CN107486230B - High-activity large-specific-surface-area nano sheet-shaped structure g-C3N4Preparation method of (1) - Google Patents
High-activity large-specific-surface-area nano sheet-shaped structure g-C3N4Preparation method of (1) Download PDFInfo
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- CSGNMMLYYZTWBB-UHFFFAOYSA-N nitric acid;1,3,5-triazine-2,4,6-triamine Chemical compound O[N+]([O-])=O.NC1=NC(N)=NC(N)=N1 CSGNMMLYYZTWBB-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 10
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000001699 photocatalysis Effects 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
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- 238000012719 thermal polymerization Methods 0.000 abstract description 5
- YPRTZUDVTHDBCP-UHFFFAOYSA-N N1=C(N)N=C(N)N=C1N.[N+](=O)(O)[O-].[N+](=O)(O)[O-] Chemical compound N1=C(N)N=C(N)N=C1N.[N+](=O)(O)[O-].[N+](=O)(O)[O-] YPRTZUDVTHDBCP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 3
- NSUGPGQAMVQAJJ-UHFFFAOYSA-N [N+](=O)(O)[O-].[N+](=O)(O)[O-].[N+](=O)(O)[O-].N1=C(N)N=C(N)N=C1N Chemical compound [N+](=O)(O)[O-].[N+](=O)(O)[O-].[N+](=O)(O)[O-].N1=C(N)N=C(N)N=C1N NSUGPGQAMVQAJJ-UHFFFAOYSA-N 0.000 abstract description 3
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- 239000002086 nanomaterial Substances 0.000 description 23
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 7
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 6
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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
- 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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- B01J35/40—
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- B01J35/50—
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- B01J35/615—
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Abstract
g-C with high activity and high specific surface area3N4A method for preparing a nano sheet structure material. Melamine is used as a raw material, acetic acid or deionized water is used as a melamine solvent, and different nitric acid amounts are added to prepare energetic materials of melamine mononitrate, melamine dinitrate and melamine trinitrate for preparing g-C3N4The precursor of (1). The method utilizes the strong energy released during the thermal polymerization of melamine nitrate to convert the blocky g-C3N4Stripping into nanometer sheet, reducing temperature and reaction time required by thermal polymerization, and avoiding traditional high specific area nanometer sheet g-C3N4The high temperature and secondary calcination process in solid phase synthesis greatly reduces the synthesis energy consumption level. The method is simple and easy to implement, low in cost and good in repeatability, and has wide application prospects in the fields of photolysis of water, photocatalytic oxidation of environmental pollutants and the like.
Description
Technical Field
The invention belongs to the field of new materials, new energy utilization and environmental pollution treatment, and relates to a preparation method of high-activity large-specific-surface-area nano-sheet-shaped structure g-C3N4A preparation method of a photocatalytic material.
Background
Graphene phase carbon nitride (g-C)3N4) The material is a novel polymeric material, consists of non-metallic elements, has cheap and abundant raw materials and special structure and performance, and is a semiconductor material with environmental friendliness and biocompatibility. In recent years, researchers can lead the material to show excellent performance in the fields of energy, environment, medicine and the like by optimizing preparation and modification methods. However, bulk g-C prepared by thermal polymerization method3N4The problems of small specific surface area, few active sites, low quantum efficiency in a visible light region and the like exist, and the photocatalytic efficiency is poor. The specific surface area can be increased, the reactive sites can be increased, the electron transfer efficiency can be improved, the electron and hole recombination can be inhibited, and the carbon nitride content can be improved by adopting a nano structure and morphology regulation and control meansPhotocatalytic activity. At present, a hard template method, a soft template method and a supermolecular self-assembly method are common methods for preparing the carbon nitride nano material. However, the silicon dioxide or the aluminum oxide is used as a hard template, which relates to the tedious precursor filling and template agent removing process, and the fluorine-containing toxic chemical reagent is adopted, so that the problems of large pollution, high cost, long period and the like exist. The soft template method and the supermolecule method have the problems of complex equipment, complex operation process, low conversion efficiency and the like. Therefore, a simple, fast and environment-friendly method is developed to regulate and control the nano structure of the carbon nitride and improve the photocatalytic performance of the carbon nitride.
