性,可以作为优良的电极材料,应用于锂离子电池和超级电容器。多孔碳材料的制备主要通过含碳前驱体原料在惰性气氛保护下,高温处理形成,通过选择前驱体的种类以及多样的活化方式,对碳材料的形貌、孔径结构和表面组分进行调控。除了需要经过高温活化合成碳材料以外,在材料活化过程中往往需要加入一些助剂如水蒸气、CO2、KOH、ZnCl2等。虽然上述方法能够获得高孔径分布、高比表面积的多孔碳材料,但往往能耗较高,产量偏低,后处理会产生二次污染,不利于节能环保。Porous carbon materials have the characteristics of size-controllable pore structure, good electrical and thermal conductivity, and adjustable surface composition. They can be used as excellent electrode materials for lithium-ion batteries and supercapacitors. The preparation of porous carbon materials is mainly formed by high-temperature treatment of carbon-containing precursor raw materials under the protection of an inert atmosphere. By selecting the type of precursor and various activation methods, the morphology, pore structure and surface components of carbon materials are regulated. In addition to high temperature activation to synthesize carbon materials, it is often necessary to add some additives such as water vapor, CO 2 , KOH, ZnCl 2 , etc. during the material activation process. Although the above methods can obtain porous carbon materials with high pore size distribution and high specific surface area, they often consume high energy consumption and low yield, and post-processing will cause secondary pollution, which is not conducive to energy conservation and environmental protection.
微波反应法作为一种新型的加热方法,具有升温速率快、反应程度高、节能环保等优点。Voiry研究组采用家用微波炉预热处理结合微波还原的方法(Science,2016,353,1413),制备的石墨烯碳基团含量高、表面缺陷数量少。微波产生的瞬间高热可使氧化石墨烯发生深度脱氧以及促进碳原子的重组使缺陷减少。但是,预处理需要长时间传统加热方式对氧化石墨烯进行预还原。中国专利申请CN108258240A中,虽采用了微波辅助实验,但只是采用微波合成了混合物,并且后续还需要高温煅烧才能制得多孔结构的空心碳球,实验步骤繁琐,耗时长,成本较高。As a new heating method, the microwave reaction method has the advantages of fast heating rate, high reaction degree, energy saving and environmental protection. Voiry's research group adopted the method of household microwave preheating combined with microwave reduction (Science, 2016, 353, 1413), and the prepared graphene has a high content of carbon groups and a small number of surface defects. The instantaneous high heat generated by microwave can deeply deoxidize graphene oxide and promote the recombination of carbon atoms to reduce defects. However, the pretreatment requires a long time of traditional heating to pre-reduce graphene oxide. In the Chinese patent application CN108258240A, although microwave-assisted experiments were used, the mixture was only synthesized by microwaves, and subsequent high-temperature calcination was required to produce hollow carbon spheres with a porous structure. The experimental steps were cumbersome, time-consuming, and costly.
发明内容Contents of the invention
本发明的目的在于提供一种快速高效合成且具有高比表面积和较高比电容的微波制备多孔碳纳米材料的方法,解决现有技术的反应时间长、能耗大、生产成本高的问题。The purpose of the present invention is to provide a rapid and efficient method for preparing porous carbon nanomaterials by microwave with high specific surface area and high specific capacitance, so as to solve the problems of long reaction time, large energy consumption and high production cost in the prior art.
实现本发明目的的技术方案如下:The technical scheme that realizes the object of the present invention is as follows:
微波制备多孔碳纳米材料的方法,具体步骤如下:The method for microwave preparation of porous carbon nanomaterials, the specific steps are as follows:
以质量比为1:1的碳粉与甲苯的混合物为微波反应剂,按质量比为1:10~200将微波反应剂和柠檬酸钾混合后研磨,再置于200~800W下微波加热,反应结束后,自然冷却,洗涤,减压抽滤并干燥,得到多孔碳纳米材料。Use the mixture of carbon powder and toluene with a mass ratio of 1:1 as the microwave reactant, mix the microwave reactant and potassium citrate at a mass ratio of 1:10-200, grind them, and then place them under 200-800W for microwave heating. After the reaction is finished, cool naturally, wash, filter under reduced pressure and dry to obtain a porous carbon nanomaterial.
