CN110918085A - Porous WO3Preparation method of/C nanosheet mesoporous composite photocatalyst - Google Patents
Porous WO3Preparation method of/C nanosheet mesoporous composite photocatalyst Download PDFInfo
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- CN110918085A CN110918085A CN201911289926.6A CN201911289926A CN110918085A CN 110918085 A CN110918085 A CN 110918085A CN 201911289926 A CN201911289926 A CN 201911289926A CN 110918085 A CN110918085 A CN 110918085A
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 150000001412 amines Chemical class 0.000 claims abstract description 6
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 8
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 3
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 3
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 229910002651 NO3 Inorganic materials 0.000 abstract description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract description 6
- 238000009830 intercalation Methods 0.000 abstract description 3
- 230000010718 Oxidation Activity Effects 0.000 abstract description 2
- 238000005286 illumination Methods 0.000 abstract description 2
- 230000031700 light absorption Effects 0.000 abstract description 2
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 48
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000013335 mesoporous material Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- -1 nitrate ions Chemical class 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
-
- B01J35/39—
-
- B01J35/612—
-
- B01J35/64—
-
- 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
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
Abstract
The invention provides a porous WO3A preparation method of a/C nanosheet mesoporous composite photocatalyst comprises the step of intercalating organic amine into WO3·2H2Adding O hybrid into a porcelain boat, then placing into a tube furnace, introducing nitrogen, heating, keeping the temperature for reaction, naturally cooling to room temperature after the reaction is finished, and obtaining the porous WO3a/C nanosheet mesoporous composite photocatalyst material. Porous WO prepared by the method of the invention3the/C nanosheet mesoporous composite photocatalyst consists of C and porous WO3The composite material with the mesoporous structure formed by the nanosheets has good light absorption performance and a large specific surface area, can efficiently convert nitrogen into nitrate under illumination, and has good photocatalytic oxidation activity.
Description
Technical Field
The invention belongs to the technical field of photocatalysis and photoelectrochemical materials, and particularly relates to porous WO3A preparation method of a/C nanosheet mesoporous composite photocatalyst.
Background
Tungsten trioxide is an n-type semiconductor material with a wide forbidden band, the forbidden band width at room temperature is 2.63eV, the tungsten trioxide can absorb visible light and ultraviolet light below 500nm, and the tungsten trioxide has important application value in the fields of electrochromism, gas sensors, photocatalysis and photoelectric conversion. Compared with the traditional semiconductor material, the nano tungsten trioxide has the advantages of narrow forbidden band width, good photoelectric response performance under the condition of visible light, low price, stable performance, harmlessness and no toxicity, can be used as a photocatalyst, degrades organic pollutants in water and waste gas in air by utilizing sunlight, and is efficient, energy-saving, clean and pollution-free. However, WO3Is closely related to its crystalline phase, morphology, size, morphology, crystal defects and surface properties, which are mainly determined by WO3The preparation method and the preparation conditions of (1). The porous nanosheet is a two-dimensional structure with a cavity, has a high specific surface area, and shows high anisotropy and quantum confinement effect. When the porous nanosheets form a mesoporous structure, diffusion of media is facilitated, and photocatalytic efficiency is improved. Based on this, the present invention provides a porous WO3A preparation method of a/C nanosheet mesoporous composite photocatalyst.
Disclosure of Invention
The invention aims to provide a porous WO3A preparation method of a/C nanosheet mesoporous composite photocatalyst, and solves the problem of the existing WO3The nano-sheet array material has the technical problems of insufficient photoelectric property and low photocatalytic efficiency.
The purpose of the invention is realized by the following technical scheme:
porous WO3A preparation method of a/C nanosheet mesoporous composite photocatalyst comprises the step of intercalating organic amine into WO3·2H2Adding O hybrid into the porcelain boat, then placing into a tube furnace, introducing nitrogen, addingHeating, keeping the temperature for reaction, and naturally cooling to room temperature after the reaction is finished to obtain the porous WO3a/C nanosheet mesoporous composite photocatalyst material.
