CN108927197B - g-C with high catalytic performance3N4Preparation method and use of - Google Patents
g-C with high catalytic performance3N4Preparation method and use of Download PDFInfo
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 13
- ISAKRJDGNUQOIC-UHFFFAOYSA-N Uracil Chemical compound O=C1C=CNC(=O)N1 ISAKRJDGNUQOIC-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229940035893 uracil Drugs 0.000 claims abstract description 26
- 230000001699 photocatalysis Effects 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 16
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims 1
- 238000007334 copolymerization reaction Methods 0.000 abstract description 7
- 239000011941 photocatalyst Substances 0.000 abstract description 7
- 239000002262 Schiff base Substances 0.000 abstract description 5
- 150000004753 Schiff bases Chemical class 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 239000000969 carrier Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000031700 light absorption Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000010276 construction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000006303 photolysis reaction Methods 0.000 description 3
- 230000015843 photosynthesis, light reaction Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- HNYOPLTXPVRDBG-UHFFFAOYSA-N barbituric acid Chemical compound O=C1CC(=O)NC(=O)N1 HNYOPLTXPVRDBG-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing 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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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/038—Precipitation; Co-precipitation to form slurries or suspensions, e.g. a washcoat
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- 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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- 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
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Abstract
The invention belongs to the technical field of industrial catalysis, and particularly relates to g-C with high catalytic performance3N4The preparation method and the application thereof. The raw materials of the invention are uracil and dicyanodiamine, and g-C with high catalytic activity is obtained through Schiff base reaction and copolymerization3N4A photocatalyst. Direct synthesis of g-C with high catalytic activity by simple and rapid copolymerization method3N4The photocatalyst can be used for preparing hydrogen by decomposing water under the photocatalysis of visible light.
Description
Technical Field
The invention belongs to the technical field of industrial catalysis, and relates to a method for directly synthesizing g-C with high catalytic activity by utilizing a simple and quick copolymerization method3N4The photocatalyst can be used for preparing hydrogen by decomposing water under the photocatalysis of visible light.
Background
Two Japanese scientists, Fujishima and Honda since 1972, utilized n-type TiO2Since the electrodes were used to decompose water to produce hydrogen (a. fujishima, k. honda, Nature,1972,238,37-38.), researchers have invested a great deal of effort in developing sustainable novel photocatalytic materials for solar energy storage and environmental pollution treatment. At present, graphite phase C3N4(g-C3N4) As C3N4The most stable allotrope of the material has certain visible light absorption performance due to the narrow band gap (about 2.7eV), excellent thermal stability and low price, and is considered as the most promising organic semiconductor photocatalytic material. However, g-C is severely limited by the low specific surface area and insufficient light absorption range due to the ultra-high exciton binding energy3N4Photocatalytic activity of (1). At present, for increasing g-C3N4There have been many methods for improving photocatalytic activity, including the construction of nanostructures, element doping (B, P, S, I), and the formation of heterojunctions in combination with other semiconductors. However, element doping and heterojunction formation tend to generate recombination centers of photon-generated carriers, which often makes it difficult to effectively improve the photocatalytic performance of the catalyst, and the construction of the nanostructure consumes time and energy, resulting in increased material cost. Therefore, efficient and inexpensive g-C was developed3N4Method of Material construction of, for g-C3N4IndustrializationThe application is of great importance.
