CN107537544B - g-C3N4-CNTs heterojunction photocatalyst and preparation method thereof - Google Patents
g-C3N4-CNTs heterojunction photocatalyst and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a g-C3N4A preparation method of the-CNTs heterojunction photocatalyst. The method comprises the following steps: evenly mixing melamine with carbon nano tubes, and then calcining at high temperature to obtain g-C3N4CNTs; the obtained g-C3N4/CNTs is put into mixed solution of sulfuric acid/nitric acid for acidification and oxidation treatment to obtain g-C with carboxylated surface3N4CNTs-COOH; the obtained g-C3N4reacting/CNTs-COOH under the action of a dehydrating agent to obtain g-C3N4-CNTs heterojunction photocatalysts.
Description
Technical Field
The invention relates to the field of photocatalytic materials, in particular to g-C3N4-CNTs heterojunction photocatalyst and a preparation method thereof.
Background
Photocatalysis based on semiconductor materials has great potential as an emerging and green technology in solving energy shortage and environmental problems. Graphite phase carbon nitride (g-C)3N4) As a completely non-metal semiconductor, the compound has the advantages of stable chemical property, narrow forbidden band width, strong compatibility and the like, and becomes secondary nano TiO2Followed by another field of photocatalytic star materials. However, it was found that in the photocatalytic reaction, g-C3N4The surface photoproduction electrons and the holes are easy to be combined, so that the light quantum efficiency is low, and the photocatalytic activity is inhibited. Thus, in the pair g-C3N4How to promote the separation of surface photogenerated electrons and holes has been a hot research issue in research and development.
Carbon Nanotubes (CNTs) have been the most active research in nanomaterials since their discovery in the nineties of the last centuryThe field of the technology. Due to the special nano-scale tube cavity structure and higher specific surface area and surface activity of the CNTs, the CNTs have good charge transmission performance and adsorption performance. Thus, the semiconductor g-C3N4Coupled with CNTs, the g-C can be promoted by virtue of the charge transport properties of the CNTs3N4The separation of surface photogenerated electrons and holes improves the photon efficiency; on the other hand, the CNTs have stronger adsorption performance and can realize the rapid enrichment of pollutants, so that g-C in a coupling system3N4Promoting g-C in higher concentration pollutant environment3N4Surface photocatalytic reaction occurs. However, the preparation process of the photocatalytic material of the existing coupling system is complex, the preparation conditions are harsh, tight heterogeneous bonding is often lacked between the coupling systems, the synergistic interaction effect is not obvious, and the catalyst activity is low. Therefore, the development of the high-efficiency photocatalytic material with simple preparation process and easy implementation has important research significance and application value.
Disclosure of Invention
The invention aims to solve the problem of g-C in the prior art3N4The invention provides a g-C with compact heterogeneous amido bond chemical bond, which has the problems of lower photocatalytic efficiency and photocatalytic activity, easy recombination of photoproduction electrons and holes and the like of a photocatalyst3N4-CNTs composite photocatalyst and a preparation method thereof. The invention is realized by constructing g-C3N4The carbon nanotubes are chemically bonded with the CNTs to form a compact heterostructure, so that separation of photogenerated electrons and holes is promoted, and meanwhile, the large specific surface area and the surface activity of the CNTs are utilized to enhance the enrichment capacity of pollutants in a water body, so that the carbon nanotubes have important significance for improving the photocatalytic activity of the coupled system and improving the application of the coupled system in the aspect of environment.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
g-C3N4The preparation method of the-CNTs heterojunction photocatalyst comprises the following steps: (1): taking melamine and CNTs to be uniformly mixed to obtain a mixture, and calcining the mixture at high temperature to obtain g-C3N4/CNTs；
(2): will be provided withg-C obtained in step (1)3N4/CNTs is put into mixed acid solution for oxidation reaction to prepare g-C3N4/CNTs-COOH；
(3): g-C obtained in the step (2)3N4adding/CNTs-COOH into tetrahydrofuran solution, and simultaneously adding a dehydrating agent for reaction to obtain g-C3N4-CNTs heterojunction photocatalysts.
