CN115301278B - Preparation method of carbon nitride photocatalyst and prepared photocatalyst - Google Patents
Preparation method of carbon nitride photocatalyst and prepared photocatalyst Download PDFInfo
- Publication number
- CN115301278B CN115301278B CN202211161474.5A CN202211161474A CN115301278B CN 115301278 B CN115301278 B CN 115301278B CN 202211161474 A CN202211161474 A CN 202211161474A CN 115301278 B CN115301278 B CN 115301278B
- Authority
- CN
- China
- Prior art keywords
- carbon nitride
- catalyst
- ccl
- photocatalyst
- nitride photocatalyst
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 36
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 17
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 239000011541 reaction mixture Substances 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims abstract description 12
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims abstract description 10
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 230000001699 photocatalysis Effects 0.000 claims description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 230000005587 bubbling Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 claims description 4
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical group [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims 2
- 239000003054 catalyst Substances 0.000 abstract description 49
- 238000000034 method Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 230000031700 light absorption Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 239000010453 quartz Substances 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 101001091571 Homo sapiens Kinocilin Proteins 0.000 description 1
- 102100035796 Kinocilin Human genes 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- DLGYNVMUCSTYDQ-UHFFFAOYSA-N azane;pyridine Chemical compound N.C1=CC=NC=C1 DLGYNVMUCSTYDQ-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000010893 electron trap Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
Classifications
-
- 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
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/027—Preparation from water
-
- 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
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Catalysts (AREA)
Abstract
The utility model discloses a preparation method of a carbon nitride photocatalyst and the prepared catalyst, which comprises the steps of firstly mixing a carbon-nitrogen source, potassium salt and LiCl according to a weight ratio of 1:1-2:1-2 to obtain a reaction mixture; the reaction mixture was then subjected to inert gas and CCl 4 Heating the mixture of gases to 450-600 ℃ to react to obtain a reaction product; finally, the reaction product is post-treated to obtain the carbon nitride photocatalyst with K doping and marginal nitrogen vacancy. The preparation method is simple in process and convenient to popularize and implement, and the prepared catalyst has N vacancies and K doping, and has the advantages of remarkably improved light absorption and carrier separation performance and practical value.
Description
Technical Field
The utility model relates to a photocatalyst, in particular to a preparation method of a carbon nitride photocatalyst and the prepared photocatalyst.
Background
The photocatalysis technology has important application prospect in the fields of energy sources, environment and the like as a catalysis technology utilizing solar energy, such as decomposing water into hydrogen and oxygen and CO by utilizing photocatalysis 2 Reducing into organic matters, etc. However, in practice, the photocatalytic reaction also suffers from the disadvantages of low quantum yield, low solar energy utilization rate, easy deactivation of the catalyst, and the like.
Graphite-like phase carbon nitride (GCN) is a stable, low cost and high reserves of polymeric semiconductors. GCN has good visible light response, proper forbidden band position and higher stability in terms of photocatalysis, but it also has higher photogenerated electron-hole recombination rate and lower carrier concentration, which makes GCN overall lower photocatalytic efficiency. For this reason, various attempts have been made to improve GCN photocatalytic efficiency, such as morphology control, heteroatom doping (e.g., S, co and O), vacancy modification, and the like. For example, K atoms are doped, the doped K atoms and pyridine nitrogen can form Lewis acid-base sites, and the life of carriers can be prolonged to a certain extent, but the life of GCN electrons doped by pure K is still too short. Further, if the GCN is modified by N vacancy, the N vacancy can be used as an electron trapping site or an active site to promote charge separation, and the original GC can be improved after modificationN photocatalytic properties, as disclosed in the utility model patent CN109607499B, a marginal nitrogen vacancy g-C 3 N 4 Photocatalyst, process for producing the same, and defect-free g-C 3 N 4 Compared with the prior art, the photocatalytic performance is obviously improved, but the light utilization rate and the carrier separation efficiency are further improved if the photocatalytic performance has practical value.
Disclosure of Invention
The utility model aims to provide a preparation method of a carbon nitride photocatalyst and a corresponding photocatalyst, wherein the preparation method is simple in preparation process and convenient to popularize and implement, and the prepared catalyst has N vacancies and K doping, and the light absorption and carrier separation performances are obviously improved, so that the method has practical value.
