WO2020220591A1 - Preparation method for carbon nanocage material - Google Patents
Preparation method for carbon nanocage material Download PDFInfo
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- WO2020220591A1 WO2020220591A1 PCT/CN2019/110427 CN2019110427W WO2020220591A1 WO 2020220591 A1 WO2020220591 A1 WO 2020220591A1 CN 2019110427 W CN2019110427 W CN 2019110427W WO 2020220591 A1 WO2020220591 A1 WO 2020220591A1
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- potassium chloride
- carbon
- inert gas
- ball
- tube furnace
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
Definitions
- the invention belongs to the technical field of carbon nano materials, and specifically relates to a method for preparing a carbon nano cage material.
- Carbon nanocages are cage-like carbon nanomaterials formed by crimping carbon layers. As a new type of low-dimensional carbon nanomaterials, they have received more and more attention.
- carbon nanocage preparation methods include metal reduction method, carbon evaporation method, catalytic pyrolysis method, benzene flame combustion method, conversion of nitrogen-containing inorganic substances, etc., but these methods have high cost, complex process or used The reagent is corrosive and toxic. The development of a cheap, non-toxic, low-energy-consumption carbon nanomaterial preparation method is the goal pursued by researchers.
- the purpose of the present invention is to provide a method for preparing carbon nanocage materials, which has easy-to-obtain raw materials and low cost, and the preparation process is environmentally friendly and does not have toxicity or corrosiveness. ...
- the preparation method of the carbon nanocage material of the present invention specifically includes the following steps:
- Sugar is one of sucrose or glucose. ...
- the mass ratio of sugar to potassium chloride is controlled at 0.01-100:1. ...
- the mass ratio of ball to material is controlled at 1 ⁇ 100:1. ...
- the time of ball milling is 0.1-12h. ...
- the inert gas is one or more of nitrogen, argon or helium, and the flow rate of the inert gas in the tube furnace is 20-100 mL min -1 .
- the heating rate of the tube furnace is 5 ⁇ 20°C ⁇ min -1 .
- the immersion time in the aqueous solution is 0.1-24h, and the immersion is hot water, and the temperature of the hot water is 20-100°C.
- the present invention uses sugar as the carbon source and potassium chloride as the template.
- the raw materials are cheap, non-toxic and non-polluting.
- the two are uniformly mixed by ball milling in a ball milling tank. After ball milling, it is easy to wrap the sugar in the
- the potassium surface is then carbonized at a high temperature under inert gas. When removing the hard template potassium chloride, no acid or lye is needed. Just dissolve and remove the potassium chloride with water.
- the whole preparation process is green and pollution-free, and suitable Industrial large-scale preparation;
- the carbon nanocage material prepared by the present invention has a uniform characteristic with a size of 500 nm, and the specific surface area of the prepared carbon nanocage material can reach 580 m 2 ⁇ g -1 .
- the prepared carbon nanocage material has high specific surface area, hierarchical porous structure and graphitized carbon component, so it has good conductivity and good electrolyte ion transport performance.
- the prepared carbon nanocage material has a specific surface area of 580m 2 ⁇ g -1 ;
- the prepared carbon nanocage material has a wide diffraction peak at 26°, indicating that the material has a low degree of graphitization
- the prepared carbon nanocage material cage has a uniform size, and the size is about 500 nm.
Abstract
The present invention relates to the technical field of carbon nanomaterials, and specifically relates to a preparation method for a carbon nanocage material. The method comprises: a carbohydrate is used as a carbon source, and potassium chloride is used as a template, so that the raw materials are cheap, nontoxic, and pollution-free; the carbohydrate and potassium chloride are uniformly ball-milled and mixed in a ball milling pot; after ball milling, the carbohydrate is easily wrapped on the surface of potassium chloride, and then high-temperature carbonization is performed under an inert gas, so that an acid liquor or an alkali liquor is not required when hard template potassium chloride is removed, and only water is required to dissolve and remove potassium chloride. The whole preparation process is green and pollution-free, and is applicable for industrial large-scale preparation.
Description
本发明属于碳纳米材料技术领域，具体涉及一种碳纳米笼材料的制备方法。The invention belongs to the technical field of carbon nano materials, and specifically relates to a method for preparing a carbon nano cage material.
