CN110980665A - Preparation method of two-dimensional thin-layer structure carbon nitride - Google Patents
Preparation method of two-dimensional thin-layer structure carbon nitride Download PDFInfo
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- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 claims description 11
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B01J35/39—
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- B01J35/61—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The invention discloses a preparation method of two-dimensional thin-layer structure carbon nitride, which comprises the steps of dissolving melamine and glycero-phosphatidylcholine in deionized water, and placing the mixture in a hydrothermal kettle for hydrothermal reaction to obtain a mixture solution; centrifuging and washing the mixture solution, and drying to obtain a solid substance; adding KOH into the solid to obtain a solid mixture; mixing carbon fibers with the solid mixture according to the mass ratio (0.01-0.1) of 1 to the solid mixture, placing the mixture into a crucible, placing the crucible into a microwave oven resonant cavity, heating in vacuum, and cooling to room temperature to obtain a heated product; and washing and drying the heated product to obtain the carbon nitride with the two-dimensional thin-layer structure. The method has high stripping yield and short time consumption, and can solve the problem of pollution in the stripping process.
Description
Technical Field
The invention belongs to the technical field of material chemistry, and relates to a preparation method of two-dimensional thin-layer structure carbon nitride.
Background
With the increasing environmental pollution and the excessive use of high pollution energy sources such as fossil energy, the development of an environment-friendly clean energy source is the focus of attention. Graphite phase carbon nitride (g-C)3N4) The method has the advantages of wide precursor source, simple and convenient preparation method, no toxicity, high photochemical stability and suitable energy band structure, can realize the photocatalytic hydrogen production and the like, and has actively and widely researched in the field of photocatalytic water decomposition. However, carbon nitride synthesized by a general calcination method or the like is generally bulk and in a block shape, and the block-shaped carbon nitride has problems of limited absorption capacity for visible light, small specific surface area, few photocatalytic reaction active sites, low capability of separating and utilizing photogenerated charges, and the like due to weak van der Waals force in and between layers, and the like, and the g-C is limited by the defects3N4The development of (1). In order to solve the above problems, an effective method is to synthesize two-dimensional layered carbon nitride, increase the specific surface area by reducing the number of layers of carbon nitride, weaken the van der waals force between layers, enhance the transmission and separation efficiency of photo-generated charges, and enhance the visible light response range, thereby improving the photocatalytic performance [ marcheng, liu jian, welcoming spring, preparation of two-dimensional graphite-phase carbon nitride nanosheets, and research progress in the field of photocatalysis [ J ] of]Application chemistry, 2019,36(03):22-31.]。
At present g-C3N4The preparation method of the nano sheet mainly comprises the following steps: thermal oxidation stripping method [ Yan S C, Li Z S, Zou ZG. Photodiffusion performance of g-C3N4 patterned by direct lift amine [ J ]].Langmuir,2009,25(17):10397-10401.][Li Y,Jin R,Xing Y,etal.Macroscopic foam-like holey ultrathin g-C3N4 nanosheets for drasticimprovement of visible-light photocatalytic activity[J].Advanced EnergyMaterials,2016,6(24):1601273.]And liquid phase stripping method [ Liang Q, Li Z, Bai Y, et almonolayer carbon nitride nanosheets for highly improved photoresponsefor cell imaging and photocatalysis[J].Science China Materials,2017,60(2):109-118.]AFM research on dispersion of carbon nitride exfoliated by Zhudonbo, Liuhui, Shao Xiang in solution method on various substrates [ J]Chemical notification (printing plate), 2017(2017, 11):1036-1042.]Chemical stripping method [ Zhang X, Luo X, Zheng X, et al.Protonation-Assisted ionization of N-contacting 2D Conjugated Polymers [ J ]].Small,2019:1903643.][ Li Jiaojiao, Zhao Wei Feng, Zhang Shi, et al concentrated sulfuric acid method for fast preparing protonized g-C3N4 nanobelt and research on ultraviolet light catalytic degradation of organic dye [ J]Higher school chemical newspaper, 2018,39(12).]And so on. The preparation methods have respective advantages, but the hot oxygen etching method has the defects of simple operation and low stripping yield and poor effect; the liquid phase stripping method is generally combined with the ultrasonic, the stripping effect is improved, but the time consumption is longer; chemical stripping is rapid but uses various strong acids to strip and causes great environmental pollution.