The mass ratio of the melamine to the CNTs in the step (1) is preferably 20-40: 0.5-2.5, the calcination temperature is 400-600 ℃, and the calcination time is 3-6 h. Preferably 4 hours. Preferably, the calcination is carried out in an air atmosphere to obtain g-C3N4g-C in CNTs3N4Is a graphite phase.
In a preferred step (2), the g-C3N4The mass-volume ratio of the/CNTs to the mixed acid solution is (1-3) g: (30-50) mL, wherein the reaction temperature is 40-50 ℃, and the reaction time is 8-24 h. In the mixed acid, sulfuric acid is concentrated sulfuric acid with the mass fraction of about 98%, nitric acid is concentrated nitric acid with the mass fraction of about 67%, and the volume ratio of the sulfuric acid to the nitric acid is 1: (2-5). Obtaining g-C3N4CNTs surface is rich in-COOH in CNTs-COOH.
Preferred is the case where g to C in step (3) is3N4The mass-volume ratio of/CNTs-COOH to tetrahydrofuran is (1-5) g: (50-200) mL
In the preferable step (3), the dehydrating agent is dicyclohexylcarbodiimide, and the g to C3N4The mass ratio of/CNTs-COOH to dicyclohexylcarbodiimide is (1-5): (1-3), said g-C3N4The mass-volume ratio of/CNTs-COOH to tetrahydrofuran is (1-5) g: (50-200) mL; the reaction temperature is 40-65 ℃ and the reaction time is 8-24 h. g-C obtained3N4CNTs have a heterojunction structure.
Preferred is the case where g to C in step (3) is3N4The mass ratio of the-CNTs-COOH to the dicyclohexylcarbodiimide is 1: 1.6, the reaction temperature is 50 ℃, and the reaction time is 8 h.
Preferably, the mixed acid solution in the step (2) is composed of sulfuric acid and nitric acid, the sulfuric acid is concentrated sulfuric acid with a mass fraction of 98%, the nitric acid is concentrated nitric acid with a mass fraction of 67%, and the volume ratio of the sulfuric acid to the nitric acid is 1: 2-5.
g-C provided by the invention3N4-CNTs heterojunction photocatalyst is made by the process of the present invention.
Invention g-C3N4-preparation principle of CNTs heterojunction photocatalyst: the graphite phase g-C is prepared by calcining the mixture of melamine and CNTs and carrying out thermal depolymerization3N4While at the same time, making g-C3N4Loading on the surface of CNTs to prepare g-C3N4CNTs coupled system, then g-C3N4/CNTs is subjected to mixed acid oxidation reaction, the surface of the CNTs is introduced with-COOH, and then g-C is added3N4Reaction of/CNTs-COOH under the action of a dehydrating agent dicyclohexylcarbodiimide, g-C3N4surface-NH2Dehydrating and condensing with-COOH on the surface of CNTs to form amido bond C (O) -N, thereby preparing g-C3N4-CNTs heterojunction photocatalysts.
Compared with the prior art, the invention has the following positive effects:
(1) g-C provided by the invention3N4–CNTSThe composite photocatalyst has a compact heterojunction structure, can effectively inhibit the recombination of photo-generated electrons and holes during the photocatalytic reaction, and has higher photocurrent response performance;
(2) g-C provided by the invention3N4–CNTSThe composite photocatalyst has stronger pollutant enrichment capacity;
(3) the catalyst provided by the invention has a wide spectral response range and high photocatalytic activity, and has high practical value and application prospect in the field of environmental protection;
(4) the photocatalyst of the invention has simple preparation method, easily obtained raw materials, low cost, no environmental pollution and easy industrial production.
Drawings
FIG. 1: is g-C prepared in example 3 of the invention3N4-CNTs and g-C3N4A photocurrent response graph of/CNTs;
FIG. 2: is g-C prepared in example 3 of the invention3N4XPS profile of/CNTs;
FIG. 3: g-C prepared in inventive example 33N4-XPS profile of CNTs;
FIG. 4: is g-C prepared in example 3 of the invention3N4–CNTs、g-C3N4CNTs and g-C3N4Photocatalytic activity is compared.