Preparing g-C with wide photoresponse range and strong photocatalytic activity3N4Can be realized by modifying the internal structure of the molecule. In principle, in g-C3N4Embedding other organic functional groups in the molecule can reduce the band gap width and improve the light capture capability. For example: che et al reported a novel (Cring) -C3N4The structure realizes the rapid separation of carriers and further realizes the high-efficiency hydrogen production by photolysis of water (W.Che, W.R.Cheng, T.Yao, F.M.Tang, W.Liu, H.Su, Y.Y.Huang, Q.H.Liu, J.K.Liu, F.C.Hu, Z.Y.Pan, Z.H.Sun, S.Q.Wei, J.Am.chem.Soc.2017,139, 3021-3026.). Zhang et al obtained near infrared responsive g-C by copolymerization of barbituric acid and dicyanodiamine3N4(J.S.Zhang, X.F.Chen, K.Takanabe, K.Maeda, K.Domen, J.P.Epping, X.Z.Fu, M.Antonietti, X.C.Wang, Angew.chem. int.Ed.2010,49, 441-. Recently, Wang et al reported the intercalation of carbon quantum dots into g-C3N4The new method inside the molecular structure greatly weakens the energy barrier of photon-generated carrier transfer (Y.Wang, X.Q.Liu, J.Liu, B.Han, X.Q.Hu, F.Yang, Z.W.Xu, Y.C.Li, S.R.Jia, Z.Li, Angew.chem. int.Ed.2018,57, 5765-charge 5771.). Fully illustrated by the presence of a catalyst in g-C3N4Other organic functional groups or organic components are embedded in the molecule to effectively improve g-C3N4Photocatalytic activity.
Disclosure of Invention
The invention aims to provide a simple and rapid method for synthesizing g-C with high catalytic activity3N4And the photocatalyst is used for photocatalytic water decomposition with visible light to prepare hydrogen. The raw materials of the invention are uracil and dicyanodiamine, and g-C with high catalytic activity is obtained through Schiff base reaction and copolymerization3N4The invention relates to a photocatalyst, which is used for copolymerizing uracil and dicyanodiamine through Schiff base reaction to change g-C3N4The internal structure of the molecule can effectively improve the activity of hydrogen production by photocatalytic water decomposition.
The invention provides g-C with high photocatalytic performance3N4The preparation method of the photocatalyst mainly comprises the following steps:
step 1: mixing dicyanodiamine and uracil, adding distilled water, performing ultrasonic treatment to fully mix the dicyanodiamine and the uracil to obtain a white suspension mixture, transferring the mixture into a reaction kettle to react, and drying the obtained precursor for later use.
The mass ratio of dicyanodiamine to uracil is as follows: 3:0.05-0.1, preferably 3: 0.075.
The mass volume ratio of dicyanodiamine to distilled water is as follows: 3g, 15 mL.
The ultrasonic time is 5 min.
The reaction temperature is 373K, and the reaction time is 24 h.
The drying refers to drying for 12 hours in a vacuum drying oven.
Step 2: calcining the dried precursor in a muffle furnace at 550 ℃ and 2.3 ℃/min for 4h, and grinding to obtain g-C with high photocatalytic performance3N4A photocatalyst.
According to the Schiff base reaction mechanism and the copolymerization process of dicyanodiamine and uracil, after carbon-carbon double bonds are fused in molecules, the band gap is reduced, which can be proved by a Tauc diagram in a figure 1. Furthermore, the mobility of the photogenerated carriers is greatly improved, as shown in fig. 2, a steady-state PL test shows that the exciton recombination chance is reduced by uracil modification, and therefore, the hydrogen production activity is significantly improved.
As shown in FIG. 3, two diffraction peaks appearing in the X-ray diffraction (XRD) pattern are ascribed to g-C3N4Is in accordance with the standard card (JCPDS No. 71-0639). The spectrum shows that g-C is modified by a small amount of uracil3N4The basic structure is not obviously damaged, which indicates that the modification effect of uracil is feasible and the g-C is not completely changed3N4The physicochemical property of the catalyst can realize the hydrogen production by photolysis of water and water.
As shown in FIG. 4, the ultraviolet-visible diffuse reflectance absorption spectrum (UV-Vis) demonstrates the g-C obtained by copolymerizing uracil and dicyanodiamide3N4The light absorption capacity is enhanced, and the light absorption range can be expanded to a near infrared region.