本发明所述的碳粉选自石墨、乙炔黑或活性炭。The carbon powder of the present invention is selected from graphite, acetylene black or activated carbon.
优选地,所述的微波反应剂和柠檬酸钾的质量比为1:100~200。Preferably, the mass ratio of the microwave reactant to potassium citrate is 1:100-200.
优选地,所述的研磨时间为10~20min,所述的微波加热时间为60~600s,在保证原料的充分反应的同时又能够降低能耗。Preferably, the grinding time is 10-20 min, and the microwave heating time is 60-600 s, which can reduce energy consumption while ensuring sufficient reaction of raw materials.
优选地,所述的洗涤为依次采用10~50%的稀盐酸和水洗涤去除杂质。Preferably, the washing is sequentially washing with 10-50% dilute hydrochloric acid and water to remove impurities.
优选地,所述的干燥温度为50~100℃,所述温度下既能使多孔碳纳米材料充分干燥,又可以防止多孔碳纳米材料表面的氧化。Preferably, the drying temperature is 50-100° C., which can not only fully dry the porous carbon nanomaterials, but also prevent the surface oxidation of the porous carbon nanomaterials.
与现有技术相比,本发明具有以下优点:Compared with the prior art, the present invention has the following advantages:
本发明方法简单易行,反应时间短,无需使用大型高能耗加热装置,以柠檬酸钾作为碳源,绿色环保,成本低,制得的多孔碳纳米材料物化性质稳定,且具有较高比表面积和比电容。The method of the invention is simple and easy, has short reaction time, does not need to use a large-scale high-energy-consuming heating device, uses potassium citrate as a carbon source, is environmentally friendly, and has low cost, and the prepared porous carbon nanomaterial has stable physical and chemical properties and has a relatively high specific surface area. and specific capacitance.
附图说明Description of drawings
图1是实施例1所制备材料的扫描电镜图。FIG. 1 is a scanning electron microscope image of the material prepared in Example 1.
图2是实施例1所制备材料的(a)循环伏安曲线,(b)充放电曲线图。Fig. 2 is (a) cyclic voltammetry curve, (b) charge-discharge curve diagram of the material prepared in Example 1.
图3是实施例2所制备材料的(a)循环伏安曲线,(b)充放电曲线图。Fig. 3 is (a) cyclic voltammetry curve, (b) charge-discharge curve diagram of the material prepared in Example 2.
图4是实施例3所制备材料的(a)循环伏安曲线,(b)充放电曲线图。Fig. 4 is (a) cyclic voltammetry curve, (b) charge-discharge curve diagram of the material prepared in Example 3.
图5是对比例1所制备材料的(a)循环伏安曲线,(b)充放电曲线图。Fig. 5 is (a) cyclic voltammetry curve, (b) charge-discharge curve diagram of the material prepared in Comparative Example 1.
图6是对比例2所制备材料的(a)循环伏安曲线,(b)充放电曲线图。Fig. 6 is (a) cyclic voltammetry curve and (b) charge-discharge curve diagram of the material prepared in Comparative Example 2.
具体实施方式Detailed ways
下面结合实施例和附图对本发明作进一步详述。The present invention will be described in further detail below in conjunction with the embodiments and accompanying drawings.
实施例1Example 1
称取微波反应剂0.01g和柠檬酸钾1g,其中微波反应剂为石墨和甲苯的混合物,质量比为1:1,将微波反应剂和柠檬酸钾混合于研钵中充分研磨10分钟,然后置于微波反应器中进行微波加热,反应功率为600W,反应时间为300s。待产物自然冷却后,将产物用1mol/L盐酸和水洗涤去除杂质,减压抽滤并在60℃烘箱中干燥,得到多孔碳纳米材料。其比表面积为1200m2/g。Take by weighing microwave reactant 0.01g and potassium citrate 1g, wherein microwave reactant is the mixture of graphite and toluene, mass ratio is 1:1, microwave reactant and potassium citrate are mixed in mortar and ground fully 10 minutes, then Place in a microwave reactor for microwave heating, the reaction power is 600W, and the reaction time is 300s. After the product was naturally cooled, the product was washed with 1 mol/L hydrochloric acid and water to remove impurities, filtered under reduced pressure and dried in an oven at 60°C to obtain a porous carbon nanomaterial. Its specific surface area is 1200 m 2 /g.
