CN117960168A - Zinc oxide ultrathin nanosheet capable of performing photocatalytic conversion on sulfur hexafluoride as well as preparation method and application thereof - Google Patents
Zinc oxide ultrathin nanosheet capable of performing photocatalytic conversion on sulfur hexafluoride as well as preparation method and application thereof Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 175
- 229910018503 SF6 Inorganic materials 0.000 title claims abstract description 101
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229960000909 sulfur hexafluoride Drugs 0.000 title claims abstract description 101
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 87
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 79
- 239000002135 nanosheet Substances 0.000 title claims abstract description 79
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 104
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 69
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 50
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 48
- 238000003756 stirring Methods 0.000 claims abstract description 35
- 239000012046 mixed solvent Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 26
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 24
- 239000011592 zinc chloride Substances 0.000 claims abstract description 24
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 18
- VJGCZWVJDRIHNC-NSCUHMNNSA-N (e)-1-fluoroprop-1-ene Chemical compound C\C=C\F VJGCZWVJDRIHNC-NSCUHMNNSA-N 0.000 claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000007146 photocatalysis Methods 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 14
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 13
- 229910052731 fluorine Inorganic materials 0.000 claims description 13
- 239000011737 fluorine Substances 0.000 claims description 13
- 229910052724 xenon Inorganic materials 0.000 claims description 8
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 3
- VEFXTGTZJOWDOF-UHFFFAOYSA-N benzene;hydrate Chemical compound O.C1=CC=CC=C1 VEFXTGTZJOWDOF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 abstract description 13
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 50
- 239000000843 powder Substances 0.000 description 34
- 230000000052 comparative effect Effects 0.000 description 22
- 230000005540 biological transmission Effects 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 12
- 239000007791 liquid phase Substances 0.000 description 12
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 12
- 238000004108 freeze drying Methods 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 238000001228 spectrum Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 239000013078 crystal Substances 0.000 description 8
- 238000013032 photocatalytic reaction Methods 0.000 description 8
- 239000010453 quartz Substances 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 239000002585 base Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 238000005481 NMR spectroscopy Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001420 photoelectron spectroscopy Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 239000012084 conversion product Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000005457 ice water Substances 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 230000005311 nuclear magnetism Effects 0.000 description 1
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- 239000004094 surface-active agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention discloses a zinc oxide ultrathin nanosheet capable of performing photocatalytic conversion on sulfur hexafluoride, a preparation method and application, wherein the preparation method comprises the following steps: dissolving sodium dodecyl benzene sulfonate in a mixed solvent of water and ethanol, adding zinc chloride, stirring at 10-18 ℃ for the first time, adding a tetramethyl ammonium hydroxide aqueous solution, a mixed solvent of water and ethanol, stirring at 10-18 ℃ for the second time, separating solid from liquid, washing, drying and calcining at 600-800 ℃ in an air atmosphere. The zinc oxide ultrathin nanosheets are prepared by a simple precipitation method, have uniform morphology and pure phases, and can be used as a photocatalyst and for converting sulfur hexafluoride into 1-fluoropropene by photocatalysis; compared with the traditional method for photo-thermal degradation of SF 6, the method uses the synthesized zinc oxide ultrathin nanosheets as catalysts, has strong catalytic capability, low energy consumption and excellent performance, can simply and stably convert SF 6 gas under normal pressure, and is environment-friendly and sustainable.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a zinc oxide ultrathin nanosheet capable of performing photocatalytic conversion on sulfur hexafluoride, and a preparation method and application thereof.
Background
Sulfur hexafluoride plays an important role in advanced scientific research and related production departments, and is widely applied particularly in the power industry due to excellent electrical insulation and arc extinction. In recent years, the use amount of sulfur hexafluoride has been gradually increased with the continuous development of the electric power industry, and as a powerful greenhouse gas, the global warming potential (Global warming potential, GWP) of sulfur hexafluoride is 23500 times that of CO 2, and the atmospheric lifetime is as long as 3200 years, so that the environmental impact is also increasingly remarkable. However, the chemical property of the sulfur hexafluoride is very stable, so that a large amount of sulfur hexafluoride discharged or leaked to the atmosphere in various industries exists for a long time, and the atmospheric environment is seriously threatened. Therefore, how to simply select a proper catalyst to convert sulfur hexafluoride gas under photo-thermal conditions in order to alleviate the greenhouse effect caused by the sulfur hexafluoride gas is a problem to be solved.
