CN111943181A - Annular peeling device and peeling method for producing graphene by graphite powder electrochemical method - Google Patents
Annular peeling device and peeling method for producing graphene by graphite powder electrochemical methodDownload PDFInfo
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Abstract
Translated fromChinese
Description
Translated fromChinese技术领域technical field
本发明涉及制备石墨烯领域，具体是一种石墨粉电化学法生产石墨烯的环形剥离装置及剥离方法。The invention relates to the field of graphene preparation, in particular to a ring-shaped peeling device and a peeling method for producing graphene by a graphite powder electrochemical method.
背景技术Background technique
电化学剥离石墨生产石墨烯是一种新兴的石墨烯生产技术，与现有机械剥离法、CVD法、氧化还原法等技术相比，具有低成本、快速高效、绿色环保等优点，近年来受到学术界和工业界的广泛关注和青睐。但是现有以石墨粉为原料剥离制备石墨烯的技术所获得的石墨烯收率普遍较低，其中一个重要的原因是电剥离过程中石墨颗粒离散分布在电解液内，石墨颗粒与临近颗粒的接触点有限甚至为零，因此，电化学处理而膨胀的球团表面上的石墨粒子与电解质接触后，会迅速松动与球团的接触，使其膨胀在过程的相对早期停止，这部分石墨颗粒由于不能再获得电子，即不能再通过电化学剥离的方法进一步产生石墨烯，因而极大降低了石墨粉电化学剥离制备石墨烯的收率，如果能使从电极基体上脱落的石墨颗粒能停留（限制）在石墨电极基体的表面，保持和石墨电极集流体的电子电流的导通，因而就可以使从电极基体上脱落的石墨颗粒继续进行电化学剥离，从而继续产生石墨烯，最终使电化学剥离石墨制备石墨烯的收率提高。Electrochemical exfoliation of graphite to produce graphene is an emerging graphene production technology. Compared with the existing mechanical exfoliation method, CVD method, redox method and other technologies, it has the advantages of low cost, fast efficiency, green environmental protection and so on. Widespread attention and favor from academia and industry. However, the graphene yield obtained by the existing technology of exfoliating graphene with graphite powder as raw material is generally low. One of the important reasons is that the graphite particles are discretely distributed in the electrolyte during the electro-exfoliation process, and the graphite particles and adjacent particles are separated. The contact points are limited or even zero. Therefore, after the graphite particles on the surface of the pellets expanded by electrochemical treatment, after contacting with the electrolyte, the contact with the pellets will be quickly loosened, so that the expansion stops relatively early in the process. This part of the graphite particles Since electrons can no longer be obtained, that is, graphene cannot be further produced by electrochemical exfoliation, which greatly reduces the yield of graphene prepared by electrochemical exfoliation of graphite powder. (Limited) On the surface of the graphite electrode substrate, the electron current conduction with the graphite electrode current collector is maintained, so that the graphite particles falling off the electrode substrate can continue to be electrochemically exfoliated, so as to continue to generate graphene, and finally make the electricity. The yield of graphene prepared by chemical exfoliation of graphite is improved.
发明内容SUMMARY OF THE INVENTION
本发明针对现有的技术中存在的不足，提供一种石墨粉电化学法生产石墨烯的环形剥离装置及剥离方法。这种方法，能够实现规模化、稳定、高效、低成本的电化学剥离石墨粉生产石墨烯，提高了石墨烯收率，稳定了剥离电流。Aiming at the deficiencies existing in the prior art, the present invention provides an annular peeling device and a peeling method for producing graphene by a graphite powder electrochemical method. This method can realize large-scale, stable, high-efficiency, and low-cost electrochemical exfoliation of graphite powder to produce graphene, improve the yield of graphene, and stabilize the exfoliation current.