Disclosure of Invention
The invention provides g-C with high activity and high specific surface area3N4A method for preparing a nano sheet structure material. Melamine is used as a raw material, acetic acid or deionized water is used as a melamine solvent, and different nitric acid amounts are added to prepare energetic materials of melamine mononitrate, melamine dinitrate and melamine trinitrate for preparing g-C3N4The precursor of (1). The method utilizes the strong energy released during the thermal polymerization of melamine nitrate to convert the blocky g-C3N4Stripping into nanometer sheet, reducing temperature and reaction time required by thermal polymerization, and avoiding traditional high specific area nanometer sheet g-C3N4The high temperature and secondary calcination process in solid phase synthesis greatly reduces the synthesis energy consumption level. The method is simple and easy to implement, low in cost and good in repeatability, and has wide application prospects in the fields of photolysis of water, photocatalytic oxidation of environmental pollutants and the like; another object of the present invention is to provide a flake g-C having high activity and high specific surface area prepared by the method3N4And (3) nano materials.
High-activity large-specific-surface-area nano sheet-shaped structure g-C3N4The preparation method of the photocatalytic material comprises the following steps:
(1) 4g of melamine is dried for 24h at 60 ℃, dissolved in 10 ml of deionized water or acetic acid and uniformly mixed by ultrasonic;
(2) putting 3 ml, 4 ml or 5 ml of 60% HNO3 solution into the mixed solution in the step (1), and uniformly stirring to obtain paste melamine nitrate;
(3) placing the melamine nitrate obtained in the step (2) into a covered crucible, and placing the crucible into a muffle furnace heated to 190-200 ℃; then heating the muffle furnace to 500 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 2 hours, then immediately taking out the crucible and naturally cooling to obtain the light yellow large-surface-area nano flaky structure g-C3N4A material.
g-C provided by the invention3N4The specific surface area of the nano material is as high as 240m2/g, and the nano material has excellent capability of decomposing water and degrading organic pollution due to the quantum effect of the nano sheet. The preparation method provided by the invention has the advantages of cheap raw materials, simple preparation method, low energy consumption, high practical value and high application prospect.
Drawings
FIG. 1 is an XRD pattern of g-C3N4 nanomaterials 1-4.
FIG. 2 is a TEM image of g-C3N4 nanomaterials 1-4: (a) g-C3N4 nanomaterial 1; (b) g-C3N4 nanomaterial 2; (c) g-C3N4 nanomaterial 3; (d) g-C3N4 nanomaterial 4.
FIG. 3 is a graph showing the change of the efficiency of degrading rhodamine by g-C3N4 nano materials 1-4 and a block g-C3N 4: (a) block g-C3N 4; (b) g-C3N4 nanomaterial 1; (c) g-C3N4 nanomaterial 2; (d) g-C3N4 nanomaterial 3; (e) g-C3N4 nanomaterial 4.
Detailed Description
The methods and techniques of the present invention are described below by way of example.
Example 1: weighing 4g of melamine dried for 24h at 60 ℃, dissolving in 10 ml of deionized water, and uniformly mixing by 1000W ultrasound for 10 min; (2) measuring 3 ml of 60 percent HNO3Putting the solution into the mixed solution in the step (1), and uniformly stirring to obtain pasty melamine mononitrate; (3) putting the melamine mononitrate obtained in the step (2) into a covered crucible, and putting into a muffle furnace heated to 190 ℃; then heating the muffle furnace to 500 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 2 hours, then immediately taking out the crucible and naturally cooling to obtain the light yellow large-surface-area nano flaky structure g-C3N4Material 1.
Example 2: weighing 4g of melamine dried for 24h at 60 ℃, dissolving in 10 ml of deionized water, and uniformly mixing by 1000W ultrasound for 10 min; (2) measuring 4 ml of 60% HNO3Putting the solution into the mixed solution in the step (1), and uniformly stirring to obtain pasty melamine dinitrate; (3) putting the melamine mononitrate obtained in the step (2) into a covered crucible, and putting into a muffle furnace heated to 200 ℃; then heating the muffle furnace to 500 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 2 hours, then immediately taking out the crucible and naturally cooling to obtain the light yellow large-surface-area nano flaky structure g-C3N4Material 2.
Example 3: weighing 4g of melamine dried for 24h at 60 ℃, dissolving in 10 ml of deionized water, and uniformly mixing by 1000W ultrasound for 10 min; (2) measuring 5 ml of 60 percent HNO3Putting the solution into the mixed solution in the step (1), and uniformly stirring to obtain paste melamine trinitrate; (3) putting the melamine mononitrate obtained in the step (2) into a covered crucible, and putting into a muffle furnace heated to 200 ℃; then heating the muffle furnace to 500 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 2 hours, then immediately taking out the crucible and naturally cooling to obtain the light yellow large-surface-area nano flaky structure g-C3N4Material 3.