Detailed Description
The invention will be described in further detail with reference to the following figures and specific embodiments. The following examples are merely illustrative and explanatory of the present invention and should not be construed as limiting the scope of the invention. All techniques implemented based on the teachings of this disclosure are intended to be within the scope of this disclosure.
Example 1g-C3N4-preparation of CNTs heterojunction photocatalyst:
(1) uniformly mixing 30g of melamine with 1g of CNTs, placing the mixture in a tube furnace, and calcining the mixture for 4 hours at 450 ℃ in the air atmosphere to obtain g-C3N4/CNTs。
(2) g-C obtained in the step (1)3N4/CNTs weighing 2.0g, adding into 40mL of mixed acid solution of sulfuric acid/nitric acid (volume ratio is 1:2), refluxing and reacting at 40 ℃ for 12h, washing the product after reaction with distilled water and drying to obtain g-C3N4/CNTs-COOH。
(3) g-C obtained in the step (2)3N4Weighing 1.5g of/CNTs-COOH, adding the weighed 1.5g of the solution into 150mL of tetrahydrofuran solution, simultaneously adding 1g of dicyclohexylcarbodiimide, heating and refluxing the solution at 50 ℃ for 8 hours, and washing and drying a product after the reaction to obtain g-C3N4-CNTs heterojunction photocatalysts.
Example 2g-C3N4-preparation of CNTs heterojunction photocatalyst:
(1) 30g of melamine and 1.5g of CNTs are uniformly mixed and then placed in a tube furnace, and calcined for 4 hours at 500 ℃ in the air atmosphere to obtain g-C3N4/CNTs。
(2) g-C obtained in the step (1)3N4/CNTs weighing 2.0g, adding into 40mL of mixed acid solution of sulfuric acid/nitric acid (volume ratio is 1:2), refluxing and reacting at 45 ℃ for 16h, washing the product after reaction with distilled water and drying to obtain g-C3N4/CNTs-COOH。
(3) g-C obtained in the step (2)3N4Weighing 1.5g of/CNTs-COOH, adding the weighed 1.5g of the solution into 150mL of tetrahydrofuran solution, simultaneously adding 1.5g of dicyclohexylcarbodiimide, heating and refluxing the solution at the temperature of 55 ℃ for 12 hours, and washing and drying a product after the reaction to obtain g-C3N4-CNTs heterojunction photocatalysts.
Example 3g-C3N4-preparation of CNTs heterojunction photocatalyst:
(1) uniformly mixing 30g of melamine with 2g of CNTs, placing the mixture in a tube furnace, and calcining the mixture for 4 hours at 520 ℃ in air atmosphere to obtain g-C3N4/CNTs。
(2) g-C obtained in the step (1)3N4/CNTs 2.0g is weighed and added into 40mL mixed acid solution of sulfuric acid/nitric acid (volume ratio is 1:3), reflux reaction is carried out for 24h at the temperature of 45 ℃, the product after reaction is washed by distilled water and dried, and g-C is prepared3N4/CNTs-COOH。
(3) g-C obtained in the step (2)3N4Weighing 1.5g of/CNTs-COOH, adding the weighed 1.5g of the mixture into 150mL of tetrahydrofuran solution, simultaneously adding 2g of dicyclohexylcarbodiimide, heating and refluxing the mixture at the temperature of 60 ℃ for 12 hours, and washing and drying a product after the reaction to obtain g-C3N4-CNTs heterojunction photocatalysts.
Example 4g-C3N4-preparation of CNTs heterojunction photocatalyst:
(1) 30g of melamine and 2.5g of CNTs are uniformly mixed and then placed in a tube furnace, and calcined for 4 hours at 550 ℃ in the air atmosphere to obtain g-C3N4/CNTs。
(2) g-C obtained in the step (1)3N4/CNTs 2.0g is weighed and added into 40mL mixed acid solution of sulfuric acid/nitric acid (volume ratio is 1:4), reflux reaction is carried out for 24h at 50 ℃, and the product after reactionWashing the product with distilled water and drying to obtain g-C3N4/CNTs-COOH。
(3) g-C obtained in the step (2)3N4Weighing 1.5g of/CNTs-COOH, adding the weighed 1.5g of the solution into 150mL of tetrahydrofuran solution, simultaneously adding 2.5g of dicyclohexylcarbodiimide, heating and refluxing the solution at the temperature of 65 ℃ for 12 hours, and washing and drying a product after the reaction to obtain g-C3N4-CNTs heterojunction photocatalysts.