Porous WO of the invention3The preparation method of the/C nanosheet mesoporous composite photocatalyst comprises the step of calcining organic amine in nitrogen to intercalate WO3·2H2Inorganic/organic layered hybrids of O in porous WO3Carbon is introduced into the surface of the nanosheet in situ to construct porous WO3the/C nanosheet mesoporous material has increased specific surface area and gas adsorbing capacity, and raised visible light absorbing and photoinduced charge separating efficiency, and is favorable to separating electron from hole and raising reaction efficiency and separating efficiency to raise the photocatalytic performance.
In the present invention, organic amine intercalation WO3·2H2The hybrid of O is WO3·2H2O/n-propylamine inorganic/organic layered hybrid, WO3·2H2O/n-butylamine inorganic/organic layered hybrid, WO3·2H2O/n-octylamine inorganic/organic layered hybrid and WO3·2H2O/dodecylamine inorganic/organic layered hybrid.
In the invention, the heating rate is 10-25 ℃/min, the heating is carried out to 400-600 ℃, and the reaction time is 2-4 h.
Compared with the prior art, the invention has the following beneficial effects:
(1) porous WO prepared by the method of the invention3the/C nanosheet mesoporous composite photocatalyst consists of C and porous WO3The composite material with the mesoporous structure formed by the nanosheets has good light absorption performance and a large specific surface area, can efficiently convert nitrogen into nitrate under illumination, and has good photocatalytic oxidation activity.
(2) Porous WO prepared according to the invention3The capability of the/C nanosheet mesoporous composite photocatalyst in photocatalytic oxidation of nitrogen into nitrate is obviously higher than that of pure porous WO3The nano-sheet mesoporous structure can be used as a visible light response material and has great application potential in the aspect of converting nitrogen by photocatalysis.
(3) Porous WO of the invention3The preparation method of the/C nanosheet mesoporous composite photocatalyst is simple and convenient to operate, mild in condition and high in yield, and the prepared material has good photocatalytic water decomposition performance and has great application value in the aspect of photoelectric conversion.
Drawings
FIG. 1 is a porous WO prepared in example 13An XRD (X-ray diffraction) pattern of the/C nanosheet mesoporous composite photocatalyst material;
FIG. 2 shows porous WO prepared in example 1 of the present invention3A TEM image of the/C nanosheet mesoporous composite photocatalyst material;
FIG. 3 shows porous WO prepared in example 1 of the present invention3SEM image of the/C nanosheet mesoporous composite photocatalyst material;
FIG. 4 shows porous WO prepared in example 1 of the present invention3An ultraviolet-visible diffuse reflection spectrogram of the/C nanosheet mesoporous composite photocatalyst material;
FIG. 5 shows porous WO prepared in example 1 of the present invention3An adsorption-desorption diagram of the/C nanosheet mesoporous composite photocatalyst material;
FIG. 6 shows porous WO prepared in example 1 of the present invention3Photocatalytic oxidation N of/C nanosheet mesoporous composite photocatalyst material2To NO3 -A graph of (a).
Detailed Description
The present invention is further described below in conjunction with specific examples to better understand and implement the technical solutions of the present invention for those skilled in the art.
Example 1
Porous WO3The preparation method of the/C nanosheet mesoporous composite photocatalyst comprises the following steps:
0.1gWO3·2H2The O/n-propylamine inorganic/organic layered hybrid is added into a porcelain boat, and then the porcelain boat is put into a tube furnace and nitrogen is introduced. Setting the heating rate at 10 ℃/min, the heating time at 40min, heating to 400 ℃, and the heat preservation time at 2 h. Naturally cooling to room temperature after the reaction is finished, and taking out to obtain the porous WO3a/C nanosheet mesoporous composite photocatalyst material.
Porous WO in this example3An XRD (X-ray diffraction) pattern of the/C nanosheet mesoporous composite photocatalyst material is shown in figure 1; porous WO3A TEM image of the/C nanosheet mesoporous composite photocatalyst material is shown in FIG. 2; porous WO3SEM images of the/C nanosheet mesoporous composite photocatalyst material under different magnifications are shown in figure 3, wherein (a) is 60000 times, (b) is 30000 times, (C) is 10000 times, and (d) is 5000 times; porous WO3An ultraviolet-visible diffuse reflection spectrogram of the/C nanosheet mesoporous composite photocatalyst material is shown in figure 4; porous WO3An adsorption-desorption diagram of the/C nanosheet mesoporous composite photocatalyst material is shown in figure 5.