碳在元素周期表中排第六位，是自然界分布广泛的元素，也是目前最重要的、最使人着迷的元素之一。碳纳米材料有很多，其中重要的是零维的富勒烯、一维的碳纳米管和二维的石墨烯。这些碳纳米材料不仅能够稳定存在，而且具有很多令人惊奇的性质。广泛应用于储能、催化、电子、环境等多个领域。但是富勒烯、碳纳米管、石墨烯这三种材料制备工艺复杂、结构可控性差，产品纯度不高，因此很难具有商业规模的应用。Carbon ranks sixth in the periodic table. It is an element widely distributed in nature and one of the most important and fascinating elements at present. There are many carbon nanomaterials, among which the most important are zero-dimensional fullerenes, one-dimensional carbon nanotubes and two-dimensional graphene. These carbon nanomaterials can not only exist stably, but also have many surprising properties. It is widely used in energy storage, catalysis, electronics, environment and other fields. However, the three materials, fullerene, carbon nanotube, and graphene, have complex preparation processes, poor structural controllability, and low product purity, so it is difficult to have commercial-scale applications.
碳纳米笼是由碳层卷曲形成的笼状结构的纳米碳材料，作为一种新型的低维碳纳米材料受到越来越广泛的关注。现有技术中碳纳米笼制备方法有金属还原法、碳蒸发法、催化热解法、苯火焰燃烧法、含氮无机物的转化等，但是这些方法都存在成本高、工艺复杂或者所使用的试剂腐蚀性和毒性较强等。发展一种廉价、无毒、低耗能的碳纳米材料制备方法是研究者共同追求的目标。Carbon nanocages are cage-like carbon nanomaterials formed by crimping carbon layers. As a new type of low-dimensional carbon nanomaterials, they have received more and more attention. In the prior art, carbon nanocage preparation methods include metal reduction method, carbon evaporation method, catalytic pyrolysis method, benzene flame combustion method, conversion of nitrogen-containing inorganic substances, etc., but these methods have high cost, complex process or used The reagent is corrosive and toxic. The development of a cheap, non-toxic, low-energy-consumption carbon nanomaterial preparation method is the goal pursued by researchers.
针对以上技术问题，本发明目的在于提供一种碳纳米笼材料的制备方法，原料易得成本低，制备过程绿色环保，不存在有毒性或腐蚀性。
In view of the above technical problems, the purpose of the present invention is to provide a method for preparing carbon nanocage materials, which has easy-to-obtain raw materials and low cost, and the preparation process is environmentally friendly and does not have toxicity or corrosiveness. …
本发明所述的碳纳米笼材料的制备方法，具体包括如下步骤：
The preparation method of the carbon nanocage material of the present invention specifically includes the following steps:
(1)以糖类、氯化钾为原料，置于球磨罐中球磨得固体粉末；
(1) Using sugar and potassium chloride as raw materials, ball milling in a ball mill tank to obtain solid powder;
(2)将固体粉末置于石英舟中，然后放入装有石英管的管式炉中，通入惰性气体，升温至500～1000℃，保温0.1-24h，冷却至室温，得初产物；
(2) Put the solid powder in a quartz boat, and then put it into a tube furnace equipped with a quartz tube, pass in inert gas, heat up to 500-1000°C, keep for 0.1-24h, and cool to room temperature to obtain the initial product;
(3)将初产物投入水中浸泡，过滤、烘干得成品。
(3) Put the initial product into water to soak, filter and dry to obtain the finished product. …
糖类为蔗糖或葡萄糖中的一种。 Sugar is one of sucrose or glucose. …
糖类与氯化钾的质量比控制在0.01～100：1。
The mass ratio of sugar to potassium chloride is controlled at 0.01-100:1. …
球磨时球、料质量比控制在1～100:1。
During ball milling, the mass ratio of ball to material is controlled at 1～100:1. …
球磨的时间为0.1-12h。 The time of ball milling is 0.1-12h. …
惰性气体为氮气、氩气或氦气中的一种或多种，惰性气体在管式炉中的流速在20～100mL min
-1。
The inert gas is one or more of nitrogen, argon or helium, and the flow rate of the inert gas in the tube furnace is 20-100 mL min -1 .
管式炉升温速率为5～20℃·min
-1。
The heating rate of the tube furnace is 5～20℃·min -1 .
水溶液中浸泡的时间为0.1～24h，浸泡时为热水，热水温度为20-100℃。The immersion time in the aqueous solution is 0.1-24h, and the immersion is hot water, and the temperature of the hot water is 20-100°C.