In order to achieve the above purpose, the present utility model adopts the following technical scheme:
a preparation method of a carbon nitride photocatalyst comprises the following steps:
step S1: mixing a carbon-nitrogen source, potassium salt and LiCl according to a weight ratio of 1:1-2:1-2 to obtain a reaction mixture, wherein the carbon-nitrogen source is one or more of melamine, urea, thiourea and dicyandiamide;
step S2: the reaction mixture is reacted under inert gas and CCl 4 Heating the mixture of gases to 450-600 ℃ to react to obtain a reaction product;
step S3: and (3) carrying out post-treatment on the reaction product to obtain the K-doped and marginal nitrogen vacancy carbon nitride photocatalyst.
Preferably, in the step S1, the potassium salt is KSCN, KCl, KNO 3 One or more of the following.
Preferably, the inert gas and CCl 4 The mixed gas of the gases is obtained by passing inert gas through liquid CCl 4 Bubbling to obtain the final product.
Preferably, the inert gas and CCl 4 The flow rate of the mixed gas of the gases is 30-1000 sccm.
Preferably, in the step S3, the post-treatment is to wash out the unreacted potassium salt and LiCl in the reaction product with water.
Preferably, the inert gas is nitrogen or argon.
In the technical scheme, the K-doped marginal nitrogen vacancy carbon nitride photocatalyst is successfully prepared by calcining carbon nitrogen sources such as melamine, urea, thiourea, dicyandiamide and the like, potassium salt and LiCl at high temperature in the atmosphere of inert gas and carbon tetrachloride gas, and the catalyst is easier to generate photo-generated electrons-holes and smoothly realize transfer, and has good photocatalytic performance. During the preparation process, the addition of LiCl can help to adjust the melting point of the molten salt formed by LiCl and potassium salt, thereby affecting potassium salt doping and finally affecting the photocatalytic performance of the catalyst. CCl (CCl) 4 The method is favorable for introducing active chlorine into a reaction system so as to effectively improve the polymerization degree of the carbon nitride photocatalyst and also favorable for forming marginal nitrogen vacancies of the photocatalyst.
Drawings
FIG. 1 is an optical photograph of a carbon nitride photocatalyst prepared in example one of the present utility model;
FIG. 2 is an SEM image of a carbon nitride photocatalyst prepared in accordance with one embodiment of the present utility model;
FIG. 3 is an infrared spectrum of the carbon nitride photocatalyst prepared in example one of the present utility model and the catalyst prepared in comparative example 1;
FIG. 4 is a graph showing the comparison of the UV-visible absorption spectra of the carbon nitride photocatalyst prepared in example one of the present utility model and the catalyst prepared in comparative example 1;
FIG. 5 is a graph of N1 s high resolution XPS spectrum of the carbon nitride photocatalyst prepared in example one of the present utility model and the catalyst prepared in comparative example 1;
FIG. 6 is an EDS diagram of a carbon nitride photocatalyst prepared in example one of the present utility model;
FIG. 7 is an EDS diagram of the catalyst prepared in comparative example 1 of the present utility model;
FIG. 8 is a graph showing the comparison of the photocatalytic hydrogen production performance of the carbon nitride photocatalyst prepared in example one of the present utility model and the catalyst prepared in comparative example 1;
FIG. 9 shows photocatalytic production of H by the carbon nitride photocatalyst prepared in example one of the present utility model and the catalyst prepared in comparative example 1 2 O 2 Is a performance graph of (a).
Detailed Description
The utility model is further described below with reference to the accompanying drawings:
example 1 preparation of carbon nitride photocatalyst with K doping and Nitrogen vacancies example 1
Step S1: after 10mmol of melamine, 10mmol of KSCN and 15 mmol of LiCl were ground and mixed uniformly, a reaction mixture was obtained, and the reaction mixture was placed in a quartz boat, and then the quartz boat was placed in a quartz tube.
Step S2: the quartz tube was placed in a tube furnace and then at 300 sccm N 2 /CCl 4 (N 2 From liquid CCl by bubbling machine 4 Inner bulge thus bringing out CCl 4 Gas) is heated for 10 hours at 520 ℃ to obtain a reaction product.