Example 2
Porous WO3The preparation method of the/C nanosheet mesoporous composite photocatalyst comprises the following steps:
0.5gWO3·2H2Adding the O/n-butylamine inorganic/organic layered hybrid into a porcelain boat, then putting the porcelain boat into a tube furnace, and introducing nitrogen. Setting the heating rate at 25 ℃/min, the heating time at 40min, heating to 600 ℃, and the heat preservation time at 4 h. Naturally cooling to room temperature after the reaction is finished, and taking out to obtain the porous WO3a/C nanosheet mesoporous composite photocatalyst material.
Example 3
Porous WO3The preparation method of the/C nanosheet mesoporous composite photocatalyst comprises the following steps:
0.2gWO3·2H2Adding the O/n-octylamine inorganic/organic layered hybrid into a porcelain boat, then putting the porcelain boat into a tube furnace, and introducing nitrogen. Setting the heating rate at 15 ℃/min, the heating time at 40min, heating to 500 ℃ and the heat preservation time at 3 h. Naturally cooling to room temperature after the reaction is finished, and taking out to obtain the porous WO3a/C nanosheet mesoporous composite photocatalyst material.
Example 4
Porous WO3The preparation method of the/C nanosheet mesoporous composite photocatalyst comprises the following steps:
0.3gWO3·2H2Adding O/dodecylamine inorganic/organic layered hybrid into porcelain boatThen the porcelain boat is put into a tube furnace, and nitrogen is introduced. Setting the heating rate at 20 ℃/min, the heating time at 40min, heating to 600 ℃, and the heat preservation time at 4 h. Naturally cooling to room temperature after the reaction is finished, and taking out to obtain the porous WO3a/C nanosheet mesoporous composite photocatalyst material.
Weighing of the porous WO prepared in example 13Pouring 20mg of a/C nanosheet mesoporous composite photocatalyst material sample into a beaker, adding 120mL of ultrapure water into the beaker, and carrying out ultrasonic treatment for 30 min. Checking the air tightness of the device, pouring the ultrasonic sample into a photoreactor with good air tightness, sealing again and checking the air tightness. Vacuumizing the reactor by using a vacuum pump, injecting nitrogen and oxygen into the reactor by using a needle tube (the ratio is 3:1), standing for 1h, turning on a xenon lamp current-stabilizing power supply, placing the photoreactor on a magnetic stirrer for stirring, and adjusting a light source to place the photoreactor in an illumination center. Sampling is carried out once every half hour, 8mL of the sample is taken every time and injected into the sampling tube, and a proper amount of nitrogen and oxygen is supplemented every time of sampling, so that the nitrogen and oxygen in the photoreactor are sufficient, and the reaction time is 3 hours. And after the reaction is finished, sending the taken liquid sample to an ion chromatograph to detect whether nitrate ions are contained. The nitrate concentration was calculated by measuring the peak area of the sample from a standard solution fitted curve of the nitrate concentration and the peak area, and finally a time-concentration curve was made, with the results shown in FIG. 6.
As can be seen from FIG. 1, b has distinct diffraction peaks at 23.08 °, 23.71 °, 24.09 °, 33.33 ° and 34.02 °, corresponding to WO3(001), (020), (200), (021), (220) in/C standard card (JCPDFCardNO.53-0433) shows that WO is generated3a/C complex. a is pure porous WO used as a control3A nano mesoporous material.
WO can be seen from FIG. 23The nano-sheet has many pores, and the black particles are carbon, which is compatible with the porous WO3The nanosheets being bonded together to form WO3a/C complex.
WO can be seen in FIG. 33·2H2Sintering of O/propylamine inorganic/organic layered hybrids in nitrogen to give WO3Nanosheets, and shapes between nanosheetsThe mesoporous structure is rich, and the structure has larger specific surface area and porosity, and can improve the photocatalytic performance.