Example 4: weighing 4g of melamine dried for 24h at 60 ℃, dissolving in 10 ml of acetic acid, and uniformly mixing by 1000W ultrasound for 10 min; (2) measuring 4 ml of 60% HNO3Putting the solution into the mixed solution in the step (1), and uniformly stirring to obtain pasty melamine dinitrate; (3) putting the melamine mononitrate obtained in the step (2) into a covered crucible, and putting into a muffle furnace heated to 200 ℃; then heating the muffle furnace to 500 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 2 hours, then immediately taking out the crucible and naturally cooling to obtain the light yellow large-surface-area nano flaky structure g-C3N4Material 4.
For g-C obtained above3N4The nanomaterials 1-4 were subjected to photocatalytic activity test experiments, and for comparison, the bulk g-C was also determined under the same conditions3N4Photocatalysis of materialsThe photocatalytic activity was measured by initially measuring 10 mg-L-150ml of rhodamine B (RhB) solution is used as a target degradation product and placed in a 250ml beaker, 0.01g of photocatalyst is weighed and uniformly distributed in the rhodamine B (RhB) solution, and the photocatalyst is in a suspension state in the solution. In order to achieve adsorption-desorption equilibrium, the suspension is subjected to dark reaction for 30min under the condition of magnetic stirring, the suspension is placed under a visible light source (300W xenon lamp) which is 12cm away from the liquid surface for photocatalysis experiment, the supernatant is taken at intervals, the absorbance of the supernatant is measured at the maximum absorption wavelength (554nm) of rhodamine B (RhB), and the total light reaction is carried out for 50min, and the obtained result is shown in the attached figure 1.
Attached tables 1 g-C3N4Specific surface area and pore size distribution of nano material 1-4
| Sample (I) | Specific surface area BET (m2/g) | Pore size (nm) | Pore volume (cm)3/g) |
| g-C3N4Nanomaterial 1 | 220.2 | 15.5 | 0.894 |
| g-C3N4Nanomaterial 2 | 230.8 | 10.9 | 1.137 |
| g-C3N4Nanomaterial 3 | 148.9 | 12.1 | 0.449 |
| g-C3N4Nanomaterial 4 | 240.1 | 9.2 | 1.245 |
Those skilled in the art can make various changes and modifications to the disclosed embodiments without departing from the scope of the present invention, and all such changes and modifications as would be obvious to one skilled in the art are intended to be included within the scope of the present invention.
Claims (1)
1. High-activity large-specific-surface-area nano sheet-shaped structure g-C3N4The preparation method of the photocatalytic material is characterized by comprising the following steps:
(1) drying 4g of melamine at 60 ℃ for 24h, dissolving in 10 ml of deionized water or acetic acid, and uniformly mixing by ultrasonic waves;
(2) taking 3 ml, 4 ml or 5 ml of 60% HNO3Putting the solution into the mixed solution in the step (1), and uniformly stirring to obtain paste melamine nitrate;
(3) placing the melamine nitrate obtained in the step (2) into a covered crucible, and placing the crucible into a muffle furnace heated to 190-200 ℃; then heating the muffle furnace to 500 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 2 hours, then immediately taking out the crucible and naturally cooling to obtain the light yellow large-surface-area nano flaky structure g-C3N4A material.
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| RU2690810C1 (en) * | 2018-10-05 | 2019-06-05 | Федеральное государственное бюджетное учреждение науки Научно-технологический центр уникального приборостроения Российской академии наук (НТЦ УП РАН) | Method of producing carbon nitride having an abnormally high level of fluorescence under the action of visible laser radiation |
| CN109433246B (en) * | 2018-12-26 | 2021-07-16 | 台州学院 | Carbon vacancy-containing nanosheet C3N4Photocatalyst and preparation method thereof |
| CN110075906A (en) * | 2019-06-11 | 2019-08-02 | 北华大学 | A kind of curly g-C3N4And preparation method and purposes |
| CN111250135B (en) * | 2020-02-17 | 2021-01-15 | 燕山大学 | Graphite-phase carbon nitride nanosheet material and preparation method and application thereof |
| CN116425127A (en) * | 2023-04-18 | 2023-07-14 | 鲁东大学 | g-C 3 N 4 Photocatalyst and preparation method thereof |
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| CN105271142A (en) * | 2015-11-19 | 2016-01-27 | 南京工程学院 | Irregularly-rodlike g-C3N4 material and preparation method and application thereof |
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| CN106732739A (en) * | 2017-02-20 | 2017-05-31 | 合肥工业大学 | A kind of g C3N4The preparation method of nanometer sheet |
| CN106732721A (en) * | 2016-12-06 | 2017-05-31 | 江苏大学 | A kind of high catalytic activity g C3N4Preparation method and purposes |
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| CN105271142A (en) * | 2015-11-19 | 2016-01-27 | 南京工程学院 | Irregularly-rodlike g-C3N4 material and preparation method and application thereof |
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