Step S3: the reaction products in the quartz boat are ground into powder, unreacted KSCN and LiCl are washed away by deionized water, and the K-doped and nitrogen vacancy carbon nitride photocatalyst which is denoted as a catalyst 1 (or expressed by letter KNCN) can be obtained.
Example 2 preparation of carbon nitride photocatalyst with K doping and Nitrogen vacancies example 2
Step S1: after 10mmol of thiourea, 10mmol of KCl and 15 mmol of LiCl were ground and mixed uniformly, a reaction mixture was obtained, and the reaction mixture was placed in a quartz boat, which was then placed in a quartz tube.
Step S2: the quartz tube was placed in a tube furnace and then heated at 100 sccm N 2 /CCl 4 (N 2 From liquid CCl by bubbling machine 4 Inner bulge thus bringing out CCl 4 Gas) was heated at 570℃for 4 hours to obtain a reaction product.
Step S3: and (3) grinding reaction products in the quartz boat into powder, and washing unreacted KCl and LiCl by using deionized water to obtain the K-doped and nitrogen-vacancy carbon nitride photocatalyst, which is denoted as a catalyst 2.
Example 3 preparation of carbon nitride photocatalyst with K doping and Nitrogen vacancies example 3
Step S1: 10mmol of urea and 20 mmol of KNO 3 Grinding and uniformly mixing with 20 mmol LiCl to obtain a reaction mixtureThe reaction mixture was placed in a quartz boat, which was then placed in a quartz tube.
Step S2: the quartz tube was placed in a tube furnace and then heated at 1000 sccm N 2 /CCl 4 (N 2 From liquid CCl by bubbling machine 4 Inner bulge thus bringing out CCl 4 Gas) is heated for 6 hours at 450 ℃ to obtain a reaction product.
Step S3: grinding the reaction product in the quartz boat into powder, and washing off unreacted KNO with deionized water 3 And LiCl, a K-doped and nitrogen-vacancy carbon nitride photocatalyst, designated catalyst 3, is obtained.
Example 4 preparation of carbon nitride photocatalyst with K doping and Nitrogen vacancies example 4
Step S1: mixing 10mmol dicyandiamide with 10mmol K 2 SO 4 And 10mmol LiCl are ground and uniformly mixed to obtain a reaction mixture, the reaction mixture is placed in a quartz boat, and then the quartz boat is placed in a quartz tube.
Step S2: the quartz tube was placed in a tube furnace and then at 30 sccm Ar/CCl 4 (Ar from liquid CCl by bubbling machine 4 Inner bulge thus bringing out CCl 4 Gas) is heated for 2 hours at 600 ℃ to obtain a reaction product.
Step S3: grinding the reaction product in the quartz boat into powder, and washing the unreacted K with deionized water 2 SO 4 And LiCl, a K-doped and nitrogen-vacancy carbon nitride photocatalyst, designated catalyst 4, is obtained.
Comparative example 1
The preparation process is the same as in example 1, except that CCl is not introduced 4 Gas only is introduced into N 2 The carrier gas and the product produced is designated catalyst 5 (or indicated by the acronym KCN).
Catalysts 1 to 4 obtained in examples 1 to 4 were characterized, while catalyst 5 obtained in comparative example 1 was characterized, and the results are shown in the accompanying drawings, in which:
fig. 1 is an optical photograph of a catalyst 1, and it can be seen that the catalyst 1 is a yellow powder.
Fig. 2 is an SEM picture of catalyst 1, from which it can be seen that catalyst 1 has uniform particles.
FIG. 3 is an infrared spectrum of catalyst 1 and catalyst 5. As can be seen from FIG. 3, both catalyst 1 and catalyst 5 have significant carbon nitride characteristics and are shown in 990 cm -1 There is an absorption peak, which demonstrates the successful introduction of the K element.
Fig. 4 is a graph comparing the uv-vis absorption spectra of the catalyst 1 and the catalyst 5, and it can be seen from fig. 4 that the catalyst 1 has a significant improvement in light absorption compared to the catalyst 5.
