CN112717976B - Stripped body phase g-C 3 N 4 Preparation method and application of - Google Patents
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- 239000002351 wastewater Substances 0.000 claims description 5
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 12
- 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 abstract description 8
- 229940043267 rhodamine b Drugs 0.000 abstract description 8
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 6
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 6
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- 239000000243 solution Substances 0.000 description 20
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 description 19
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- MFRIHAYPQRLWNB-UHFFFAOYSA-N sodium tert-butoxide Chemical compound [Na+].CC(C)(C)[O-] MFRIHAYPQRLWNB-UHFFFAOYSA-N 0.000 description 4
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- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
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- 125000000623 heterocyclic group Chemical group 0.000 description 1
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
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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
-
- B01J35/39—
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Abstract
The present invention provides a exfoliated phase g-C 3 N 4 The preparation method comprises the following steps of (1) slowly adding metal sodium into alcohol, and continuously stirring for 2 hours until the metal sodium completely reacts to obtain a sodium alkoxide solution; (2) Slowly adding into bulk phaseg‑C 3 N 4 Heating and stirring for stripping, filtering and washing to be neutral, and drying. The method reduces the harm of the stripped waste liquid to equipment and environment, the stripped carbon nitride material obtained by the method can be used as a catalyst in photocatalysis and wastewater treatment, the rhodamine B and methylene blue dissolving efficiency is respectively improved by 19.5 percent and 17.98 percent compared with bulk-phase carbon nitride under the condition of visible light, and the method has good application effect.
Description
Technical Field
The invention belongs to the technical field of carbon nitride materials, and particularly relates to a stripped phase g-C 3 N 4 The preparation method and the application thereof.
Background
Two-dimensional (2D) graphitic carbon nitride (g-C) since its discovery by scientists in 1834 3 N 4 ) Photocatalytic material for H as a promising organic semiconductor 2 Production, pollutant treatment and CO 2 Reduction, due to its unique optical and electronic properties, is very important in photocatalytic, non-toxic and convenient synthetic routes, and has attracted great attention. The carbon nitride material has a structure similar to that of graphene and is formed by stacking two-dimensional carbon and nitrogen atomic layers. Bulk g-C prepared by simple high temperature thermal polymerization 3 N 4 The defects of compact accumulation, small specific surface area, narrow response range to visible light, quick recombination of photo-generated electron-hole pairs and the like exist, and the large-scale popularization and application of the photo-generated electron-hole pairs are limited. Therefore, inspired by hummers method for preparing graphene oxide, the method of stripping carbon nitride by adopting concentrated sulfuric acid is applied to preparing g-C 3 N 4 Of (2) isAnd (4) slicing. However, concentrated sulfuric acid has strong oxidizing property and corrosivity, the requirement on experimental operation is high, and the stripping waste liquid has great harm to the environment. Therefore, the invention explores a new method for stripping the carbon nitride material by sodium ethoxide, provides a new scheme for solving the problems of low visible light utilization rate, difficult stripping, environment friendliness and the like of the carbon nitride material, proves that the method does not damage the structure of the carbon nitride, and explores the removal effect of the carbon nitride material on the soluble organic dye before and after stripping under the condition of visible light.
Disclosure of Invention
In order to solve the problems of low utilization rate of visible light, difficult stripping, small specific surface area and the like of the carbon nitride material, the carbon nitride material is enhanced in H 2 Production, pollutant treatment and CO 2 The invention provides a novel method for stripping a carbon nitride material by sodium ethoxide, and the carbon nitride material treated by the method can effectively enhance the degradation effect on organic dyes such as methylene blue and rhodamine B under the condition of visible light.
In order to solve the technical problem, the invention provides a method for stripping carbon nitride, which comprises the following steps of (1) slowly adding metal sodium into alcohol, continuously stirring for 2 hours, and obtaining sodium alkoxide solution after the metal sodium completely reacts; (2) Slowly add bulk phase g-C 3 N 4 And (4) obtaining stripping liquid, heating and stirring for stripping, performing suction filtration and washing to be neutral, and drying.