The Chinese patent application publication No. CN111217386A discloses a preparation method of a zinc oxide ultrathin nanosheet, which comprises the following steps: a) Sequentially dissolving sodium dodecyl benzene sulfonate and zinc chloride in a mixed solvent of water and ethanol to obtain an intermediate solution; the mass ratio of the zinc chloride to the sodium dodecyl benzene sulfonate is (240-260): (1000-1200); b) Adding tetramethyl ammonium hydroxide into the intermediate solution to react to obtain zinc oxide ultrathin nanosheets; the mass ratio of the zinc chloride to the tetramethylammonium hydroxide is (240-260): (295-323) with sodium dodecyl benzene sulfonate as surfactant and tetramethyl ammonium hydroxide as strong alkali, can prepare zinc oxide ultrathin nano-sheet with thickness of 1-2 nm in large scale at normal temperature and normal pressure, but is not pointed out that the zinc oxide ultrathin nano-sheet can be used as photocatalyst for catalytic conversion of sulfur hexafluoride to generate fluorine-containing organic substances.
Disclosure of Invention
The technical problem to be solved by the invention is how to prepare a catalyst capable of generating fluorine-containing organic matters by photocatalytic conversion of sulfur hexafluoride.
The invention solves the technical problems by the following technical means:
A preparation method of zinc oxide ultrathin nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride comprises the following steps: dissolving sodium dodecyl benzene sulfonate in a mixed solvent of water and ethanol, adding zinc chloride, stirring at the temperature of 10-18 ℃ for the first time, adding a tetramethyl ammonium hydroxide aqueous solution, a mixed solvent of water and ethanol, stirring at the temperature of 10-18 ℃ for the second time, separating solid from liquid, washing, drying and calcining the stirred product in an air atmosphere at the temperature of 600-800 ℃ to obtain the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride.
Preferably, in the mixed solvent of water and ethanol, the volume ratio of water to ethanol is 2-4: 1.
Preferably, the mass ratio of the zinc chloride to the sodium dodecyl benzene sulfonate is 1-1.5: 2.5-6.
Preferably, the mass ratio of the zinc chloride to the tetramethylammonium hydroxide in the tetramethylammonium hydroxide aqueous solution is 1-1.5: 1.23 to 1.86.
Preferably, the time of one stirring is 1.5-2.5 hours; the secondary stirring time is 1.5-2 hours; the calcination time was 1 hour.
Preferably, the stirring speed is 800-1200r/min during the primary stirring and the secondary stirring.
Preferably, the dosage ratio of the sodium dodecyl benzene sulfonate to the mixed solvent of water and ethanol for dissolving the sodium dodecyl benzene sulfonate is 2.5-6 g:25ml.
Preferably, the mass concentration of the aqueous tetramethylammonium hydroxide solution is 25%; the dosage ratio of the mixed solvent of the added tetramethyl ammonium hydroxide aqueous solution, water and ethanol to the zinc chloride is 6.2ml:6ml: 1-1.5 g.
Preferably, the method further comprises dispersing the calcined product in water, obtaining a uniform suspension after ultrasonic treatment, adding H 2PdCl4 solution under heating, stirring, washing the obtained product, and drying.
Preferably, the preparation method of the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride comprises the following steps: dissolving sodium dodecyl benzene sulfonate into a mixed solvent of water and ethanol, wherein the dosage ratio of the mixed solvent of sodium dodecyl benzene sulfonate, water and ethanol is 2.5-6 g:25ml of zinc chloride is added, stirring is carried out once at the temperature of 10-18 ℃, and then the mixed solvent of the aqueous solution of tetramethyl ammonium hydroxide, water and ethanol is added, wherein the dosage ratio of the added mixed solvent of the aqueous solution of tetramethyl ammonium hydroxide, water and ethanol to the zinc chloride is 6.2ml:6ml: 1-1.5 g, carrying out secondary stirring at 10-18 ℃, carrying out solid-liquid separation, washing and drying on the stirred product, calcining at 600-800 ℃ in an air atmosphere, dispersing the calcined product in water, carrying out ultrasonic treatment to obtain a uniform suspension, and adding an H 2PdCl4 solution at 100 ℃, wherein the dosage ratio of H 2PdCl4 in the calcined product and the H 2PdCl4 solution is 200mg: and (3) 0.02mmol, washing and drying the obtained product after stirring to obtain the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride.