实施例2Example 2
称取微波反应剂0.01g和柠檬酸钾0.1g,其中微波反应剂为石墨和甲苯的混合物,质量比为1:1,将微波反应剂和柠檬酸钾混合于研钵中充分研磨10分钟,然后置于微波反应器中进行微波加热,反应功率为600W,反应时间为300s。待产物自然冷却后,将产物用1mol/L盐酸和水洗涤去除杂质,减压抽滤并在60℃烘箱中干燥,得到多孔碳纳米材料。Take by weighing microwave reactant 0.01g and potassium citrate 0.1g, wherein microwave reactant is the mixture of graphite and toluene, mass ratio is 1:1, microwave reactant and potassium citrate are mixed in mortar and ground fully 10 minutes, Then place it in a microwave reactor for microwave heating, the reaction power is 600W, and the reaction time is 300s. After the product was naturally cooled, the product was washed with 1 mol/L hydrochloric acid and water to remove impurities, filtered under reduced pressure and dried in an oven at 60°C to obtain a porous carbon nanomaterial.
实施例3Example 3
称取微波反应剂0.01g和柠檬酸钾2g,其中微波反应剂为石墨和甲苯的混合物,质量比为1:1,将微波反应剂和柠檬酸钾混合于研钵中充分研磨10分钟,然后置于微波反应器中进行微波加热,反应功率为600W,反应时间为300s。待产物自然冷却后,将产物用1mol/L盐酸和水洗涤去除杂质,减压抽滤并在60℃烘箱中干燥,得到多孔碳纳米材料。Take by weighing microwave reactant 0.01g and potassium citrate 2g, wherein microwave reactant is the mixture of graphite and toluene, mass ratio is 1:1, microwave reactant and potassium citrate are mixed in mortar and ground fully 10 minutes, then Place in a microwave reactor for microwave heating, the reaction power is 600W, and the reaction time is 300s. After the product was naturally cooled, the product was washed with 1 mol/L hydrochloric acid and water to remove impurities, filtered under reduced pressure and dried in an oven at 60°C to obtain a porous carbon nanomaterial.
对比例1Comparative example 1
称取微波反应剂0.01g和柠檬酸钾0.09g,其中微波反应剂为石墨和甲苯的混合物,质量比为1:1,将微波反应剂和柠檬酸钾混合于研钵中充分研磨10分钟,然后置于微波反应器中进行微波加热,反应功率为600W,反应时间为300s。待产物自然冷却后,将产物用1mol/L盐酸和水洗涤去除杂质,减压抽滤并在60℃烘箱中干燥,得到多孔碳纳米材料。Take by weighing microwave reactant 0.01g and potassium citrate 0.09g, wherein microwave reactant is the mixture of graphite and toluene, mass ratio is 1:1, microwave reactant and potassium citrate are mixed in mortar and ground fully 10 minutes, Then place it in a microwave reactor for microwave heating, the reaction power is 600W, and the reaction time is 300s. After the product was naturally cooled, the product was washed with 1 mol/L hydrochloric acid and water to remove impurities, filtered under reduced pressure and dried in an oven at 60°C to obtain a porous carbon nanomaterial.
对比例2Comparative example 2
称取微波反应剂0.01g和柠檬酸钾2.1g,其中微波反应剂为石墨和甲苯的混合物,质量比为1:1,将微波反应剂和柠檬酸钾混合于研钵中充分研磨10分钟,然后置于微波反应器中进行微波加热,反应功率为600W,反应时间为300s。待产物自然冷却后,将产物用1mol/L盐酸和水洗涤去除杂质,减压抽滤并在60℃烘箱中干燥,得到多孔碳纳米材料。Take by weighing microwave reactant 0.01g and potassium citrate 2.1g, wherein microwave reactant is the mixture of graphite and toluene, mass ratio is 1:1, microwave reactant and potassium citrate are mixed in mortar and ground fully 10 minutes, Then place it in a microwave reactor for microwave heating, the reaction power is 600W, and the reaction time is 300s. After the product was naturally cooled, the product was washed with 1 mol/L hydrochloric acid and water to remove impurities, filtered under reduced pressure and dried in an oven at 60°C to obtain a porous carbon nanomaterial.