Preferably, in step (1), the alcohol includes one or more of methanol, ethanol and tert-butanol.
Preferably, the bulk phase g-C 3 N 4 The mass ratio of the sodium metal to the sodium metal is 1 (1-2).
Preferably, in the step (2), the heating and stirring are carried out at the temperature of 40-80 ℃ for 6-12 h.
Preferably, in the step (2), the drying is performed at 60 ℃ for 12h.
Preferably, in the step (2), the concentration of the stripping solution is 3 to 10g/L.
As another aspect of the invention, the invention provides a post-exfoliation carbon nitride material.
As another aspect of the invention, the invention provides a use of the carbon nitride material after exfoliation as a catalyst in photocatalysis and wastewater treatment.
Preferably, the wastewater is organic dye wastewater.
The invention has the beneficial effects that:
the reagent required by the invention has low danger and simple operation process, and does not need complex and expensive equipment. The invention reduces the harm of the stripped waste liquid to equipment and environment; the preparation method provided by the invention is determined by characterization means such as XRD, infrared spectrogram and SEM that the structure of the carbon nitride material is not damaged, and the efficiency of the prepared stripped carbon nitride material as a photocatalyst for degrading rhodamine B and methylene blue is improved by 19.5% and 17.98% respectively compared with bulk-phase carbon nitride.
Drawings
FIG. 1 is an XRD pattern of the carbon nitride material before and after exfoliation of sodium ethoxide prepared in example 2;
FIG. 2 is an SEM image of carbon nitride material before and after sodium ethoxide exfoliation prepared in example 2, wherein a and b are g-C 3 N 4 SEM pictures of different specifications before stripping, C and d are g-C stripped by sodium ethoxide 3 N 4 SEM pictures under different specifications;
FIG. 3 is a Fourier infrared spectrum of the carbon nitride material before and after sodium ethoxide exfoliation prepared in example 2;
FIG. 4 is a graph showing the effect of carbon nitride materials on rhodamine B degradation before and after sodium ethoxide exfoliation, prepared in example 2, wherein the front and back correspond to the left and right, respectively;
FIG. 5 is a graph showing the degradation effect of the carbon nitride material on methylene blue before and after stripping sodium ethoxide prepared in example 2, wherein the front and the back correspond to the left and the right, respectively;
FIG. 6 is a schematic structural diagram of the sodium ethoxide exfoliated carbon nitride material prepared by the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Bulk phases g-C for use in the invention 3 N 4 The material is prepared by the following steps:
heating melamine as a raw material to 400 ℃ at a speed of 10 ℃/min in a muffle furnace, and keeping the temperature for 1h; then continuously heating to 550 ℃, preserving heat for 2 hours, cooling to room temperature, taking out and grinding to obtain the product.
Example 1
A novel method for stripping carbon nitride is characterized by comprising the following steps:
(1) Adding 150ml of methanol into a 250ml three-neck flask, weighing 1g of metal sodium, slowly adding the metal sodium into a methanol solution, continuously stirring for 6 hours, generating bubbles at the moment, and obtaining a sodium methoxide solution after the metal sodium completely reacts;
(2) Weighing 1g of bulk phase g-C 3 N 4 The material is slowly added into the mixed solution in the sodium methoxide solution in the step (1), and then the mixed solution is put into an oil bath kettle at the temperature of 70 ℃ to be heated, refluxed, stirred and stripped for 12 hours.
(3) And (3) filtering and washing the reaction mixed liquor obtained in the step (2) to be neutral, then placing the solid material in an oven for drying at 60 ℃ for 12h, grinding and bottling to obtain the sodium methoxide stripping carbon nitride.