FIG. 5 is a graph of high resolution XPS spectra of N1 s for catalyst 1 and catalyst 5, with the results of FIG. 5 showing that catalyst 1 has significantly lower nitrogen content than catalyst 5, demonstrating successful N vacancy introduction.
Fig. 6 is an EDS diagram of the present catalyst 1, fig. 7 is an EDS diagram of the catalyst 5, and comparing fig. 6 and 7, it can be seen that the catalyst 1 has a significantly lower amount of N element compared to the catalyst 5, which proves the successful construction of the marginal nitrogen vacancies.
FIG. 8 is a graph showing comparison of the photocatalytic hydrogen production performance of catalyst 1 and catalyst 5, and it can be seen from FIG. 8 that catalyst 1 exhibits excellent hydrogen production activity (18.77 mmol g -1 h -1 ) About catalyst 5 (0.039 mmol g) -1 h -1 ) The simultaneous introduction of K element and N vacancy has great promotion effect on hydrogen production activity.
FIG. 9 shows the photocatalytic production of H for catalyst 1 and catalyst 5 2 O 2 The performance diagram of (a) proves that the K element and the N vacancy are simultaneously introduced into the photocatalytic system to produce H 2 O 2 The activity is greatly improved.
The characterization and performance of catalyst 2, catalyst 3 and catalyst 4 are substantially identical to that of catalyst 1.
The present embodiments are merely illustrative of the present utility model and are not intended to be limiting, and the technical solutions that are not substantially transformed under the present utility model are still within the scope of protection.
Claims (6)
1. The application of the carbon nitride photocatalyst in preparing hydrogen peroxide by photocatalysis is characterized in that the preparation method of the carbon nitride photocatalyst comprises the following steps:
step S1: mixing a carbon-nitrogen source, potassium salt and LiCl according to a weight ratio of 1:1-2:1-2 to obtain a reaction mixture, wherein the carbon-nitrogen source is one or more of melamine, urea, thiourea and dicyandiamide;
step S2: the reaction mixture is reacted under inert gas and CCl 4 Heating the mixture of gases to 450-600 ℃ to react to obtain a reaction product;
step S3: and (3) carrying out post-treatment on the reaction product to obtain the K-doped and marginal nitrogen vacancy carbon nitride photocatalyst.
2. The use according to claim 1, wherein in step S1, the potassium salt is KSCN, KCl, KNO 3 One or more of the following.
3. The use according to claim 1, wherein the inert gas and CCl 4 The mixed gas of the gases is obtained by passing inert gas through liquid CCl 4 Bubbling to obtain the final product.
4. The use according to claim 3, wherein the inert gas and CCl 4 The flow rate of the mixed gas of the gases is 30-1000 sccm.
5. The use according to claim 1, wherein in step S3, the post-treatment is washing off unreacted potassium salt and LiCl in the reaction product with water.
6. The use according to claim 3 or 4, wherein the inert gas is nitrogen or argon.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202211161474.5A CN115301278B (en) | 2022-09-23 | 2022-09-23 | Preparation method of carbon nitride photocatalyst and prepared photocatalyst |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202211161474.5A CN115301278B (en) | 2022-09-23 | 2022-09-23 | Preparation method of carbon nitride photocatalyst and prepared photocatalyst |
Publications (2)
Publication Number | Publication Date |
---|---|
CN115301278A CN115301278A (en) | 2022-11-08 |
CN115301278B true CN115301278B (en) | 2024-03-01 |
Family
ID=83866279
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202211161474.5A Active CN115301278B (en) | 2022-09-23 | 2022-09-23 | Preparation method of carbon nitride photocatalyst and prepared photocatalyst |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115301278B (en) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20180114670A (en) * | 2017-04-11 | 2018-10-19 | 포항공과대학교 산학협력단 | Metal ion coordinated polymeric carbon nitride complex, method for manufacturing the same and use thereof |
CN108940338A (en) * | 2018-07-09 | 2018-12-07 | 湖南大学 | Potassium element adulterates nitride porous carbon photochemical catalyst and its preparation method and application |
CN109607499A (en) * | 2018-12-17 | 2019-04-12 | 山东大学 | A kind of limit nitrogen vacancy g-C3N4Photochemical catalyst and preparation method thereof |