Preferably, in the mixed solvent of water and ethanol for dissolving sodium dodecyl benzene sulfonate, the volume ratio of water to ethanol is 4:1, a step of; in the mixed solvent of water and ethanol added after primary stirring, the volume ratio of water to ethanol is 2:1.
Preferably, the solid-liquid separation and the washing of the product after the secondary stirring are freeze-drying, and the freeze-drying temperature is-50 ℃ to-30 ℃ for more than 36 hours.
The invention also provides a zinc oxide ultrathin nanosheet capable of performing photocatalytic conversion on sulfur hexafluoride, and the zinc oxide ultrathin nanosheet is prepared by adopting the preparation method of the zinc oxide ultrathin nanosheet capable of performing photocatalytic conversion on sulfur hexafluoride.
Preferably, the crystal form of the zinc oxide ultrathin nanosheets capable of photocatalytically converting sulfur hexafluoride is completely consistent with JCPDS card No. 36-1451.
The invention also provides an application of the zinc oxide ultrathin nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride as a catalyst to perform photocatalytic conversion on sulfur hexafluoride to generate fluorine-containing organic substances.
Preferably, the zinc oxide ultrathin nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride are used as catalysts for performing photocatalytic conversion on sulfur hexafluoride to generate fluorine-containing organic substances, CH 3 CN and sulfur hexafluoride are used as reaction raw materials for performing photocatalytic reaction to obtain 1-fluoropropene, and the structural formula of the 1-fluoropropene isThe reaction pressure is normal pressure, the temperature is 60 ℃, the light source is a 300W xenon lamp, and the irradiation time is 10h.
The invention has the advantages that:
According to the invention, the zinc oxide ultrathin nanosheets prepared by a simple precipitation method are calcined at a specific temperature of 600-800 ℃, the obtained product has uniform morphology and pure phase, and meanwhile, more catalytic sites are introduced through calcination treatment, so that the obtained product can be used as a photocatalyst and can be used for converting sulfur hexafluoride into 1-fluoropropene through photocatalysis; compared with the traditional method for photo-thermal degradation of SF 6, the method has the advantages that the calcined zinc oxide ultrathin nanosheets are used as catalysts for photo-catalytic reaction, the reaction energy consumption is low, the performance is excellent, and SF 6 gas can be simply and stably converted into fluorine-containing organic chemicals at normal pressure and near normal temperature, so that the method is environment-friendly and sustainable.
Drawings
FIG. 1 is an XRD diffraction pattern of ultra-thin zinc oxide nanosheets capable of photocatalytic conversion of sulfur hexafluoride prepared in example 1 of the invention;
FIG. 2 is a Transmission Electron Microscope (TEM) and a High Resolution Transmission Electron Microscope (HRTEM) of an ultrathin zinc oxide nano-sheet capable of photocatalytically converting sulfur hexafluoride prepared in example 1 of the invention; wherein, the left image is TEM, the right image is HRTEM;
FIG. 3 is an X-ray photoelectron spectrum (XPS) Zn spectrum of a zinc oxide ultrathin nanosheet capable of performing photocatalytic conversion on sulfur hexafluoride prepared in example 1 of the invention;
FIG. 4 is an X-ray photoelectron spectrum (XPS) O spectrum of a zinc oxide ultrathin nanosheet capable of performing photocatalytic conversion on sulfur hexafluoride prepared in example 1 of the invention;
FIG. 5 is an XRD diffraction pattern of the product prepared in comparative example 1 of the present invention;
FIG. 6 is a Transmission Electron Microscope (TEM) image of the product prepared according to comparative example 1 of the present invention;
FIG. 7 is an XRD diffraction pattern of the product prepared in example 2 of the present invention;
FIG. 8 is a Transmission Electron Microscope (TEM) and a High Resolution Transmission Electron Microscope (HRTEM) of the product prepared in example 2 of the present invention; wherein, the left image is TEM, the right image is HRTEM;
FIG. 9 is an X-ray photoelectron spectrum (XPS) Zn spectrum of a zinc oxide ultrathin nanosheet capable of performing photocatalytic conversion on sulfur hexafluoride prepared in example 2 of the invention;