(1)本发明以糖类为碳源，以氯化钾为模版，原料廉价、无毒、无污染，二者在球磨罐中球磨混合均匀，经过球磨后，很容易将糖包裹于氯化钾表面，然后在惰性气体下进行高温碳化，去除硬模板氯化钾时不需要用到酸液或者碱液，只需用水将氯化钾溶解去除即可，整个制备过程绿色无污染，并且适合工业大规模制备；
(1) The present invention uses sugar as the carbon source and potassium chloride as the template. The raw materials are cheap, non-toxic and non-polluting. The two are uniformly mixed by ball milling in a ball milling tank. After ball milling, it is easy to wrap the sugar in the The potassium surface is then carbonized at a high temperature under inert gas. When removing the hard template potassium chloride, no acid or lye is needed. Just dissolve and remove the potassium chloride with water. The whole preparation process is green and pollution-free, and suitable Industrial large-scale preparation;
(2)本发明所制备的碳纳米笼材料，具有尺寸为500nm的均一特性，所制备的碳纳米笼材料比表面积可达580m
2·g
-1。所制得碳纳米笼材料具备高的比表面积、分级多孔结构以及石墨化碳成分，因此具有良好的导电性和良好的电解质离子传输性能。
(2) The carbon nanocage material prepared by the present invention has a uniform characteristic with a size of 500 nm, and the specific surface area of the prepared carbon nanocage material can reach 580 m 2 ·g -1 . The prepared carbon nanocage material has high specific surface area, hierarchical porous structure and graphitized carbon component, so it has good conductivity and good electrolyte ion transport performance.
图1、实施例1所制得的碳纳米笼材料的氮气吸附-脱附曲线；
Figure 1. Nitrogen adsorption-desorption curve of the carbon nanocage material prepared in Example 1;
图2、实施例1所制得的碳纳米笼材料的XRD图；
Figure 2. XRD pattern of the carbon nanocage material prepared in Example 1;
图3、实施例1所制得的碳纳米笼材料的扫描电镜图片(SEM)。
Figure 3. Scanning electron micrograph (SEM) of the carbon nanocage material prepared in Example 1. …
如图1所示，所制得的碳纳米笼材料比表面积为580m
2·g
-1；
As shown in Figure 1, the prepared carbon nanocage material has a specific surface area of 580m 2 ·g -1 ;
如图2所示，所制得的碳纳米笼材料在26°处出现较宽的衍射峰，说明此材料石墨化程度较低；
As shown in Figure 2, the prepared carbon nanocage material has a wide diffraction peak at 26°, indicating that the material has a low degree of graphitization;
如图3所示，所制得的碳纳米笼材料笼尺寸均匀，尺寸大小在500nm左右。As shown in Fig. 3, the prepared carbon nanocage material cage has a uniform size, and the size is about 500 nm.
下面结合实施例和说明书附图对本发明做进一步说明。
The present invention will be further described below in conjunction with the embodiments and the drawings of the specification. …
实施例1
Embodiment 1
,
称取2g蔗糖、10g氯化钾放入聚四氟球磨罐中，然后称取质量100g的玛瑙球放入球磨罐中，球磨4h。将球磨后的固体粉末置于石英舟内，然后放入装有石英管的管式炉中；通入氮气惰性气体，惰性气体在管式炉中的流速在50mLmin
-1，然后以5℃min
-1的升温速率将温度升至800℃，高温碳化保温时间为2h，得初产物。将得到的初产物用热水浸泡处理8h，然后抽滤，置于烘箱中80℃下干燥24h，得到碳纳米笼材料。
Weigh 2g of sucrose and 10g of potassium chloride into a polytetrafluoroethylene ball mill pot, then weigh 100g of agate balls into the ball mill pot, and ball mill for 4 hours. Put the ball-milled solid powder in a quartz boat, and then put it into a tube furnace equipped with a quartz tube; pass nitrogen inert gas, the flow rate of the inert gas in the tube furnace is 50mLmin -1 , and then at 5℃min The temperature rise rate of -1 raises the temperature to 800°C, the high temperature carbonization holding time is 2h, and the initial product is obtained. The obtained initial product was immersed in hot water for 8 hours, then suction filtered, and dried in an oven at 80° C. for 24 hours to obtain a carbon nanocage material.
实施例2
Example 2
...