CN111992236A (en) * | 2020-09-01 | 2020-11-27 | 福州大学 | Carbon nitrogen catalyst prepared by molten salt thermal polymerization method and having function of photocatalytic oxidation of hydrogen sulfide gas, and preparation method and application thereof |
-
2022
- 2022-09-23 CN CN202211161474.5A patent/CN115301278B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20180114670A (en) * | 2017-04-11 | 2018-10-19 | 포항공과대학교 산학협력단 | Metal ion coordinated polymeric carbon nitride complex, method for manufacturing the same and use thereof |
CN108940338A (en) * | 2018-07-09 | 2018-12-07 | 湖南大学 | Potassium element adulterates nitride porous carbon photochemical catalyst and its preparation method and application |
CN109607499A (en) * | 2018-12-17 | 2019-04-12 | 山东大学 | A kind of limit nitrogen vacancy g-C3N4Photochemical catalyst and preparation method thereof |
CN111992236A (en) * | 2020-09-01 | 2020-11-27 | 福州大学 | Carbon nitrogen catalyst prepared by molten salt thermal polymerization method and having function of photocatalytic oxidation of hydrogen sulfide gas, and preparation method and application thereof |
Also Published As
Publication number | Publication date |
---|---|
CN115301278A (en) | 2022-11-08 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108940344B (en) | Modified graphite phase carbon nitride photocatalyst and preparation method and application thereof | |
CN107824210B (en) | Titanium dioxide composite photocatalyst coated by nitrogen-doped mesoporous carbon and preparation method and application thereof | |
CN108906111B (en) | Self-assembly carbon nitride copolymerized photocatalytic composite material and preparation method and application thereof | |
CN108435229B (en) | Phosphorus-doped hierarchical pore carbon nitride nanosheet and preparation method thereof | |
CN110302824B (en) | Molybdenum-doped graphite-phase carbon nitride catalyst and preparation method and application thereof | |
CN109261188B (en) | Cuprous oxide-copper oxide/carbon nitride composite oxide with adjustable oxygen vacancy as well as preparation method and application thereof | |
CN108993574B (en) | Preparation method of high-performance graphite-phase carbon nitride photocatalytic material | |
CN112495421B (en) | Preparation method of nitrogen-doped carbon quantum dot modified nitrogen-rich graphite type carbon nitride photocatalyst | |
CN113145138B (en) | Thermal response type composite photocatalyst and preparation method and application thereof | |
CN110560119A (en) | Preparation and application of potassium-doped inverse opal carbon nitride photocatalyst | |
CN112871196A (en) | Preparation method of aminated fluorine-doped carbon nitride photocatalyst | |
CN109772394B (en) | Phosphorus-doped carbon/cuprous oxide composite catalyst and preparation method and application thereof | |
CN109607499B (en) | Marginal nitrogen vacancy g-C3N4Photocatalyst and preparation method thereof | |
CN115301278B (en) | Preparation method of carbon nitride photocatalyst and prepared photocatalyst | |
CN108704660B (en) | Preparation and application of nitrogen vacancy modified oxygen-enriched titanium dioxide nano composite material | |
CN113385210A (en) | Photocatalytic hydrogen production catalyst and preparation method and application thereof | |
CN111889127A (en) | In-situ growth preparation of beta-Bi2O3/g-C3N4Method for preparing nano composite photocatalyst | |
CN114345383B (en) | Indium oxide/indium phosphide hollow hexagonal prism p-n junction heterostructure photocatalyst and preparation and application thereof | |
CN108847495A (en) | A kind of film catalyst being used to prepare fuel cell hydrogen and preparation method | |
CN115715989A (en) | Hydroxyl-functionalized double-doped high-crystallinity carbon nitride and preparation method and application thereof | |
CN113441144A (en) | Photocatalytic hydrogen production cocatalyst, photocatalytic system and hydrogen production method | |
CN111905808A (en) | Graphene-based composite material and preparation method thereof | |
CN112717977A (en) | Preparation method and application of ammonia-free airflow synthesis boron-carbon-nitrogen material | |
CN115340071B (en) | Preparation method of hydrogen peroxide | |
CN115283002B (en) | Preparation method and application of carbon nitride-nickel phosphide-crystalline red phosphorus composite photocatalyst |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |