CN114100656A - Preparation method of S-CN-D homogeneous nano heterojunction - Google Patents
Preparation method of S-CN-D homogeneous nano heterojunction Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 42
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 34
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004202 carbamide Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 15
- 239000011593 sulfur Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 14
- 230000007547 defect Effects 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000012719 thermal polymerization Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 4
- 238000005580 one pot reaction Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 description 11
- 239000011941 photocatalyst Substances 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 229910021397 glassy carbon Inorganic materials 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002674 ointment Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000007832 Na2SO4 Substances 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 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
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- B01J35/615—
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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
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention discloses a preparation method of an S-CN-D homogeneous nano heterojunction, which comprises the following steps: mixing urea and a sulfur source, adding N, N-dimethylformamide, and stirring and mixing uniformly; heating to 150-400 ℃ for 1-4 h, and then heating to 500-600 ℃ for 1-5 h; naturally cooling to room temperature, and grinding to obtain the S-CN-D homogeneous nano heterojunction; according to the method, urea, a sulfur source and N, N-Dimethylformamide (DMF) are subjected to one-step thermal polymerization, when CN is generated by thermal polymerization of urea, DMF enables rich C defects to be generated to form CD-D, meanwhile, part of S is doped at the position of the C defects to form S-CN, the S-CN-D homogeneous nano heterojunction is prepared through one-step reaction, and meanwhile, a large amount of gas generated by heating DMF has a stripping effect on the homogeneous nano heterojunction, so that the specific surface area of the S-CN-D homogeneous nano heterojunction is as high as 135.7m2G, photocatalytic decomposition of aquatic product H2The rate was 3190. mu. molh‑1g‑18.6 times that of the unmodified CN.
Description
Technical Field
The invention belongs to the technical field of photocatalytic hydrogen production, and particularly relates to a preparation method of an S-CN-D homogeneous nano heterojunction.
Background
Photocatalytic decomposition of aquatic product H2The solar energy is converted into new clean energy and is considered as an environment-friendly energy regeneration mode. Decomposition of aquatic products H2Is a two electron process (H)2O→H2+1/2O2，△G＝+237.2kJ mol-1). The band gap of the photocatalyst should exceed the decomposition energy of water (1.23eV), so as to ensure successful water decomposition. Two dimensional (2D) g-C3N4Has proper positions of a conduction band (CB, -1.3eV) and a valence band (VB, +1.4eV) and a moderate band gap (approximatively equals to 2.7eV), can be used for photocatalytic decomposition of aquatic products H2。2D g-C3N4The thinner, due to quantum size effects, 2D g-C3N4CB and VB are moved in opposite directions, resulting in g-C3N4The band gap of the nano-sheet is increased, and the wide band gap enables g-C3N4Has more negative conduction band position (stronger reduction potential) and is more favorable for decomposing aquatic product H2. However, there are problems in that the water is decomposed completely theoretically, such as a large defect in a kinetic process during separation and transport of carriers, and the efficiency of water decomposition is severely inhibited due to low hole mobility. Therefore, 2D g-C can be endowed by modification strategies such as heteroatom sulfur doping, defect introduction, heterojunction construction and the like3N4Stronger photocatalytic decomposition of aquatic product H2And (4) activity.
Disclosure of Invention
The invention aims to provide a preparation method for preparing a modified CN homogeneous nano heterojunction by one-step reaction, and the specific surface area of the obtained product is as high as 135.7m2G, photocatalytic decomposition of aquatic product H2The rate was 3190. mu. molh-1g-1。
In order to achieve the purpose, the technical scheme is as follows:
a preparation method of S-CN-D homogeneous nano heterojunction comprises the following steps:
mixing urea and a sulfur source, adding N, N-dimethylformamide, and stirring and mixing uniformly;
heating to 150-400 ℃ for 1-4 h, and then heating to 500-600 ℃ for 1-5 h;
and naturally cooling to room temperature, and grinding to obtain the S-CN-D homogeneous nano heterojunction.
According to the scheme, the sulfur source is sublimed sulfur powder, ammonium sulfate or thiourea.