图1是实施例1所制备材料的扫描电镜图,从图中可以看出氮掺杂碳纳米片为多孔状结构,孔径约为0.4微米,壁厚约为30纳米。Fig. 1 is a scanning electron microscope image of the material prepared in Example 1. It can be seen from the figure that the nitrogen-doped carbon nanosheet is a porous structure with a pore diameter of about 0.4 microns and a wall thickness of about 30 nanometers.
图2是实施例1所制备材料的(a)循环伏安曲线、(b)充放电曲线图,从曲线中可知实施例1所制备材料的比电容为318F/g,具有较高的比电容量。Fig. 2 is (a) cyclic voltammetry curve, (b) charge-discharge curve diagram of the material prepared in embodiment 1, it can be known from the curve that the specific capacitance of the material prepared in embodiment 1 is 318F/g, has higher specific electric capacity capacity.
图3是实施例2所制备材料的(a)循环伏安曲线、(b)充放电曲线图,从曲线中可知实施例2所制备材料的比电容为186.2F/g。Fig. 3 is (a) cyclic voltammetry curve, (b) charge-discharge curve diagram of the material prepared in Example 2, and it can be known from the curve that the specific capacitance of the material prepared in Example 2 is 186.2 F/g.
图4是实施例3所制备材料的(a)循环伏安曲线、(b)充放电曲线图,从曲线中可知实施例3所制备材料的比电容为259F/g。Fig. 4 is (a) cyclic voltammetry curve, (b) charge-discharge curve diagram of the material prepared in Example 3, and it can be known from the curve that the specific capacitance of the material prepared in Example 3 is 259 F/g.
图5是对比例1所制备材料的(a)循环伏安曲线、(b)充放电曲线图,从曲线中可知对比例1所制备材料的比电容为30F/g,具有低的比电容量。Fig. 5 is (a) cyclic voltammetry curve, (b) charge-discharge curve diagram of the material prepared in comparative example 1, as can be seen from the curve, the specific capacitance of the material prepared in comparative example 1 is 30F/g, has a low specific capacitance .
图6是本发明对比例2所制备材料的(a)循环伏安曲线、(b)充放电曲线图,从曲线中可知对比例2所制备材料的比电容为176F/g,具有较低的比电容量。Fig. 6 is (a) cyclic voltammetry curve, (b) charge-discharge curve diagram of the material prepared in comparative example 2 of the present invention, it can be seen from the curve that the specific capacitance of the material prepared in comparative example 2 is 176F/g, which has a lower Specific capacitance.
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CN103833006A (en) * | 2014-03-06 | 2014-06-04 | 安徽工业大学 | One-step preparation method of three-dimensional mesoporous nanometer cage-shaped carbon material for super capacitor |
CN103936006A (en) * | 2014-04-21 | 2014-07-23 | 北京理工大学 | Method for preparing porous activated carbon material from rice bran |
CN107619035A (en) * | 2017-11-09 | 2018-01-23 | 扬州大学 | A kind of preparation method of nitrogen-doped carbon nano material |
CN108328599A (en) * | 2018-01-30 | 2018-07-27 | 东莞理工学院 | Method for preparing nitrogen-doped porous carbon material based on citric acid transition/alkali metal complex salt |
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2019
- 2019-05-08 CN CN201910378231.9A patent/CN110127660B/en active Active
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2020
- 2020-05-06 ZA ZA2020/02472A patent/ZA202002472B/en unknown
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103833006A (en) * | 2014-03-06 | 2014-06-04 | 安徽工业大学 | One-step preparation method of three-dimensional mesoporous nanometer cage-shaped carbon material for super capacitor |
CN103936006A (en) * | 2014-04-21 | 2014-07-23 | 北京理工大学 | Method for preparing porous activated carbon material from rice bran |
CN107619035A (en) * | 2017-11-09 | 2018-01-23 | 扬州大学 | A kind of preparation method of nitrogen-doped carbon nano material |
CN108328599A (en) * | 2018-01-30 | 2018-07-27 | 东莞理工学院 | Method for preparing nitrogen-doped porous carbon material based on citric acid transition/alkali metal complex salt |
Non-Patent Citations (1)
Title |
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Chaozheng Liu et al..Fast Microwave Synthesis of Hierarchical Porous Carbons from Waste Palm Boosted by Activated Carbons for Supercapacitors.《Nanomaterials》.2019,第9卷(第3期),第405-417页. * |
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ZA202002472B (en) | 2021-09-29 |
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