WO can be seen from FIG. 43The n-propylamine precursor has no absorption between 300-500nm, WO3Porous WO with powder having larger absorption in the range of less than 500nm3The absorption range of the nano-sheet mesoporous structure is below 450 nm. Porous WO3the/C nanosheet mesoporous composite material has high absorption in ultraviolet and high absorption in the whole visible light region, and is prepared by modifying carbon in porous WO3Results on/C nanoplates. The carbon modification enhances the absorption of a visible light region, can improve the utilization rate of the visible light and enhances the photocatalytic activity.
From FIG. 5, it can be seen that the porous WO3The mesoporous structure of the/C nanosheet has large specific surface area (5.5855 m)2/g), more active sites may be generated, thereby contributing to the enhancement of the photocatalytic performance of the composite material.
WO porosity can be seen in FIG. 63the/C nanosheet mesoporous composite material is used as a catalyst, the yield of the generated silver nitrate is continuously increased, and the yield of the silver nitrate is always higher than that of pure porous WO within the same reaction time3Nanosheet mesoporous material, in particular porous WO after 1.5h of reaction3The catalytic efficiency of the/C nanosheet mesoporous composite material is increased and is obviously higher than that of pure porous WO3A nano-sheet mesoporous material. This indicates that the photocatalytic performance of the composite is better.
The above embodiments illustrate various embodiments of the present invention in detail, but the embodiments of the present invention are not limited thereto, and those skilled in the art can achieve the objectives of the present invention based on the disclosure of the present invention, and any modifications and variations based on the concept of the present invention fall within the scope of the present invention, which is defined by the claims.
Claims (3)
1. Porous WO3The preparation method of the/C nanosheet mesoporous composite photocatalyst is characterized in that organic amine is intercalated into WO3·2H2Of OAdding the hybrid into a porcelain boat, then placing the porcelain boat into a tube furnace, introducing nitrogen, heating, keeping the temperature for reaction, naturally cooling to room temperature after the reaction is finished, and obtaining the porous WO3a/C nanosheet mesoporous composite photocatalyst material.
2. Porous WO according to claim 13The preparation method of the/C nanosheet mesoporous composite photocatalyst is characterized in that organic amine is intercalated into WO3·2H2The hybrid of O is WO3·2H2O/n-propylamine inorganic/organic layered hybrid, WO3·2H2O/n-butylamine inorganic/organic layered hybrid, WO3·2H2O/n-octylamine inorganic/organic layered hybrid and WO3·2H2O/dodecylamine inorganic/organic layered hybrid.
3. Porous WO according to claim 1 or 23The preparation method of the/C nanosheet mesoporous composite photocatalyst is characterized in that the heating rate is 10-25 ℃/min, the heating is carried out to 400-600 ℃, and the reaction time is 2-4 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111514911A (en) * | 2020-05-08 | 2020-08-11 | 桂林理工大学 | Carbon-doped WP nanosheet electrocatalyst with mesoporous structure and preparation method thereof |
| CN112604697A (en) * | 2020-12-20 | 2021-04-06 | 桂林理工大学 | Copper ion doped zinc oxide/cadmium sulfide high-performance water decomposition hydrogen production photocatalyst and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111514911A (en) * | 2020-05-08 | 2020-08-11 | 桂林理工大学 | Carbon-doped WP nanosheet electrocatalyst with mesoporous structure and preparation method thereof |
| CN111514911B (en) * | 2020-05-08 | 2023-04-07 | 桂林理工大学 | Carbon-doped WP nanosheet electrocatalyst with mesoporous structure and preparation method thereof |
| CN112604697A (en) * | 2020-12-20 | 2021-04-06 | 桂林理工大学 | Copper ion doped zinc oxide/cadmium sulfide high-performance water decomposition hydrogen production photocatalyst and preparation method thereof |
| CN112604697B (en) * | 2020-12-20 | 2022-06-17 | 桂林理工大学 | Copper ion doped zinc oxide/cadmium sulfide high-performance water decomposition hydrogen production photocatalyst and preparation method thereof |
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