FIG. 10 is an X-ray photoelectron spectrum (XPS) O spectrum of a zinc oxide ultrathin nanosheet capable of performing photocatalytic conversion on sulfur hexafluoride prepared in example 2 of the invention;
FIG. 11 is an XRD diffraction pattern of the product prepared in comparative example 2 of the present invention;
FIG. 12 is a Transmission Electron Microscope (TEM) image of the product prepared according to comparative example 2 of the present invention;
FIG. 13 is an XRD diffraction pattern of the product prepared in comparative example 3 of the present invention;
FIG. 14 is a Transmission Electron Microscope (TEM) image of the product prepared according to comparative example 3 of the present invention;
FIG. 15 is a nuclear magnetic resonance spectrum of a liquid phase product obtained by photocatalytically converting sulfur hexafluoride, which is a product of comparative example 2 of the present invention;
FIG. 16 is a nuclear magnetic resonance spectrum of a liquid phase product obtained by photocatalytically converting sulfur hexafluoride, which is a product of example 1 of the present invention;
FIG. 17 is an XRD diffraction pattern of ultra-thin nanosheets of zinc oxide capable of photocatalytic conversion of sulfur hexafluoride prepared in example 4 of this invention;
FIG. 18 is a Transmission Electron Microscope (TEM) of an ultrathin nano-sheet of zinc oxide capable of photocatalytically converting sulfur hexafluoride prepared in example 4 of the invention;
FIG. 19 is a nuclear magnetic resonance spectrum of a liquid phase product obtained by photocatalytically converting sulfur hexafluoride, which is a product of example 2 of the present invention;
FIG. 20 is a nuclear magnetic resonance spectrum of a liquid phase product obtained by photo-catalytically converting sulfur hexafluoride with the product of comparative example 1 of the present invention;
FIG. 21 is a nuclear magnetic resonance spectrum of a liquid phase product obtained by photocatalytically converting sulfur hexafluoride, which is a product of comparative example 3 of the present invention;
FIG. 22 is a nuclear magnetic resonance spectrum of a liquid phase product obtained by photo-catalytically converting sulfur hexafluoride in comparative example 9 of the present invention;
FIG. 23 is an XRD diffraction pattern of the product prepared in example 6 of the present invention;
FIG. 24 is a Transmission Electron Microscope (TEM) image of the product prepared according to example 6 of the present invention;
FIG. 25 is an XRD diffraction pattern of the product prepared in example 7 of the present invention;
FIG. 26 is a Transmission Electron Microscope (TEM) image of the product prepared according to example 7 of the present invention;
FIG. 27 is a nuclear magnetic resonance spectrum of a liquid phase product obtained by photocatalytically converting sulfur hexafluoride, which is a product of example 7 of the present invention;
FIG. 28 is a nuclear magnetic resonance spectrum of a liquid phase product obtained by photo-catalytically converting sulfur hexafluoride, which is a product of example 6 of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The test materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Those of skill in the art, without any particular mention of the techniques or conditions, may follow the techniques or conditions described in the literature in this field or follow the product specifications.
Example 1
A preparation method of zinc oxide ultrathin nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride comprises the following steps: 5.576g of sodium dodecyl benzene sulfonate is dissolved in 25mL of a mixed solvent with the volume ratio of water to ethanol being 4:1, 1.225g of zinc chloride is added, and the mixture is stirred at the temperature of 15 ℃ for 2 hours at the speed of 800 revolutions per minute, and 6.2mL of a tetramethyl ammonium hydroxide aqueous solution with the mass fraction of 25% and 6mL of water to ethanol with the volume ratio of 2:1, and stirring at a speed of 800 rpm at 15 ℃ for 1.5 hours. After the reaction, centrifuging, washing the obtained powder with ethanol and water in sequence, and freeze-drying at the temperature of-50 ℃ to-30 ℃ for two days. And (3) placing the dried powder in a muffle furnace at 700 ℃ and calcining for 1 hour in an air atmosphere, wherein the obtained powder is the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride, the mass is about 0.5g, and the zinc oxide ultrathin nanosheets are stored in a dryer for standby.