Disclosure of Invention
The invention aims to provide a preparation method of two-dimensional thin-layer structure carbon nitride, which has high stripping yield and short time consumption and solves the problem of pollution in the stripping process.
The invention is realized by the following technical scheme:
a preparation method of carbon nitride with a two-dimensional thin-layer structure comprises the following steps:
step 1: 1g of melamine was taken and mixed with 1: (1.38-2.56) dissolving melamine and glycerol phosphatidylcholine in 60-120 ml of deionized water to obtain a mixture solution, placing the mixture solution in a hydrothermal kettle, performing hydrothermal reaction at 180-240 ℃, centrifuging, washing and drying to obtain a solid substance;
step 2: adding 0.02-0.1 g of KOH into the solid to obtain a solid mixture; then taking carbon fibers according to the mass ratio (0.01-0.1) of the solid to the carbon fibers, mixing the carbon fibers with the solid mixture, placing the mixture into a crucible, placing the crucible into a resonant cavity of a microwave oven, heating the mixture in vacuum at 500-560 ℃, and cooling the mixture to room temperature to obtain a heated product;
and step 3: and washing and drying the heated product to obtain the carbon nitride with the two-dimensional thin-layer structure.
Further, in the step 1, the melamine and the glycerol phosphatidylcholine are dissolved in the deionized water and then are continuously stirred for 15-60 min.
Further, in the step 1, the lining of the hydrothermal kettle is made of polytetrafluoroethylene, and the hydrothermal reaction time is 10-24 hours.
Further, in the step 1, deionized water is adopted for washing for 3-5 times.
Further, in the step 1, drying is carried out at 60-100 ℃ for 9-12 h.
Further, the microwave power in the resonant cavity of the microwave oven during vacuum heating in the step 2 is 1-5 kW.
Further, the vacuum degree of vacuum heating in the step 2 is less than 1 multiplied by 104Pa。
Further, the vacuum heating time in the step 2 is 10-120 min.
Further, in the step 3, washing is carried out for 2-3 times by adopting absolute ethyl alcohol.
Further, in the step 3, the drying is carried out for 2-6 hours at 35-60 ℃ in vacuum, and the vacuum degree of the vacuum drying is 10-3～10-1Pa。
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a preparation method of two-dimensional thin-layer structure carbon nitride, which combines P atom doping and nitrogen defect to prepare the two-dimensional thin-layer structure carbon nitride, weakens the van der Waals force between layers by element doping, and introduces the nitrogen defect in situ to enable the prepared g-C3N4The visible light response range is enlarged, and simultaneously, the doped non-metal element P is utilized to weaken the van der Waals force between layers and increase the migration rate of electrons between the layers, so that the high-efficiency organic silicon solar cell has excellent charge transmission and separation efficiency, more active edge sites and improved stripping yield; in addition, the preparation process combines a hydrothermal alkali auxiliary method and a microwave irradiation method to rapidly heat and fire the product, and the g-C containing nitrogen defects is prepared by simple one-step synthesis3N4Material, preparation methodThe method has the advantages of simple process control, short time consumption, lower cost, suitability for large-scale production, improved stripping yield, avoidance of use of dangerous goods such as strong acid in the preparation process, and remarkable advantages in safety and environmental protection; the g-C synthesized by the microwave irradiation method has the characteristic of rapid temperature rise and heating3N4The specific surface area is greatly increased, and the energy consumption is effectively reduced.
Drawings
FIG. 1 is an X-ray diffraction XRD pattern of two-dimensional thin-layer structured carbon nitride prepared in example 2;
fig. 2 is a scanning electron microscope SEM image of the two-dimensional thin-layer structure carbon nitride prepared in example 2.
Detailed Description
Specific examples are given below.
Example 1
A preparation method of carbon nitride with a two-dimensional thin-layer structure comprises the following steps:
step 1: 1g of melamine was taken and mixed with 1: dissolving melamine and glycerol phosphatidylcholine in 60ml of deionized water according to the molar ratio of 1.38, continuously stirring for 15min until the melamine and the glycerol phosphatidylcholine are completely dissolved to obtain a mixture solution, then placing the mixture solution into a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 180 ℃ for 10h, centrifuging, washing for 3 times by using deionized water, and drying at 60 ℃ for 12h to obtain a solid;
step 2: adding 0.02g of KOH into the solid to obtain a solid mixture; then taking carbon fiber according to the mass ratio of the solid to the carbon fiber of 0.01:1, mechanically mixing the carbon fiber with the solid mixture to obtain a raw material, placing the raw material into a 500mL corundum crucible, covering the corundum crucible, placing the corundum crucible into a resonant cavity of an NJZ-10 type microwave oven, and vacuumizing the resonant cavity to 1 x 10 by adopting a water ring pump4Below Pa, performing irradiation treatment on the raw materials by a microwave oven resonant cavity under the microwave power of 2kW, rapidly heating the microwave oven resonant cavity to 500 ℃, then performing vacuum heating for 10min at 500 ℃, and cooling to room temperature to obtain a heated product;
and step 3: washing the heated product with anhydrous ethanol for 2 times, and vacuum degree of 10-2Pa vacuum drying oven at 35Vacuum drying at the temperature of 2 hours to obtain the carbon nitride with the two-dimensional thin-layer structure.
