CN114180554A - Preparation method of flaky hexagonal hollow carbon material - Google Patents

Preparation method of flaky hexagonal hollow carbon material Download PDF

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Publication number
CN114180554A
CN114180554A CN202111493625.2A CN202111493625A CN114180554A CN 114180554 A CN114180554 A CN 114180554A CN 202111493625 A CN202111493625 A CN 202111493625A CN 114180554 A CN114180554 A CN 114180554A
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carbon material
flaky
magnesium oxide
hexagonal
hollow carbon
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钱进
沈绍典
刘兆鑫
胡孟
毛东森
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials

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  • Organic Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

The invention provides a preparation method of a flaky hexagonal hollow carbon material, which comprises the steps of taking flaky hexagonal magnesium oxide as a template, taking vegetable oil as a carbon source, coating the vegetable oil on the surface of the magnesium oxide, roasting and carbonizing the magnesium oxide by temperature programming under the atmosphere of nitrogen, and removing the magnesium oxide by acid to obtain the hollow two-dimensional hexagonal flaky carbon material. The preparation method has the remarkable advantages of low production cost, simplicity in operation, short production time and the like, and the prepared carbon material is hexagonal hollow, has the advantages of high dispersity, large specific surface area and the like, and can be used as a photocatalytic material or an adsorbent.