称取1g蔗糖、18g氯化钾放入聚四氟球磨罐中，然后称取质量50g的玛瑙球放入球磨罐中，球磨0.5h。将球磨后的固体粉末置于石英舟内，然后放入装有石英管的管式炉中；通入氮气惰性气体，惰性气体在管式炉中的流速在60mLmin
-1，然后以10℃min
-1的升温速率将温度升至700℃，高温碳化保温时间为4h，得初产物。将得到的初产物用热水浸泡处理10h，然后抽滤，置于烘箱中80℃下干燥24h，得到碳纳米笼材料。
Weigh 1g of sucrose and 18g of potassium chloride into a polytetrafluoroethylene ball mill tank, then weigh 50g of agate balls into the ball mill tank, and ball mill for 0.5h. Put the ball-milled solid powder in a quartz boat, and then put it into a tube furnace equipped with a quartz tube; pass nitrogen inert gas, the flow rate of the inert gas in the tube furnace is 60mLmin -1 , and then at 10℃min The heating rate of -1 raises the temperature to 700°C, and the high-temperature carbonization holding time is 4h to obtain the initial product. The obtained initial product was immersed in hot water for 10 hours, then filtered by suction, and dried in an oven at 80° C. for 24 hours to obtain a carbon nanocage material.
实施例3
Example 3
称取2g葡糖糖、1g氯化钾放入聚四氟球磨罐中，然后称取质量200g的玛瑙球放入球磨罐中，球磨4h。将球磨后的固体粉末置于石英舟内，然后放入装有石英管的管式炉中；通入氮气惰性气体，惰性气体在管式炉中的流速在80mLmin
-1，然后以5℃min
-1的升温速率将温度升至600℃，高温碳化保温时间为2h，得初产物。将得到的初产物用热水浸泡处理8h，然后抽滤，置于烘箱中80℃下干燥24h，得到碳纳米笼材料。
Weigh 2g glucose and 1g potassium chloride into a polytetrafluoroethylene ball mill jar, then weigh 200g agate balls into the ball mill jar and ball mill for 4 hours. Put the ball-milled solid powder in a quartz boat, and then put it into a tube furnace equipped with a quartz tube; pass nitrogen inert gas, the flow rate of the inert gas in the tube furnace is 80mLmin -1 , then at 5℃min The heating rate of -1 raises the temperature to 600°C, and the high-temperature carbonization holding time is 2h to obtain the initial product. The obtained initial product was immersed in hot water for 8 hours, then suction filtered, and dried in an oven at 80° C. for 24 hours to obtain a carbon nanocage material.
实施例4
Embodiment 4
称取10g蔗糖、10g氯化钾放入聚四氟球磨罐中，然后称取质量80g的玛瑙球放入球磨罐中，球磨6h。将球磨后的固体粉末置于石英舟内，然后放入装有石英管的管式炉中；通入氮气惰性气体，惰性气体在管式炉中的流速在90mLmin
-1，然后以2℃min
-1的升温速率将温度升至900℃，高温碳化保温时间为0.5h，得初产物。将得到的产物用热水浸泡处理2h，然后抽滤，置于烘箱中80℃下干燥24h，得到碳纳米笼材料。
Weigh 10g of sucrose and 10g of potassium chloride into a polytetrafluoroethylene ball mill tank, and then weigh 80g of agate balls into the ball mill tank and mill for 6 hours. Put the ball-milled solid powder in a quartz boat, and then put it into a tube furnace equipped with a quartz tube; pass nitrogen inert gas, the flow rate of the inert gas in the tube furnace is 90mLmin -1 , and then at 2℃min The temperature rise rate of -1 raises the temperature to 900°C, the high temperature carbonization holding time is 0.5h, and the initial product is obtained. The obtained product was immersed in hot water for 2 hours, then filtered by suction, and dried in an oven at 80° C. for 24 hours to obtain a carbon nanocage material.
实施例5
Embodiment 5
称取1g葡萄糖、100g氯化钾放入聚四氟球磨罐中，然后称取质量0.9g的玛瑙球放入球磨罐中，球磨0.1h。将球磨后的固体粉末置于石英舟内，然后放入装有石英管的管式炉中；通入氮气惰性气体，惰性气体在管式炉中的流速在100mLmin
-1，然后以20℃min
-1的升温速率将温度升至500℃，高温碳化保温时间为0.1h，得初产物。将得到的产物用热水浸泡处理 0.1h，然后抽滤，置于烘箱中80℃下干燥24h，得到碳纳米笼材料。
Weigh 1g glucose and 100g potassium chloride into a polytetrafluoroethylene ball mill tank, then weigh 0.9g agate balls into the ball mill tank and mill for 0.1h. Put the ball-milled solid powder in a quartz boat, and then put it into a tube furnace equipped with a quartz tube; pass nitrogen inert gas, the flow rate of the inert gas in the tube furnace is 100mLmin -1 , and then at 20℃min The heating rate of -1 raises the temperature to 500°C, and the high-temperature carbonization holding time is 0.1h to obtain the initial product. The obtained product was immersed in hot water for 0.1 h, then filtered by suction, and dried in an oven at 80° C. for 24 h to obtain a carbon nanocage material.