Example 2
A preparation method of carbon nitride with a two-dimensional thin-layer structure comprises the following steps:
step 1: 1g of melamine was taken and mixed with 1: dissolving melamine and glycerol phosphatidylcholine in 80ml of deionized water according to the molar ratio of 1.58, continuously stirring for 30min until the melamine and the glycerol phosphatidylcholine are completely dissolved to obtain a mixture solution, then placing the mixture solution into a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 200 ℃ for 15h, centrifuging, washing for 4 times by using deionized water, and drying at 70 ℃ for 11h to obtain a solid;
step 2: adding 0.05g of KOH into the solid to obtain a solid mixture; then taking carbon fibers according to the mass ratio of the solid to the carbon fibers of 0.018:1, mechanically mixing the carbon fibers with the solid mixture to obtain a raw material, placing the raw material into a 500mL corundum crucible, covering the corundum crucible, placing the corundum crucible into a resonant cavity of an NJZ-10 type microwave oven, and vacuumizing the resonant cavity to 1 x 10 by using a water ring pump4Below Pa, performing irradiation treatment on the raw materials by a microwave oven resonant cavity under the microwave power of 4kW, rapidly heating the microwave oven resonant cavity to 550 ℃, then performing vacuum heating for 60min at 550 ℃, and cooling to room temperature to obtain a heated product;
and step 3: washing the heated product with anhydrous ethanol for 3 times, and vacuum degree of 10-3And (3) carrying out vacuum drying for 4h in a vacuum drying oven of Pa at the temperature of 50 ℃ to obtain the carbon nitride with the two-dimensional thin-layer structure.
From FIG. 1, it can be observed that the two typical characteristic peaks of the two-dimensional thin-layer structure carbon nitride prepared at the positions of 13.1 DEG and 27.7 DEG, which correspond to g-C, respectively3N4(JCPDS has a number of 87-1526) crystal faces of (100) and (002).
It can be observed from fig. 2 that carbon nitride has successfully changed from a bulk structure to a two-dimensional layered structure.
Example 3
A preparation method of carbon nitride with a two-dimensional thin-layer structure comprises the following steps:
step 1: 1g of melamine was taken and mixed with 1: 2.56, dissolving melamine and glycerol phosphatidylcholine in 120ml of deionized water, continuously stirring for 60min until the melamine and the glycerol phosphatidylcholine are completely dissolved to obtain a mixture solution, then placing the mixture solution in a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 240 ℃ for 24h, centrifuging, washing for 5 times by using deionized water, and drying at 100 ℃ for 10h to obtain a solid;
step 2: adding 0.1g of KOH into the solid to obtain a solid mixture; then taking carbon fiber according to the mass ratio of the solid to the carbon fiber of 0.025:1, mechanically mixing the carbon fiber with the solid mixture to obtain a raw material, placing the raw material into a 500mL corundum crucible, covering the corundum crucible, placing the corundum crucible into a resonant cavity of an NJZ-10 type microwave oven, and vacuumizing the resonant cavity to 1 x 10 by adopting a water ring pump4Below Pa, irradiating the raw materials by a resonant cavity of the microwave oven under the microwave power of 5kW, rapidly heating the resonant cavity of the microwave oven to 560 ℃, then heating in vacuum for 120min at 560 ℃, and cooling to room temperature to obtain a heated product;
and step 3: washing the heated product with anhydrous ethanol for 3 times, and vacuum degree of 10-3And (3) carrying out vacuum drying for 6h in a vacuum drying oven of Pa at the temperature of 60 ℃ to obtain the carbon nitride with the two-dimensional thin-layer structure.