Description

Preparation method of flaky hexagonal hollow carbon material
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to a preparation method of a flaky hexagonal hollow carbon material.
Background
The micro-morphology of the nano material has important influence on the application performance of the nano material, and the performance of the nano material can be effectively improved by regulating the micro-morphology of the nano material. For example, carbon materials with developed pore structures have significant advantages when used as adsorbents; the carbon material with the two-dimensional structure or the hollow nano structure is suitable for being used as a photocatalyst carrier. Therefore, the micro morphology of the carbon material is regulated and controlled according to the application field of the carbon material, and the carbon material with different morphological characteristics is important in a plurality of research subjects of nano materials.
The hollow nano structure has huge space inside, so that the photocatalyst can generate light scattering and slow photon effect, thereby being beneficial to light absorption. Meanwhile, the structure has higher specific surface area, and can provide more active sites and larger light receiving area for the photocatalyst. Researchers have demonstrated that photocatalysts with hollow nanostructures exhibit better photocatalytic performance than solid particles. Zhuang et al, using glucose to prepare hollow carbon spheres, and then adding TiO2Covering the surface of the hollow carbon sphere to prepare TiO2A hollow carbon sphere composite photocatalyst having excellent performance in photodegradation of dyes (Zhuang Y, Sun J, Guan M. template free preparation of TiO2/C core-shell pore for high performance photo-catalysis [ J]Journal of Alloys and Compounds 2016,662: 84-88.). The strategy for preparing the carbon material by using the template is widely applied. The invention of xucauhajust et al uses the mixture of graphite phase carbon nitride precursor and carbon point precursor as precursor, and mesoporous silicon dioxide as hard template, and prepares the hollow sphere photocatalyst by in-situ thermal polymerization and template etching. The material prepared by the method shows high-efficiency photocatalytic performance under visible light (application number: 202011564729.3).
Based on the analysis, the preparation of the hollow carbon material with a specific morphology has important significance in research in the fields of light, electricity and catalysis, but documents or patents have few reports about two-dimensional hollow carbon materials.
Disclosure of Invention
The invention aims to solve the problems, and provides a preparation method of a sheet-shaped hexagonal hollow carbon material, which has the advantages of simple process and low cost, the prepared carbon material is hexagonal hollow, has high dispersibility, large specific surface area and the like, and can be used as a photocatalytic material or an adsorbent.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a flaky hexagonal hollow carbon material comprises the steps of taking flaky hexagonal magnesium oxide as a template, taking vegetable oil as a carbon source, coating the vegetable oil on the surface of the magnesium oxide, roasting and carbonizing the magnesium oxide by temperature programming under the nitrogen atmosphere, and removing the magnesium oxide by acid to obtain the hollow two-dimensional hexagonal flaky carbon material.
Further, the preparation method of the flaky hexagonal hollow carbon material specifically comprises the following steps:
(a) putting the flaky hexagonal magnesium oxide and vegetable oil with certain mass together, and stirring and mixing;
(b) heating the obtained mixture in a nitrogen atmosphere, and carbonizing at high temperature to obtain a magnesium oxide-carbon composite;
(c) adding the magnesium oxide carbon compound into acid with a certain concentration, carrying out hydrothermal reaction for a period of time, filtering, and drying to obtain the flaky hexagonal hollow carbon.
Further, the vegetable oil comprises one or more of rapeseed oil, sunflower seed oil, soybean oil, corn oil, peanut oil, olive oil and walnut oil.
Further, the mass ratio of the vegetable oil to the magnesium oxide is 1.0-2.5: 1.
Further, in the step (b), the temperature is raised to 600-800 ℃ at the speed of 1-5/min from the room temperature, and the temperature is kept for 2-4 h.
Further, the acid solution in the step (c) is 1-3 mol-1Hydrochloric acid, sulfuric acid or nitric acid.
Further, in the step (c), the mixture is hydrothermally treated at 100 ℃ for 24 hours, taken out, filtered, washed and dried at 50 ℃.
Compared with the prior art, the invention has the following beneficial effects:
in the prior art, the carbon sources which can be selected by the template method for preparing the hollow carbon material mainly comprise methane, furfuryl alcohol, glucose, asphalt, phenolic resin and the like, most of the carbon sources belong to petrochemical resources, and reports of preparing the hollow carbon by using vegetable oil as the carbon source are not found. The vegetable oil is mainly formed by one molecule of glycerol and three molecules of long-chain fatty acids containing 8-22 carbon atoms respectively, has rich sources, and is a biological resource with great application prospect. In addition, vegetable oils containing triglyceride groups are considered as precursors of synthetic polymers, and different types of polymers, including polyesters, polyamides, epoxy resins and polyurethanes, have been prepared by different polymerization reactions, such as cationic polymerization, condensation polymerization and radical copolymerization, based on vegetable oils or modified vegetable oils.
The invention takes two-dimensional sheet hexagonal magnesium oxide as a template, uses vegetable oil as a carbon source, coats the vegetable oil on the surface of the sheet hexagonal magnesium oxide to generate a polymer, and finally prepares the hollow two-dimensional hexagonal sheet carbon material through high-temperature carbonization.
Drawings
FIG. 1 is a scanning electron microscope image of the flaky hexagonal hollow carbon material prepared in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
A preparation method of a flaky hexagonal hollow carbon material comprises the following steps:
(1) mixing the sheet hexagonal magnesium oxide and vegetable oil in porcelain boat in different proportion, N2Calcining in a tubular furnace under the atmosphere to obtain MgO/C;
(2) and adding the carbonized sample into 2M hydrochloric acid, removing magnesium oxide by hydrothermal treatment, performing centrifugal separation, washing with hot water to remove magnesium chloride, filtering, and drying to obtain the flaky hexagonal hollow carbon.
Wherein the nitrogen roasting temperature is 600 ℃, the roasting time is 2 hours, and the mass ratio of the flaky hexagonal magnesium oxide to the vegetable oil is 1: 1.5; adding 50mL of 2M hydrochloric acid, carrying out hydrothermal treatment at 100 ℃ for 12h, drying at 40 ℃ for 24h, and placing in an oven.
Example 1
A preparation method of a flaky hexagonal hollow carbon material comprises the following steps: mixing hexagonal flaky magnesium oxide and peanut oil according to the proportion of 1: 2.5 proportion of N2Roasting in the atmosphere at 800 deg.C for 2 hr to obtain product in 2M hydrochloric acid solutionHydrothermal for 24h at medium 100 ℃ to obtain the hexagonal hollow carbon, wherein the SEM image of the product is shown in figure 1, and the product is flaky hexagonal hollow carbon and has regular appearance.
Example 2
A preparation method of a flaky hexagonal hollow carbon material comprises the following steps: mixing hexagonal flaky magnesium oxide and peanut oil according to the proportion of 1: 1.5, N2Roasting in the atmosphere at 800 ℃ for 2 h.
And (3) carrying out hydrothermal treatment on the roasted product in a 2M hydrochloric acid solution at 100 ℃ for 24 hours to obtain the flaky hexagonal hollow carbon.
Example 3
A preparation method of a flaky hexagonal hollow carbon material comprises the following steps: mixing hexagonal flaky magnesium oxide and rapeseed oil according to the proportion of 1: 1.5, N2Roasting in atmosphere at 850 deg.c for 2 hr.
And (3) carrying out hydrothermal treatment on the roasted product in a 3.0M sulfuric acid solution at 100 ℃ for 24 hours to obtain the flaky hexagonal hollow carbon.
Example 4
A preparation method of a flaky hexagonal hollow carbon material comprises the following steps: mixing hexagonal flaky magnesium oxide and olive oil according to the weight ratio of 1: 1, N2Roasting in the atmosphere at 900 ℃ for 2 h. And (3) carrying out hydrothermal treatment on the roasted product in a 1.0M nitric acid solution at 100 ℃ for 24 hours to obtain the flaky hexagonal hollow carbon.
Example 5
A preparation method of a flaky hexagonal hollow carbon material comprises the following steps: mixing hexagonal flaky magnesium oxide and walnut oil according to the proportion of 1: 2, N2Roasting in the atmosphere at 800 ℃ for 2 h. Hydrothermal reaction of the product obtained after roasting in 2.0M hydrochloric acid solution at 100 ℃ for 24 hours to obtain the flaky hexagonal hollow carbon.
Example 6
A preparation method of a flaky hexagonal hollow carbon material comprises the following steps: mixing hexagonal flaky magnesium oxide and corn oil according to the weight ratio of 1: 2.5 proportion of N2Roasting in the atmosphere at 900 ℃ for 2 h. RoastingThen the obtained product is hydrothermally treated in 2.0M hydrochloric acid solution for 24 hours at 100 ℃ to obtain the flaky hexagonal hollow carbon.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (7)