实现本发明的技术方案是：The technical scheme that realizes the present invention is:
一种石墨粉电化学法生产石墨烯的环形剥离装置，包括电解槽，电解槽内设有电解液，电解槽内设有环形对电极和带网孔的支架，环形对电极围绕支架，支架内套装滤袋膜，滤袋膜内设有石墨粉和集流体, 石墨粉和集流体组成石墨电极，其中石墨电极与环形对电极同圆心，环形对电极与石墨电极之间设有间距，滤袋膜内的石墨粉上端设有重物，环形对电极和集流体外接电源，重物给石墨粉施加的压力可调控。An annular peeling device for producing graphene by a graphite powder electrochemical method, comprising an electrolytic cell, an electrolyte solution is arranged in the electrolytic cell, a ring-shaped counter electrode and a support with mesh holes are arranged in the electrolytic cell, the ring-shaped counter electrode surrounds the support, and the inside of the support Set the filter bag membrane, the filter bag membrane is provided with graphite powder and current collector, graphite powder and current collector form a graphite electrode, in which the graphite electrode and the ring-shaped counter electrode are concentric, and there is a gap between the ring-shaped counter electrode and the graphite electrode, and the filter bag The upper end of the graphite powder in the membrane is provided with a heavy object, and the ring-shaped counter electrode and the current collector are connected to an external power supply, and the pressure exerted by the heavy object on the graphite powder can be adjusted.
所述环形对电极为耐腐蚀金属导电材料。The annular counter electrode is made of corrosion-resistant metal conductive material.
所述环形对电极底面与电解槽内底面之间设有间隙。A gap is provided between the bottom surface of the annular counter electrode and the inner bottom surface of the electrolytic cell.
所述滤袋膜设有孔隙结构，材质耐酸耐碱耐腐蚀，滤袋膜孔隙结构中的孔径小于石墨粉的粒径，滤袋膜允许电解液离子自由通过而石墨粉剥离产物被限域流动，从而提高石墨粉电化学剥离制备石墨烯的收率。The filter bag membrane is provided with a pore structure, and the material is resistant to acid, alkali, corrosion and corrosion. The pore size in the filter bag membrane pore structure is smaller than the particle size of the graphite powder. The filter bag membrane allows the electrolyte ions to pass freely and the graphite powder exfoliation products are restricted to flow. , thereby improving the yield of graphene prepared by electrochemical exfoliation of graphite powder.
所述集流体为柱状的高硬度耐腐蚀的导电材料。The current collector is a columnar conductive material with high hardness and corrosion resistance.
所述支架材质耐酸耐碱耐腐蚀。The bracket material is acid and alkali resistant and corrosion resistant.
所述环形对电极与石墨电极之间的间距为1-7cm。The distance between the annular counter electrode and the graphite electrode is 1-7 cm.
一种实现石墨粉电化学法生产石墨烯的剥离方法，包括上述实现石墨粉电化学生产石墨烯的环形剥离装置，所述方法包括如下的步骤：A peeling method for realizing the electrochemical production of graphene from graphite powder, comprising the above-mentioned annular peeling device for realizing electrochemical production of graphene from graphite powder, and the method comprises the following steps:
1）选择石墨粉材质及颗粒大小：选择人造石墨、天然石墨或是回收废旧石墨粉中的一种，石墨粉的粒径大小在50-800目；1) Select graphite powder material and particle size: choose one of artificial graphite, natural graphite or recycled waste graphite powder, the particle size of graphite powder is 50-800 mesh;
2）选择电解液：选择水系电解液、有机电解液、离子液体中的一种；2) Select electrolyte: choose one of aqueous electrolyte, organic electrolyte and ionic liquid;
3）选择滤袋膜的材质以及孔径大小：根据电解液的种类性质以及石墨粉原材料的孔径大小选择滤袋膜的材质以及目数；3) Select the material and pore size of the filter bag membrane: select the material and mesh number of the filter bag membrane according to the type and nature of the electrolyte and the pore size of the graphite powder raw material;