According to the scheme, the mass ratio of the sulfur source to the urea is (0.5-5) to 1; 1-50 mL of N, N-dimethylformamide is added.
According to the scheme, the heating rate is 5-15 ℃/min. The slower the rate, the longer the thermal polymerization time, the thicker the sheet layer of the product; the faster the rate, the shorter the thermal polymerization time and the lower the product yield.
The invention adopts urea and N, N-Dimethylformamide (DMF) to produce g-C3N4The C defect CN (CN-D) is generated, S is doped at the position of the C defect after the S source is added to form S-g-C3N4(S-CN for short), S-CN and CD-D form a homogeneous nano heterojunction (S-CN-D for short), the specific surface area is obviously increased, and H is facilitated2Adsorption on the surface of the catalyst, and the homogeneous nano heterogeneous structure exposes more active catalytic sites and cross-plane diffusion channels, so that the absorption of the induced visible light is enhanced, the separation and transmission of carriers are accelerated, and the photocatalytic decomposition of the S-CN-D reaction center on the aquatic product H is enhanced2The reactivity of (a).
According to the method, urea, a sulfur source and N, N-Dimethylformamide (DMF) are subjected to one-step thermal polymerization, the DMF generates rich C defects to form CD-D when CN is generated by thermal polymerization of the urea, meanwhile, part of S is doped at the C defects to form S-CN4, the S-CN-D homogeneous nano heterojunction is prepared through one-step reaction, and meanwhile, a large amount of gas generated by heating the DMF has a stripping effect on the homogeneous nano heterojunction, so that the specific surface area of the S-CN-D homogeneous nano heterojunction is as high as 135.7m2G, photocatalytic decomposition of aquatic product H2The rate was 3190. mu. molh-1g-18.6 times that of the unmodified CN.
The method has the advantages of simple and quick reaction, easy operation, green and pollution-free reaction process, high yield and suitability for practical application.
Drawings
FIG. 1: XRD pattern of S-CN-D homonano-heterojunction obtained in example 1;
fig. 2: a synthesis schematic diagram of an S-CN-D homogeneous nano heterojunction; (b-c) SEM images of CD-D and S-CN-D homogeneous nano-heterojunctions; (d) SEM images of S-CN-D homogeneous nano-heterojunction of example 1, C, N, and S EDS images.
Fig. 3: XPS spectrum of S-CN-D homonano heterojunction obtained in example 1;
FIG. 4: impedance plots of different photocatalysts; (b) a photo-amperometric graph;
FIG. 5: hydrogen production rate graphs of different photocatalyst decomposed water;
FIG. 6: the S-CN-D homogeneous nano heterojunction obtained in the example 1 is tested for stability.
Detailed Description
The following examples further illustrate the technical solutions of the present invention, but should not be construed as limiting the scope of the present invention.
The process of the S-CN-D homogeneous nano heterojunction of the invention is as follows:
mixing urea and a sulfur source, adding N, N-dimethylformamide, and stirring and mixing uniformly; the sulfur source is sublimed sulfur powder, ammonium sulfate or thiourea; the mass ratio of the sulfur source to the urea is (0.5-5) to 1; adding 1-50 mL of N, N-dimethylformamide when 10g of sulfur source and urea are added;
heating to 150-400 ℃ for 1-4 h, and then heating to 500-600 ℃ for 1-5 h; the heating rate is 5-15 ℃/min. The slower the rate, the longer the thermal polymerization time, the thicker the sheet layer of the product; the faster the rate, the shorter the thermal polymerization time, and the lower the product yield; the temperature rise process is preferably 200-350 ℃ for 2-3h, and then the temperature rise is carried out to 500-550 ℃ for 2-4 h;
and naturally cooling to room temperature, and grinding to obtain the S-CN-D homogeneous nano heterojunction.