1. A preparation method of a flaky hexagonal hollow carbon material is characterized in that flaky hexagonal magnesium oxide is used as a template, vegetable oil is used as a carbon source, the surface of the magnesium oxide is coated with the vegetable oil, the mixture is roasted and carbonized through temperature programming under the nitrogen atmosphere, and then the magnesium oxide is removed through acid, so that the hollow two-dimensional hexagonal flaky carbon material is obtained.
2. The method for preparing the flaky hexagonal hollow carbon material according to claim 1, which specifically comprises the following steps:
(a) putting the flaky hexagonal magnesium oxide and vegetable oil with certain mass together, and stirring and mixing;
(b) heating the obtained mixture in a nitrogen atmosphere, and carbonizing at high temperature to obtain a magnesium oxide-carbon composite;
(c) adding the magnesium oxide carbon compound into acid with a certain concentration, carrying out hydrothermal reaction for a period of time, filtering, and drying to obtain the flaky hexagonal hollow carbon.
3. The method for preparing a sheet-like hexagonal hollow carbon material according to claim 2, wherein the vegetable oil comprises one or more of rapeseed oil, sunflower seed oil, soybean oil, corn oil, peanut oil, olive oil, and walnut oil.
4. The method for preparing a sheet-like hexagonal hollow carbon material according to claim 2, wherein the mass ratio of the vegetable oil to the magnesium oxide is 1.0-2.5: 1.
5. The method for preparing a sheet-like hexagonal hollow carbon material according to claim 2, wherein the temperature in step (b) is raised from room temperature to 600 ℃ to 800 ℃ at a rate of 1 to 5/min and maintained for 2 to 4 hours.
6. The method for preparing a sheet-shaped hexagonal hollow carbon material according to claim 2, wherein the acid solution in the step (c) is 1 to 3mol-1Hydrochloric acid, sulfuric acid or nitric acid.
7. The method for preparing a flaky hexagonal hollow carbon material according to claim 2, wherein the hydrothermal treatment is carried out at 100 ℃ for 24 hours in the step (c), and the flaky hexagonal hollow carbon material is taken out, filtered, washed and dried at 50 ℃.
CN202111493625.2A 2021-12-08 2021-12-08 Preparation method of flaky hexagonal hollow carbon material Pending CN114180554A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080089828A1 (en) * 2004-09-22 2008-04-17 Showa Denko K.K. Method for Producing Vapor Grown Carbon Nanotube
CN104528704A (en) * 2014-12-29 2015-04-22 上海理工大学 Preparing method for graphitized ordered mesoporous carbon material
JP2018047421A (en) * 2016-09-21 2018-03-29 株式会社 ユーテックアプライ Carbon-carrying porous adsorbent for dioxins, heavy metals, and radioactive substances
CN112194112A (en) * 2020-08-10 2021-01-08 中国石油大学(北京) High-capacitance hierarchical pore carbon material and preparation method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080089828A1 (en) * 2004-09-22 2008-04-17 Showa Denko K.K. Method for Producing Vapor Grown Carbon Nanotube
CN104528704A (en) * 2014-12-29 2015-04-22 上海理工大学 Preparing method for graphitized ordered mesoporous carbon material
JP2018047421A (en) * 2016-09-21 2018-03-29 株式会社 ユーテックアプライ Carbon-carrying porous adsorbent for dioxins, heavy metals, and radioactive substances
CN112194112A (en) * 2020-08-10 2021-01-08 中国石油大学(北京) High-capacitance hierarchical pore carbon material and preparation method and application thereof

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