Test example: to verify the performance of the catalyst prepared by this method, the following experimental study was conducted
Test example 1: photocatalytic degradation test
The g-C prepared in examples 1-4 was measured separately using methyl orange as a target to remove contaminants3N4-photocatalytic degradation of methyl orange by CNTs.
The test method is as follows: 450mL of a 30mg/L methyl orange solution was added with 0.45g of g-C prepared in examples 1-4, respectively3N4The preparation method comprises the steps of-CNTs photocatalyst, oscillating at constant temperature for 1h, starting a visible light source to irradiate for 4h after adsorption reaches balance, carrying out a photocatalytic degradation experiment, taking out a solution after the experiment is finished, centrifuging by using a high-speed centrifuge, measuring the concentration of methyl orange in supernatant, and measuring the concentration of methyl orange according to the following formula
(1) Obtaining the removal rate, wherein (1) formula: r is the removal rate (%), C0Is the initial concentration of methyl orange in solution (mg/L), CeThe concentration of methyl orange in the solution after the photocatalytic reaction (mg/L) was used. The results are shown in Table 1.
TABLE 1g-C from examples 1 to 43N4Removal rate of methyl orange by-CNTs photocatalyst
| Selected materials | Residual concentration of methyl orange in solution (mg/L) | Removal Rate (%) |
| Example 1 | 5.3 | 82.3 |
| Example 2 | 4.1 | 86.3 |
| Example 3 | 1.6 | 94.6 |
| Example 4 | 3.1 | 89.7 |
As can be seen from the table, the removal rate of the target contaminant in the solution is higher, which indicates that the heterojunction g-C prepared by the invention3N4the-CNTs photocatalyst has better photocatalytic degradation capability.
Test example 2: photocurrent performance test
For g-C prepared in example 33N4CNTs and g-C3N4The CNTs were subjected to photocurrent performance tests, and the results are shown in FIG. 1. As can be seen from the figure, g-C is the same under the same test conditions3N4The intensity of the photocurrent generated by the-CNTs is significantly greater than that of g-C3N4CNTs, description g-C3N4And tight heterogeneous chemical bonding with CNTs can effectively promote the transfer of photon-generated carriers, inhibit the recombination of electrons and holes and further improve the photon quantum efficiency.
Test example 3: for g-C3N4CNTs and g-C3N4XPS characterization of CNTs
Analysis of g-C prepared in example 3 by XPS Spectroscopy characterization3N4CNTs and g-C3N4Chemical state of N element on the surface of CNTs, and the characterization results are shown in FIGS. 2 and 3. As shown in FIG. 2, characteristic fitting peaks of N1 s in CNTs appear at 398.4eV, 399.3eV and 400.9eV respectively, and N ═ C-N and polymeric N- (C) corresponding to triazine structures3And external C-N-H2Furthermore, fitting at 400.3eV results in a weak amide bond signal, probably due to the small amount of-COOH and g-C inherent to the surface of CNTs during calcination3N4surface-NH2And condensing to obtain the product. Compared to FIG. 2, C-NH at 400.9eV in FIG. 32The peak is obviously weakened, and the amido bond signal at 400.3eV is enhanced, which shows that the-COOH and g-C on the surface of the CNTs are oxidized by the mixed acid3N4surface-NH2Dehydrating under the action of dehydrating agent to form compact heterogeneous chemical bond.