实施例6
Example 6
称取10g蔗糖、0.1g氯化钾放入聚四氟球磨罐中，然后称取质量101g的玛瑙球放入球磨罐中，球磨12h。将球磨后的固体粉末置于石英舟内，然后放入装有石英管的管式炉中；通入氮气惰性气体，惰性气体在管式炉中的流速在70mL min
-1，然后以17℃min
-1的升温速率将温度升至1000℃，高温碳化保温时间为24h，得初产物。将得到的产物用热水浸泡处理24h，然后抽滤，置于烘箱中80℃下干燥24h，得到碳纳米笼材料。
Weigh 10g of sucrose and 0.1g of potassium chloride into a polytetrafluoroethylene ball mill pot, then weigh 101g of agate balls into the ball mill pot and mill for 12 hours. Put the ball-milled solid powder in a quartz boat, and then put it into a tube furnace equipped with a quartz tube; pass nitrogen inert gas, the flow rate of the inert gas in the tube furnace is 70mL min -1 , and then at 17℃ The heating rate of min -1 raises the temperature to 1000°C, and the holding time for high-temperature carbonization is 24h to obtain the initial product. The obtained product was immersed in hot water for 24 hours, then filtered by suction, and dried in an oven at 80° C. for 24 hours to obtain a carbon nanocage material.
Claims (1)
- 一种碳纳米笼材料的制备方法，其特征在于包括以下步骤：A preparation method of carbon nano cage material is characterized by comprising the following steps:(1)以糖类、氯化钾为原料，置于球磨罐中球磨得固体粉末；(1) Take sugar and potassium chloride as raw materials, and place them in a ball mill tank to obtain solid powder;(2)将固体粉末置于石英舟中，然后放入装有石英管的管式炉中，通入惰性气体，升温至500～1000℃，保温0.1-24h，冷却至室温，得初产物；(2) Put the solid powder in a quartz boat, and then put it into a tube furnace equipped with a quartz tube, pass in inert gas, heat up to 500-1000°C, keep for 0.1-24h, and cool to room temperature to obtain the initial product;(3)将初产物投入水中浸泡，过滤、烘干得成品；(3) Put the initial product into water to soak, filter and dry to obtain the finished product;步骤（1）中，所述糖类为蔗糖或葡萄糖中的一种；糖类与氯化钾的质量比控制在0.01～100:1；In step (1), the sugar is one of sucrose or glucose; the mass ratio of sugar to potassium chloride is controlled at 0.01-100:1;在球磨罐中球磨时球、料质量比控制在1～100:1；球磨的时间为0.1-12h；In the ball milling tank, the mass ratio of ball to material is controlled at 1～100:1; the time of ball milling is 0.1-12h;步骤（2）中，所通入的惰性气体为氮气、氩气或氦气中的一种或多种，惰性气体在管式炉中的流速在20～100mL·min -1； In step (2), the inert gas introduced is one or more of nitrogen, argon or helium, and the flow rate of the inert gas in the tube furnace is 20-100 mL·min -1 ;管式炉升温速率为5～20℃·min -1； The heating rate of the tube furnace is 5～20℃·min -1 ;步骤（3）中，所述初产物在水中浸泡的时间为0.1～24h，浸泡时水的温度为20～100℃。In step (3), the time for the initial product to be soaked in water is 0.1-24h, and the temperature of the water during soaking is 20-100°C.
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| CN108529596A (en) * | 2018-07-20 | 2018-09-14 | 广东工业大学 | A kind of preparation method of dimensional thinlayer carbon |
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- 2019-04-30 CN CN201910360946.1A patent/CN110078051B/en active Active
- 2019-10-10 WO PCT/CN2019/110427 patent/WO2020220591A1/en active Application Filing
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| CN107177399A (en) * | 2017-06-01 | 2017-09-19 | 吴锋 | A kind of preparation technology of high concentration high stable wear resistence graphene lube oil additive |
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| CN110078051A (en) | 2019-08-02 |
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