Example 4
A preparation method of carbon nitride with a two-dimensional thin-layer structure comprises the following steps:
step 1: 1g of melamine was taken and mixed with 1: 2.04, dissolving melamine and glycerol phosphatidylcholine in 100ml of deionized water, continuously stirring for 40min until the melamine and the glycerol phosphatidylcholine are completely dissolved to obtain a mixture solution, then placing the mixture solution in a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 220 ℃ for 20h, centrifuging, washing for 3 times by using deionized water, and drying at 85 ℃ for 9h to obtain a solid;
step 2: adding 0.07g of KOH into the solid to obtain a solid mixture; then taking carbon fiber according to the mass ratio of the solid to the carbon fiber of 0.1:1, mechanically mixing the carbon fiber with the solid mixture to obtain a raw material, placing the raw material into a 500mL corundum crucible, covering the corundum crucible, placing the corundum crucible into a resonant cavity of an NJZ-10 type microwave oven, and vacuumizing the resonant cavity to 1 x 10 by adopting a water ring pump4The content of the compound is less than Pa,irradiating the raw material by a microwave oven resonant cavity under the microwave power of 1kW, rapidly heating the microwave oven resonant cavity to 520 ℃, then heating in vacuum at 520 ℃ for 90min, and cooling to room temperature to obtain a heating product;
and step 3: washing the heated product with anhydrous ethanol for 2 times, and vacuum degree of 10-1And (4) carrying out vacuum drying for 5h in a vacuum drying oven of Pa at the temperature of 45 ℃ to obtain the carbon nitride with the two-dimensional thin-layer structure.
Claims (10)
1. A preparation method of carbon nitride with a two-dimensional thin-layer structure is characterized by comprising the following steps:
step 1: 1g of melamine was taken and mixed with 1: (1.38-2.56) dissolving melamine and glycerol phosphatidylcholine in 60-120 ml of deionized water to obtain a mixture solution, placing the mixture solution in a hydrothermal kettle, performing hydrothermal reaction at 180-240 ℃, centrifuging, washing and drying to obtain a solid substance;
step 2: adding 0.02-0.1 g of KOH into the solid to obtain a solid mixture; then taking carbon fibers according to the mass ratio (0.01-0.1) of the solid to the carbon fibers, mixing the carbon fibers with the solid mixture, placing the mixture into a crucible, placing the crucible into a resonant cavity of a microwave oven, heating the mixture in vacuum at 500-560 ℃, and cooling the mixture to room temperature to obtain a heated product;
and step 3: and washing and drying the heated product to obtain the carbon nitride with the two-dimensional thin-layer structure.
2. The method for preparing carbon nitride with a two-dimensional thin-layer structure according to claim 1, wherein in the step 1, the melamine and the glycerophosphatidylcholine are dissolved in the deionized water and then continuously stirred for 15-60 min.
3. The method for preparing carbon nitride with a two-dimensional thin-layer structure according to claim 1, wherein the lining of the hydrothermal kettle in the step 1 is made of polytetrafluoroethylene, and the hydrothermal reaction time is 10-24 hours.
4. The method for preparing carbon nitride with a two-dimensional thin-layer structure according to claim 1, wherein the washing in step 1 is 3-5 times with deionized water.
5. The method for preparing carbon nitride with a two-dimensional thin-layer structure according to claim 1, wherein the drying in step 1 is performed at 60-100 ℃ for 9-12 h.
6. The method for preparing carbon nitride with a two-dimensional thin-layer structure according to claim 1, wherein the microwave power in the vacuum-heated microwave oven cavity in the step 2 is 1-5 kW.
7. The method for preparing carbon nitride with two-dimensional thin-layer structure according to claim 6, wherein the degree of vacuum heating in step 2 is less than 1 x 104Pa。
8. The method for preparing carbon nitride with a two-dimensional thin-layer structure according to claim 7, wherein the time of vacuum heating in step 2 is 10-120 min.
9. The method for preparing carbon nitride with a two-dimensional thin-layer structure according to claim 1, wherein the washing in the step 3 is 2-3 times of washing with absolute ethyl alcohol.
10. The method for preparing carbon nitride with a two-dimensional thin-layer structure according to claim 1, wherein the drying in step 3 is vacuum drying at 35-60 ℃ for 2-6 h, and the vacuum degree of vacuum drying is 10-3～10-1Pa。
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| CN112320771A (en) * | 2020-11-11 | 2021-02-05 | 深圳大学 | Thin-layer porous g-C prepared by supercritical water3N4Method (2) |
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