Test example 4: comparative photocatalytic activity test
450mL of methyl orange solution with a concentration of 30mg/L was added with 0.45g of g-C prepared under the conditions of example 33N4–CNTs、g-C3N4CNTs and g-C3N4Wherein g-C3N4Prepared by direct calcination without adding CNTs. Oscillating each sample at constant temperature for 1h, starting a visible light source to irradiate for 4h after adsorption reaches balance, carrying out a photocatalytic degradation experiment, taking out a solution at certain time intervals, centrifuging the solution by a high-speed centrifuge, measuring the concentration of methyl orange in a supernatant, and calculating the removal rate according to the formula (1), wherein the result is shown in figure 4.
As can be seen from FIG. 4, the coupling system g-C3N4The photocatalytic degradation rate of CNTs to methyl orange is superior to that of pure g-C3N4The CNTs have good charge transport performance and large specific surface area, and can effectively promote the occurrence of photocatalytic reaction. In addition, with g-C3N4Relative to CNTs, g-C3N4The catalytic activity of the-CNTs is further obviously improved, which is mainly due to g-C3N4The close difference between the carbon nanotubes and the CNTsChemical bonding of the two components, not only quickening g-C3N4The photon-generated carriers on the surface migrate to the CNTs, the recombination of electron hole pairs is inhibited, and the pollutants enriched on the surface of the CNTs are promoted to g-C3N4Transferred and removed by oxidation of surface active groups.
The above-described embodiments are merely illustrative of the present invention and are not intended to limit the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Obvious variations or modifications which are within the spirit of the invention are possible within the scope of the invention.
Claims (8)
1. g-C3N4-a method for preparing a CNTs heterojunction photocatalyst, characterized in that it comprises the following steps:
(1): taking melamine and CNTs to be uniformly mixed to obtain a mixture, and calcining the mixture at high temperature to obtain g-C3N4/CNTs；
(2): g-C obtained in the step (1)3N4/CNTs is put into mixed acid solution for oxidation reaction to prepare g-C3N4/CNTs-COOH；
(3): g-C obtained in the step (2)3N4adding/CNTs-COOH into tetrahydrofuran solution, and simultaneously adding a dehydrating agent for reaction to obtain g-C3N4-CNTs heterojunction photocatalyst, the dehydrating agent is dicyclohexylcarbodiimide, the g-C3N4The mass ratio of/CNTs-COOH to dicyclohexylcarbodiimide is 1-5: 1-3, the reaction temperature is 40-65 ℃, and the reaction time is 8-24 h.
2. g-C according to claim 13N4The preparation method of the CNTs heterojunction photocatalyst is characterized in that the mass ratio of melamine to CNTs in the step (1) is 20-40: 0.5-2.5, the calcination temperature is 400-600 ℃, and the calcination time is 3-6 h.
3. g-C according to claim 13N4-a method for preparing a CNTs heterojunction photocatalyst, characterized in that in step (2), the g-C3N4The mass-volume ratio of the/CNTs to the mixed acid solution is 1-3: 30-50 ℃, the reaction temperature is 40-50 ℃, and the reaction time is 8-24 h.
4. g-C according to claim 13N4-a method for preparing a CNTs heterojunction photocatalyst, characterized in that, in step (3), said g-C3N4The mass-volume ratio of/CNTs-COOH to tetrahydrofuran is 1-5: 50-200.
5. g-C according to claim 13N4-a method for preparing a CNTs heterojunction photocatalyst, characterized in that, in step (3), said g-C3N4The mass ratio of/CNTs-COOH to dicyclohexylcarbodiimide is 1: 1.6, the reaction temperature is 50 ℃, and the reaction time is 8 h.
6. g-C according to any of claims 1 to 53N4The preparation method of the CNTs heterojunction photocatalyst is characterized in that the mixed acid solution in the step (2) is composed of sulfuric acid and nitric acid.
7. g-C according to claim 63N4The preparation method of the CNTs heterojunction photocatalyst is characterized in that in the mixed acid solution in the step (2), sulfuric acid is concentrated sulfuric acid with the mass fraction of 98%, nitric acid is concentrated nitric acid with the mass fraction of 67%, and the volume ratio of sulfuric acid to nitric acid is 1: 2-5.
8. g-C3N4-CNTs heterojunction photocatalyst, characterized in that it is prepared by the preparation method according to any one of claims 1 to 7.
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