Synthesis of near-infrared responsive g-C by simple and rapid method3N4The material is photocatalytic, and has good activity of hydrogen production by photolysis of water under the irradiation of visible light. The invention has the advantages of cheap and easily obtained raw materials, simple process, less energy consumption, low cost, convenient mass production, no toxicity and harmlessness, and meets the requirements of energy conservation and environmental protection.
Drawings
FIG. 1 is a Tauc map of the invention, showing the modification of g-C by uracil modification3N4The band gap width. Wherein pure g-C3N4The band gap width is 2.75eV, and g-C is modified by 75mg3N4Bandgap width compared to pure g-C3N4The reduction is 0.13 eV.
FIG. 2 is a steady state PL test of the present invention, from which 0.075mg of modified g-C can be seen3N4The weakest fluorescence intensity shows that the photon-generated carriers can be effectively separated, and further the photocatalytic activity can be obviously improved.
FIG. 3 is an XRD spectrum of a sample prepared in examples 1-3 of the present invention, wherein 13 DEG, 27 DEG diffraction peak corresponds to g-C3N4(100) Crystal planes (002) and (002) are basically consistent with the standard card, which shows that g-C is modified by uracil3N4The basic structure is not significantly destroyed.
FIG. 4 is a graph of the ultraviolet-visible diffuse reflectance absorption spectrum (UV-Vis) of samples prepared according to examples 1-3 of the present invention with a significant red shift of the samples with increasing uracil, wherein 0.075g uracil-modified g-C3N4The optical response capability is optimal and can reach a near infrared region.
FIG. 5 is a graph showing the effect of photocatalytic water splitting under visible light conditions on samples prepared in examples 1 to 3 of the present invention. Unmodified g-C can be seen in the figure3N4The hydrogen production efficiency is lower, and the hydrogen production activity is obviously increased along with the increase of uracil. However, when uracil exceeds 0.075g, hydrogen generation efficiency is reduced because excessive uracil addition may destroy g-C3N4The structure of (1). Wherein 0.075g of modified g-C3N4The hydrogen production efficiency is as high as 1003.94 mu mol.h-1·g-1About unmodified g-C3N44.13 times of.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Example 1
Step 1: 3.0g of dicyanodiamide is weighed and placed in an agate mortar and ground for 5min to obtain a uniform sample A.
Step 2: 0.05g of uracil and 3.0g of dicyanodiamide are weighed and placed in an agate mortar, grinding is carried out for 5min, the mixture is transferred into a 50mL beaker, 15mL of distilled water is added, ultrasonic treatment is carried out for 5min, white suspension is obtained after uniform mixing, then the white suspension is transferred into a 50mL reaction kettle, and reaction is carried out for 24h at the temperature of 373K. And after the reaction is finished, taking out the precursor, and drying the precursor in a vacuum drying oven for 12 hours to obtain a sample B.
And step 3: transferring the sample A and the sample B into a covered 50mL circular crucible, horizontally placing the crucible in a muffle furnace, heating the muffle furnace to 550 ℃ at the heating rate of 2.3 ℃/min, reacting for 4h at the temperature, naturally cooling to room temperature to obtain the sample A1And B1。
And 4, step 4: respectively mixing the samples A1And B1Transferring to an agate crucible, grinding for 5min to finally obtain pure g-C3N4(noted CNB) and 0.05g uracil-modified g-C3N4(as CNU)0.05)。
Example 2
Step 1: 3.0g of dicyanodiamide is weighed and placed in an agate mortar and ground for 5min to obtain a uniform sample A.
Step 2: 0.075g of uracil and 3.0g of dicyanodiamide are weighed out and placed in an agate mortar and ground for 5min, the mixture is transferred to a 50mL beaker, 15mL of distilled water is added, ultrasonic treatment is carried out for 5min, and after uniform mixing, a white suspension is obtained and then transferred to a 50mL reaction kettle and reacted for 24h at the temperature of 373K. And after the reaction is finished, taking out the precursor, and drying the precursor in a vacuum drying oven for 12 hours to obtain a sample B.