4）组装电剥离装置：在电解槽内装入步骤2）选择的电解液，将装有石墨粉和集流体的滤袋膜放入支架内，滤袋膜内的石墨粉和集流体组成石墨电极作为阳极或者是阴极的任意一极，环形对电极为对电极，将两电极垂直浸入到装有电解液的电解槽中，其中环形对电极围绕支架外围放置，环形对电极和石墨电极保持同圆心，两电极之间设有间隔，环形对电极底面与电解槽内底面之间设有间隙，两电极与电源的正负极连接；4) Assemble the electro-stripping device: put the electrolyte selected in step 2) into the electrolytic cell, put the filter bag membrane with graphite powder and current collector into the support, and the graphite powder and current collector in the filter bag membrane form graphite. The electrode is used as either the anode or the cathode, and the ring-shaped counter electrode is the counter electrode. The two electrodes are immersed vertically into the electrolytic cell containing the electrolyte. The center of the circle is provided with a space between the two electrodes, a gap is provided between the bottom surface of the annular counter electrode and the inner bottom surface of the electrolytic cell, and the two electrodes are connected with the positive and negative electrodes of the power supply;
5）选择重物重量：根据石墨颗粒粒径以及石墨颗粒堆密度大小，确定施加重物的重量；5) Select the weight of the heavy object: according to the particle size of the graphite particles and the bulk density of the graphite particles, determine the weight of the applied heavy object;
6）电化学剥离：依据石墨粉的质量和体积，将剥离电压设置为1-60V，剥离时间为1-10h；6) Electrochemical peeling: according to the quality and volume of graphite powder, the peeling voltage is set to 1-60V, and the peeling time is 1-10h;
7）剥离结束：滤袋膜内的石墨粉剥离成石墨烯浆液，将滤袋膜内的石墨烯浆液取出存瓶。7) End of peeling: the graphite powder in the filter bag membrane is peeled off into a graphene slurry, and the graphene slurry in the filter bag membrane is taken out and stored in a bottle.
所述的电源为直流稳压电源、交流稳压电源或者是脉冲电源中的一种。The power supply is one of a DC regulated power supply, an AC regulated power supply or a pulsed power supply.
本技术方案与现有技术相比：Compared with the prior art, this technical solution:
1. 通过给石墨粉施加外部压力以及使用滤袋膜维持剥离过程中稳定的电流传输，同时可以调节石墨粉的堆密度；1. By applying external pressure to the graphite powder and using the filter bag membrane to maintain stable current transmission during the peeling process, the bulk density of the graphite powder can be adjusted at the same time;
2. 利用滤袋膜的限域作用，保证了剥离电流的连续性，使剥离脱落的部分石墨颗粒或者石墨片层进行二次剥离，提高石墨烯收率；2. Utilize the confinement effect of the filter bag membrane to ensure the continuity of the exfoliation current, so that part of the exfoliated graphite particles or graphite flakes are exfoliated twice to improve the graphene yield;
3. 避免石墨烯和石墨颗粒对阴阳电极的短路，稳定了剥离电流。3. Avoid the short circuit of graphene and graphite particles to the anode and cathode electrodes, and stabilize the exfoliation current.
这种方法，将石墨电极基体脱落的石墨颗粒最大程度地被限制在石墨基体的表面，和石墨基体保持电子电流的导通，因为脱落的石墨颗粒能继续进行电化学剥离，继续生产石墨烯，可以极大提高石墨粉电化学制备石墨烯收率的同时对产物进行有效收集。In this method, the graphite particles exfoliated from the graphite electrode substrate are confined to the surface of the graphite substrate to the greatest extent, and the electron current is maintained with the graphite substrate, because the exfoliated graphite particles can continue to be electrochemically exfoliated and continue to produce graphene. The yield of graphene electrochemically prepared by graphite powder can be greatly improved, and the product can be effectively collected.
这种方法，能够实现规模化、稳定、高效、低成本的电化学剥离石墨粉生产石墨烯，提高了石墨烯收率，稳定了剥离电流。This method can realize large-scale, stable, high-efficiency, and low-cost electrochemical exfoliation of graphite powder to produce graphene, improve the yield of graphene, and stabilize the exfoliation current.
附图说明Description of drawings
图1为实施例的结构示意图；Fig. 1 is the structural representation of embodiment;
图2为实施例中支架的结构示意图；Fig. 2 is the structural representation of the stent in the embodiment;
图3为实施例1中剥离的石墨烯与石墨烯标准卡的XRD图；Fig. 3 is the XRD pattern of the graphene peeled off in the embodiment 1 and the graphene standard card;
图4为实施例1中剥离的石墨烯的SEM图；Fig. 4 is the SEM image of the graphene peeled off in embodiment 1;
图5为实施例2中剥离的石墨烯的TEM图。FIG. 5 is a TEM image of the exfoliated graphene in Example 2. FIG.
图中，1.电解槽 2.环形对电极 3.支架 4.集流体 5.石墨粉 6.滤袋膜 7.重物8.电源 9.电解液。In the figure, 1.
具体实施方式Detailed ways
下面结合附图及具体实施例对本发明作进一步的详细描述，但不是对本发明的限定。The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments, but it is not intended to limit the present invention.
实施例：Example:
实施例1：Example 1:
参照图1、图2，一种石墨粉电化学法生产石墨烯的环形剥离装置，包括电解槽1，电解槽1内设有电解液9，电解槽1内设有环形对电极2和带网孔的支架3，环形对电极2围绕支架3，支架3内套装滤袋膜6，滤袋膜6内设有石墨粉5和集流体4, 石墨粉5和集流体4组成石墨电极，其中石墨电极与环形对电极2同圆心，环形对电极2与石墨电极之间设有间距，滤袋膜6内的石墨粉5上端设有重物7，环形对电极2和集流体4外接电源8，重物7给石墨粉5施加的压力可调控。With reference to Fig. 1, Fig. 2, a kind of annular stripping device of graphite powder electrochemical method producing graphene, comprises electrolytic cell 1, and electrolytic cell 1 is provided with electrolyte 9, and electrolytic cell 1 is provided with
所述环形对电极2为耐腐蚀金属导电材料。The
所述环形对电极2底面与电解槽1内底面之间设有间隙。A gap is provided between the bottom surface of the
所述滤袋膜6设有孔隙结构，材质耐酸耐碱耐腐蚀，滤袋膜6孔隙结构中的孔径小于石墨粉5的粒径，滤袋膜6允许电解液离子自由通过而石墨粉剥离产物被限域流动，从而提高石墨粉电化学剥离制备石墨烯的收率。The filter bag membrane 6 is provided with a pore structure, and the material is acid-resistant, alkali-resistant and corrosion-resistant. The pore size in the filter bag membrane 6 pore structure is smaller than the particle size of the graphite powder 5. The filter bag membrane 6 allows the electrolyte ions to pass freely and the graphite powder peels off the product. Confined flow, thereby improving the yield of graphene prepared by electrochemical exfoliation of graphite powder.
所述集流体4为柱状的高硬度耐腐蚀的导电材料。The
所述支架3材质耐酸耐碱耐腐蚀。The material of the
所述环形对电极2与石墨电极之间的间距为1-7cm，本例为3cm。The distance between the
一种实现石墨粉电化学法生产石墨烯的剥离方法，包括上述实现石墨粉电化学法生产石墨烯的环形剥离装置，所述方法包括如下的步骤：A peeling method for realizing the production of graphene by an electrochemical method of graphite powder, comprising the above-mentioned annular peeling device for realizing the production of graphene by an electrochemical method of graphite powder, and the method comprises the following steps:
1）选择石墨粉5材质及颗粒大小：选择人造石墨、天然石墨或是回收废旧石墨粉中的一种，石墨粉5的粒径大小在50-800目，本例选择80-100目的人造石墨粉；1) Select the material and particle size of graphite powder 5: choose one of artificial graphite, natural graphite or recycled waste graphite powder. The particle size of graphite powder 5 is 50-800 mesh, in this example, 80-100 mesh artificial graphite is selected pink;
2）选择电解液9：选择水系电解液、有机电解液、离子液体中的一种，本例选择0.1MNa2SO4的水系电解液；2) Select electrolyte 9: select one of aqueous electrolyte, organic electrolyte, and ionic liquid, in this example, choose 0.1M Na2 SO4 aqueous electrolyte;