Example 1
Preparing an S-CN-D homogeneous nano heterojunction:
uniformly mixing 10g of urea and sublimed sulfur powder according to the mass ratio of 15:4, adding 20ml of DMF solution, magnetically stirring for 30min, heating to 300 ℃ at the speed of 10 ℃/min in a muffle furnace, maintaining for 1.5h, heating to 520 ℃, maintaining for 4h, and naturally cooling to room temperature to obtain the S-CN-D homogeneous nano heterojunction.
Preparation of CN:
heating 10g of urea in a muffle furnace at a temperature of 10 ℃/min to 550 ℃, maintaining for 4h, and naturally cooling to room temperature to obtain CN.
Preparation of CN-D:
adding 5ml of DMF solution into 10g of urea, magnetically stirring for 30min, heating to 200 ℃ at a speed of 10 ℃/min in a muffle furnace, maintaining for 2h, heating to 600 ℃, maintaining for 4h, and naturally cooling to room temperature to obtain CN-D. The XRD pattern of the S-CN-D homogeneous nano heterojunction obtained in the embodiment is shown in figure 1, and the S-CN-D homogeneous nano heterojunction has two characteristic peaks, wherein 13.1 degrees is a characteristic peak of a (100) crystal face formed by a 3-S-triazine structural unit, 27.5 degrees is a characteristic peak of a (002) crystal face formed by stacking graphite layers of a pi conjugated plane, and the sharp peak type indicates that the product has better crystallinity.
FIG. 2(a) is a schematic diagram of the S-CN-D homoheteroj unction in this example, illustrating the process to produce an S-CN-D homoheteroj unction with both carbon defects and S doping. FIG. 2(b) is a SEM photograph of CN-D having carbon defects, and it can be seen that CN-D is a large lamellar layer having a specific surface area of 112.4m2In FIG. 2(c), the S-CN-D homonano heterojunction in the example is clearly seen in SEM image as a flake, which is smaller and thinner than the CN-D plate, and has a specific surface area of 135.7m2Is also larger than CN-D. FIG. 2(D) is a mapping chart of S-CN-D homogeneous nano-heterojunction in this example, and the product contains a large amount of C, N and a small amount of S, thus proving that S is successfully incorporated into CN.
XPS of the S-CN-D homonano heterojunction obtained in this example is shown in FIG. 3, and analysis of the C/N ratio of 0.75 to 0.73 of CN shows that the S-CN-D homonano heterojunction generates carbon vacancy, and the binding energy of S is also analyzed to be 165.4eV, which further proves that S is successfully doped into CN.
Electrochemical impedance spectroscopy test:
the three photocatalysts (CN, CN-D, S-CN-D) obtained in example 1 were prepared as 1.0mg/L aqueous dispersions, and 5. mu.L of the aqueous dispersions were applied onto the surface of a glassy carbon electrode having a diameter of 3mm by dipping, and the concentration of the solution was 0.005mol/L K3[Fe(CN)6]/K4[Fe(CN)6]Compared with the test in 0.1mol/L KCl solution (shown in figure 4 a), the impedance of the S-CN-D photocatalyst is obviously reduced by 3.1 times compared with the impedance value of CN (52.4 omega)The electron transmission rate of the S-CN-D photocatalyst is obviously accelerated, and the S-CN-D photocatalyst has good photoelectrocatalysis performance.
And (3) testing photocurrent:
three photocatalysts (CN, CN-D and S-CN-D) obtained in example 1 were prepared as 1.0mg/L aqueous dispersions, and 5. mu.L of the aqueous dispersions were applied onto a glassy carbon electrode having a diameter of 3mm by pipetting. Under the illumination condition with the wavelength of 420nm, 1mol/L Na2SO4S-CN-D was measured in the solution: CN-D: the photocurrent ratio of the CN catalyst is about 6:2.5:1 (shown in figure 4 b), wherein the photocurrent of the S-CN-D is the maximum, which shows that the charge transport capability of the catalyst is enhanced and the catalyst has good photoelectrocatalysis performance.