Example 2
A novel method for stripping carbon nitride is characterized by comprising the following steps:
(1) Adding 150ml of absolute ethyl alcohol into a 250ml three-neck flask, weighing 1g of metal sodium, slowly adding the metal sodium into the absolute ethyl alcohol, continuously stirring for 6 hours until bubbles are generated, and obtaining a sodium ethoxide solution after the metal sodium completely reacts;
(2) Weighing 1g of bulk phase g-C 3 N 4 The materials are slowly added into the mixed solution of the sodium ethoxide solution in the step (1), the solution gradually becomes light yellow silky milk, and then the solution is put into an oil bath pan with the temperature of 70 ℃ to be heated, refluxed, stirred and peeled for 12 hours.
(3) And (3) filtering and washing the reaction mixed liquor obtained in the step (2) to be neutral, then placing the solid material in an oven for drying at 60 ℃ for 12h, grinding and bottling to obtain the sodium ethoxide-stripped carbon nitride.
With the knot of example 2The effect of the stripping method was analyzed. From the XRD diffractogram of fig. 1, it can be seen that the carbon nitride before and after the exfoliation has a similar diffraction peak at 27.3 °, indicating that the crystal structures before and after the exfoliation are the same, corresponding to the (002) crystal plane of the carbon nitride, indicating that the exfoliation method does not change the crystal structure of the carbon nitride; in FIG. 2, a and b are scanning electron microscope images of 500nm and 5nm of bulk carbon nitride, respectively, and it can be seen that the bulk structure of the bulk carbon nitride material is more obvious and is similar to a stone shape; and c and d are scanning electron microscope images of 500nm and 5nm of carbon nitride after sodium ethoxide stripping, compared with a and b, the blocky structures in the images of c and d are obviously reduced, and for the 5nm image, the stripped carbon nitride in the image of d shows a loose and multi-fold structure similar to schistose, which indicates that the stripping method effectively improves the appearance and the lamellar structure of bulk-phase carbon nitride. FIG. 3 is a Fourier infrared spectrum of 810cm -1 Is a characteristic absorption peak corresponding to bending vibration of the triazine ring, 890cm -1 Is vibration signal of N-H bond, and is in the range of 1100-1700cm -1 The absorption wave band shows that the C-N heterocyclic ring stretches and contracts and vibrates to absorb [ C-N (-C) -C or C-NH-C]3000-3700cm -1 Residual N-H in the non-condensed amino group and vibrational signals from the adsorption of-OH bonds in water molecules. In addition, the characteristic absorption peak of the carbon nitride after the sodium ethoxide stripping is sharper, which indicates that the crystal crystallinity of the stripped polymer after the sodium ethoxide is better; FIG. 4 is a graph of the degradation effect of a carbon nitride material on rhodamine B before and after sodium ethoxide stripping, wherein the left and right graphs are respectively the effect of bulk phase carbon nitride and the effect of carbon nitride after sodium ethoxide stripping on rhodamine B, so that the effect of carbon nitride after stripping on rhodamine B degradation is better, the time for dye solution decoloration is faster, and the stripping method is proved to improve the photocatalytic activity of the carbon nitride material; in fig. 5, the left and right images are respectively the effect images of the carbon nitride after stripping the bulk phase carbon nitride and sodium ethoxide to degrade methylene blue, and it is obvious that the carbon nitride material after stripping has better degradation and decoloration effects. Therefore, the characterization tests and experiments show that the stripping method can effectively improve the photocatalytic performance of the carbon nitride material.
Example 3
A novel method for stripping carbon nitride is characterized by comprising the following steps:
(1) Adding 150ml of tert-butyl alcohol into a 250ml three-neck flask, weighing 1g of metal sodium, slowly adding the metal sodium into a tert-butyl alcohol solution, continuously stirring for 6 hours until the metal sodium reacts completely to obtain a sodium tert-butyl alcohol solution;
(2) Weighing 1g of bulk phase g-C 3 N 4 Slowly adding the materials into the sodium tert-butoxide solution obtained in the step (1) to obtain a mixed solution, and continuously stirring and stripping the mixed solution at 70 ℃ for 12h.