And step 3: transfer sample A and sample B to capped 5, respectivelyHorizontally placing in a 0mL circular crucible in a muffle furnace, heating the muffle furnace to 550 ℃ at a heating rate of 2.3 ℃/min, reacting for 4h at the temperature, and naturally cooling to room temperature to respectively obtain a sample A1And B1。
And 4, step 4: respectively mixing the samples A1And B1Transferring to an agate crucible, grinding for 5min to finally obtain pure g-C3N4(as CNB) and 0.075g uracil-modified g-C3N4(as CNU)0.075)。
Example 3
Step 1: 3.0g of dicyanodiamide is weighed and placed in an agate mortar and ground for 5min to obtain a uniform sample A.
Step 2: weighing 0.10g of uracil and 3.0g of dicyanodiamide, placing the uracil and the dicyanodiamide in an agate mortar, grinding for 5min, transferring the mixture into a 50mL beaker, adding 15mL of distilled water, performing ultrasonic treatment for 5min, uniformly mixing to obtain a white suspension, transferring the white suspension into a 50mL reaction kettle, reacting at 373K for 24h, taking out the precursor after the reaction is finished, placing the precursor in a vacuum drying oven, and drying for 12h to obtain a sample B.
And step 3: transferring the sample A and the sample B into a covered 50mL circular crucible, horizontally placing the crucible in a muffle furnace, heating the muffle furnace to 550 ℃ at the heating rate of 2.3 ℃/min, reacting for 4h at the temperature, naturally cooling to room temperature to obtain the sample A1And B1。
And 4, step 4: respectively mixing the samples A1And B1Transferring to an agate crucible, grinding for 5min to finally obtain pure g-C3N4(noted CNB) and 0.10g uracil-modified g-C3N4(as CNU)0.10)。
Examples 1-3 controlled addition of varying amounts of uracil to dicyanodiamine to obtain varying amounts of uracil modified g-C by Schiff base reaction and copolymerization3N4In visible light (λ)>420nm), and respectively investigating the photocatalytic hydrogen production performance of the series of products under the conditions of the same catalyst amount (50mg) and the same cocatalyst (3 wt.% Pt). The photocatalysis result shows that the treatment of a small amount of uracil can be carried outObviously improve g-C3N4Photocatalytic activity. In addition, 0.075g of uracil treated product shows the best photocatalytic activity, and the hydrogen production rate can reach 1003.94 mu mol per hour-1·g-1About unmodified g-C3N44.13 times of.
Claims (4)
1. g-C with high catalytic performance3N4The preparation method is characterized by comprising the following specific steps: mixing dicyanodiamine and uracil, adding distilled water, performing ultrasonic treatment to fully and uniformly mix the dicyanodiamine and the uracil to obtain a white suspension mixture, transferring the mixture into a reaction kettle for reaction, and drying an obtained precursor for later use; placing the dried precursor into a muffle furnace for calcining, and grinding to obtain g-C with high catalytic performance3N4(ii) a The mass ratio of dicyanodiamine to uracil is as follows: 3: 0.075; the mass volume ratio of dicyanodiamine to distilled water is as follows: 15mL of 3 g; the ultrasonic time is 5 min; the reaction temperature is 373K, and the reaction time is 24 h.
2. A high catalytic performance g-C as claimed in claim 13N4The preparation method is characterized in that the drying means drying in a vacuum drying oven for 12 hours.
3. A high catalytic performance g-C as claimed in claim 13N4The preparation method is characterized in that the calcination refers to the calcination for 4 hours at the temperature rising rate of 2.3 ℃/min to 550 ℃.
4. High catalytic performance g-C prepared by the method of claim 13N4The application is characterized by being used for preparing hydrogen by photocatalytic water decomposition of visible light.
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