The hydrogen decomposition rates of the CN, CN-D, S-CN-D catalysts obtained in this example are shown in FIG. 5; the CN, CN-D, S-CN-D catalyst generates H under the irradiation of visible light with the wavelength of 420nm2The rates are 373. mu. mol. h, respectively-1·g-1，1650μmol·h-1·g-1，3190μmol·h-1·g-1Wherein the CN-D catalyst produces H2The rate is 4.4 times of CN without adding DMF, which shows that DMF generates carbon defect, enhances the reaction activity of the catalyst for photocatalytic decomposition of water to produce hydrogen, and S is doped to form homogeneous nano heterojunction to produce H2The speed is 8.6 times of CN, which shows that the S-CN-D catalyst after S doping exposes more active catalytic sites and cross-plane diffusion channels, induces the visible light absorption to be enhanced, is beneficial to the separation and transmission acceleration of current carriers, and further enhances the photocatalytic decomposition of the catalyst to produce the aquatic product H2The reactivity of (a).
The S-CN-D homogeneous nano heterojunction stability test obtained in the embodiment is shown in figure 6, and the catalytic performance is not reduced after the S-CN-D homogeneous nano heterojunction is continuously operated for 18 hours, which indicates that the catalyst has good stability.
Example 2
The preparation of S-CN-D homogeneous nano heterojunction in the same step as that in the example 1 is carried out only by changing the ratio of the urea to the sublimed sulfur powder into 15:0, 15:1, 15:3 and 15: 5. Four products are obtained, and H is produced under the irradiation of visible light with the wavelength of 420nm2The rates are: visible light H at 420nm2The rates are 1650 mu mol · h respectively-1·g-1，1730μmol·h-1·g-1，2300μmol·h-1·g-1，2800μmol·h-1·g-1。
Example 3
The three products are obtained by changing the dosage of DMF into 15mL, 20mL and 25mL and the other steps are the same as the preparation of the S-CN-D homogeneous nano heterojunction in the example 1, and H is generated under the irradiation of visible light with the wavelength of 420nm2The rates are: 1800 mu mol. h-1·g-1，3190μmol·h-1·g-1，2800μmol·h-1·g-1。
Claims (4)
1. A preparation method of S-CN-D homogeneous nano heterojunction is characterized by comprising the following steps:
mixing urea and a sulfur source, adding N, N-dimethylformamide, and stirring and mixing uniformly;
heating to 150-400 ℃ for 1-4 h, and then heating to 500-600 ℃ for 1-5 h;
and naturally cooling to room temperature, and grinding to obtain the S-CN-D homogeneous nano heterojunction.
2. The method for preparing S-CN-D homonano-heterojunction as claimed in claim 1, wherein the sulfur source is sublimed sulfur powder, ammonium sulfate or thiourea.
3. The method for preparing S-CN-D homonano-heterojunction as claimed in claim 1, wherein the mass ratio of the sulfur source to the urea is (0.5-5): 1; 1-50 mL of N, N-dimethylformamide is added.
4. The method for preparing S-CN-D homonano-heterojunction as claimed in claim 1, wherein the temperature rise rate is 5-15 ℃/min.
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| CN108579785A (en) * | 2018-04-20 | 2018-09-28 | 武汉工程大学 | Efficient visible light decomposes aquatic products H2Sulfur doping carbonitride preparation method |
| CN110201698A (en) * | 2019-06-03 | 2019-09-06 | 肇庆市华师大光电产业研究院 | A kind of preparation method of polynary nonmetal doping carbon nitride photocatalyst |
| CN110586165A (en) * | 2019-09-30 | 2019-12-20 | 江苏科技大学 | Nitrogen-doped modified g-C3N4Photocatalyst and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108579785A (en) * | 2018-04-20 | 2018-09-28 | 武汉工程大学 | Efficient visible light decomposes aquatic products H2Sulfur doping carbonitride preparation method |
| CN110201698A (en) * | 2019-06-03 | 2019-09-06 | 肇庆市华师大光电产业研究院 | A kind of preparation method of polynary nonmetal doping carbon nitride photocatalyst |
| CN110586165A (en) * | 2019-09-30 | 2019-12-20 | 江苏科技大学 | Nitrogen-doped modified g-C3N4Photocatalyst and preparation method thereof |
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