(3) And (3) filtering and washing the reaction mixed liquor obtained in the step (2) to be neutral, then placing the solid material in an oven for drying at 60 ℃ for 12h, grinding and bottling to obtain the sodium tert-butoxide stripped carbon nitride.
The sodium ethoxide stripping carbon nitride material prepared by the invention has a structure shown as a formula I in figure 6. The stripping method employed in the present invention does not alter g-C 3 N 4 But enhances its degradation properties. The invention also provides application of the carbon nitride material stripped by the sodium ethoxide to photocatalytic degradation of organic dyes rhodamine B and methylene blue, wherein the dye concentration is controlled at 10 ppm, 50mg of the carbon nitride material before and after stripping is weighed, 50ml of organic dye wastewater is added, after the material and the solution are uniformly dispersed by ultrasonic treatment for 10min, a dark reaction is carried out for 1h to achieve the adsorption and desorption balance of the catalyst on the dye solution, a lamp is turned on for degradation of the dye under visible light, 4ml of the solution is extracted at intervals, the solution is centrifuged, and the supernatant is taken to determine the ultraviolet-visible absorption spectrum. The results are shown in FIGS. 3-5.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (6)
1. A method of stripping carbon nitride, comprising: comprises the following steps of (a) preparing a solution,
(1) Slowly adding metal sodium into alcohol, and continuously stirring for 2h until the metal sodium completely reacts to obtain a sodium alkoxide solution;
the alcohol comprises one or more of methanol, ethanol and tertiary butanol;
(2) Slowly adding the bulk phase g-C 3 N 4 Obtaining stripping liquid, heating and stirring for 6-12 h at 40-80 ℃ for stripping, filtering, washing to neutrality, and drying;
said bulk phase g-C 3 N 4 The mass ratio of the sodium metal to the sodium metal is 1 (1-2).
2. The method for stripping carbon nitride as claimed in claim 1, wherein: in the step (2), the drying is carried out for 12 hours at the temperature of 60 ℃.
3. The method for stripping carbon nitride as claimed in claim 1, wherein: in the step (2), the concentration of the stripping solution is 3-10 g/L.
4. A stripped carbon nitride material obtained by the method according to any one of claims 1 to 3.
5. Use of the exfoliated carbon nitride material of claim 4 as a catalyst in photocatalysis and wastewater treatment.
6. Use according to claim 5, characterized in that: the wastewater is organic dye wastewater.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437589A (en) * | 2014-11-07 | 2015-03-25 | 江苏大学 | Silver/graphene oxide/carbon nitride composite photocatalytic material and preparation method thereof |
| CN104475140A (en) * | 2014-11-07 | 2015-04-01 | 江苏大学 | Silver-modified carbon nitride composite photocatalytic material and preparation method thereof |
| CN108671951A (en) * | 2018-04-17 | 2018-10-19 | 浙江工商大学 | A kind of nitridation carbon composite photocatalyst and its preparation method and application |
| CN110882714A (en) * | 2019-12-16 | 2020-03-17 | 吉林大学 | Curled carbon nitride thin sheet, preparation method and application thereof in hydrogen production through photocatalytic water decomposition |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437589A (en) * | 2014-11-07 | 2015-03-25 | 江苏大学 | Silver/graphene oxide/carbon nitride composite photocatalytic material and preparation method thereof |
| CN104475140A (en) * | 2014-11-07 | 2015-04-01 | 江苏大学 | Silver-modified carbon nitride composite photocatalytic material and preparation method thereof |
| CN108671951A (en) * | 2018-04-17 | 2018-10-19 | 浙江工商大学 | A kind of nitridation carbon composite photocatalyst and its preparation method and application |
| CN110882714A (en) * | 2019-12-16 | 2020-03-17 | 吉林大学 | Curled carbon nitride thin sheet, preparation method and application thereof in hydrogen production through photocatalytic water decomposition |
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