3）选择滤袋膜6的材质以及孔径大小：根据电解液9的种类性质以及石墨粉5原材料的孔径大小选择滤袋膜6的材质以及目数，本例选择孔径大小为200目的纱布作为滤袋膜；3) Select the material and pore size of the filter bag membrane 6: According to the type and nature of the electrolyte 9 and the pore size of the graphite powder 5 raw material, the material and mesh number of the filter bag membrane 6 are selected. In this example, gauze with a pore size of 200 mesh is selected as the filter. bag film;
4）组装电剥离装置：在电解槽1内装入步骤2）选择的电解液9，将装有石墨粉5和集流体4的滤袋膜6放入支架3内，滤袋膜6内的石墨粉5和集流体4组成石墨电极作为阳极或者是阴极的任意一极，环形对电极2为对电极，将两电极垂直浸入到装有电解液9的电解槽1中，其中环形对电极2围绕支架3外围放置，环形对电极2和石墨电极保持同圆心，两电极之间设有间隔，环形对电极2底面与电解槽1内底面之间设有间隙，两电极与电源8的正负极连接；4) Assemble the electro-stripping device: put the electrolyte 9 selected in step 2) into the electrolytic cell 1, put the filter bag membrane 6 containing the graphite powder 5 and the
5）选择重物重量：根据石墨颗粒粒径以及石墨颗粒堆密度大小，确定施加重物7的重量大小，本例选择施加重物7的重量为1.5kg;5) Select the weight of the heavy object: According to the particle size of the graphite particles and the bulk density of the graphite particles, determine the weight of the applied heavy object 7. In this example, the weight of the applied heavy object 7 is selected to be 1.5kg;
6）电化学剥离：依据石墨粉5的质量和体积，将剥离电压设置为1-60V，剥离时间为1-10h，本例选择剥离电压为10V，剥离时间为3h；6) Electrochemical exfoliation: According to the mass and volume of graphite powder 5, the exfoliation voltage is set to 1-60V, and the exfoliation time is 1-10h. In this example, the exfoliation voltage is selected to be 10V, and the exfoliation time is 3h;
7）剥离结束：滤袋膜6内的石墨粉剥离成石墨烯浆液，将滤袋膜6内的石墨烯浆液取出存瓶。7) End of peeling: the graphite powder in the filter bag membrane 6 is peeled off into a graphene slurry, and the graphene slurry in the filter bag membrane 6 is taken out and stored in a bottle.
步骤4）中所述的电源8为直流稳压电源、交流稳压电源或者是脉冲电源中的一种，本例选择直流稳压电源。The power supply 8 described in step 4) is one of a DC regulated power supply, an AC regulated power supply or a pulse power supply, and in this example, a DC regulated power supply is selected.
采用本例装置和方法剥离的石墨烯与石墨烯标准卡的XRD图、SEM图分别如图3、图4所示。XRD patterns and SEM pictures of graphene and graphene standard cards exfoliated by the device and method of this example are shown in Figure 3 and Figure 4, respectively.
实施例2：Example 2:
本例选择100-120目的人造石墨粉。In this example, 100-120 mesh artificial graphite powder is selected.
本例选择0.1M (NH4)2SO4的水系电解液。In this example, an aqueous electrolyte of 0.1M (NH4 )2 SO4 is selected.
本例的剥离电压为10V，剥离时间为3h。The peeling voltage in this example was 10V, and the peeling time was 3h.
其余同实施例1。The rest are the same as in Example 1.
采用本例装置和方法剥离的石墨烯的TEM图如图5所示。The TEM image of graphene exfoliated by the device and method of this example is shown in FIG. 5 .
实施例3：Example 3:
本例选择120-140目的人造石墨粉。In this example, 120-140 mesh artificial graphite powder is selected.
本例选择孔径大小为200目的尼龙作为滤袋膜。In this example, nylon with a pore size of 200 mesh is selected as the filter bag membrane.
其余同实施例1。The rest are the same as in Example 1.
使用实施例1、实施例2、实施例3剥离出的石墨烯浆液与现有技术剥离出的石墨烯浆液相比，产量有明显提升。Compared with the graphene slurry exfoliated by the prior art, the yield of the graphene slurry exfoliated by using Example 1, Example 2, and Example 3 is significantly improved.
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