The structure of the compound prepared in example 1 is identified, and the result is shown in fig. 1-4, and the XRD diffraction pattern of fig. 1 shows that the diffraction peak of the ultra-thin nano-sheet powder of zinc oxide capable of photo-catalytically converting sulfur hexafluoride prepared in example 1 is completely consistent with JCPDS card No.36-1451, which indicates that the phase is hexagonal zinc oxide, wherein the corresponding crystal planes are (1, 0), (0, 2), (1, 0, 1) crystal planes, and the corresponding crystal planes are (1, 0, 2), (1, 0) crystal planes, and (1,0,3) crystal planes when 2-Theta is 31.8 °, 34.4 ° and 36.2 °, respectively, and the corresponding crystal planes are (1, 0, 2), (1, 0) and (1,0,3) crystal planes when 2-Theta is 47.5 °, 56.6 ° and 62.9 °; FIG. 2 shows a Transmission Electron Microscope (TEM) image and a high-resolution transmission electron microscope (HRTEM) image of an ultrathin zinc oxide nano sheet capable of photocatalytically converting sulfur hexafluoride prepared in example 1, wherein the synthesized zinc oxide is in a flake shape as shown in a left TEM image, the interplanar spacing of a prepared sample is 0.285nm as shown in a right HRTEM image, and the dihedral angle is 60 degrees; FIG. 3 is a photoelectron spectrum (XPS) of a synthesized ultrathin zinc oxide nanosheet Zn 2p orbit capable of photocatalytically converting sulfur hexafluoride, wherein the Zn 2p is split into two peaks of 2p 1/2 and 2p 3/2; fig. 4 shows photoelectron spectroscopy (XPS) of synthesized ultra-thin nano-sheet O1 s orbitals of zinc oxide capable of photocatalytically converting sulfur hexafluoride, which shows a single peak, and is in line with the fact.
Example 2
A preparation method of zinc oxide ultrathin nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride comprises the following steps: 5.576g of sodium dodecyl benzene sulfonate is dissolved in 25mL of a mixed solvent with the volume ratio of water to ethanol being 4:1, 1.225g of zinc chloride is added, and the mixture is stirred at the temperature of 15 ℃ for 2 hours at the speed of 800 revolutions per minute, and 6.2mL of a tetramethyl ammonium hydroxide aqueous solution with the mass fraction of 25% and 6mL of water to ethanol with the volume ratio of 2:1, and stirring at a speed of 800 rpm at 15 ℃ for 1.5 hours. After the reaction, centrifuging, washing the obtained powder with ethanol and water in sequence, and freeze-drying at the temperature of-50 ℃ to-30 ℃ for two days. The dried powder is placed in a muffle furnace at 700 ℃ and calcined for 1 hour in an air atmosphere to obtain ZnO powder, then the obtained 200 mg ZnO powder is dispersed in 45mL of deionized water, the uniform suspension is obtained by ultrasonic treatment for 30 minutes, the suspension is transferred into a 100mL round bottom flask, the suspension is placed in an oil bath at 100 ℃, 10mL of 2mM H 2PdCl4 solution is dropwise added under stirring, the stirring is continued for 1 hour, the obtained sample is washed by deionized water for 2 times, and the dried product is placed in an oven at 80 ℃ and dried for 12H, so that the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride are obtained.
The XRD diffraction pattern of fig. 7 shows that the phase of the obtained powder product is hexagonal zinc oxide, and the Transmission Electron Microscope (TEM) and High Resolution Transmission Electron Microscope (HRTEM) of the powder of fig. 8 show that the interplanar spacing of the prepared sample is 0.28 nm, the dihedral angle is 60 °, and the morphology is ultra-thin nano-sheets. FIG. 9 shows photoelectron spectroscopy (XPS) of the Zn 2p orbitals of the synthesized palladium-loaded zinc oxide ultrathin nanosheets, and the Zn 2p split into two peaks of 2p 1/2 and 2p 3/2, and FIG. 10 shows the photoelectron spectroscopy (XPS) of the O1 s orbitals of the synthesized palladium-loaded zinc oxide ultrathin nanosheets as a single peak, which is in line with the fact.
Example 3
The photocatalytic conversion of SF 6 by ultra-thin nanoplatelets of zinc oxide generates 1-fluoropropene as an example:
10mg of the ultrathin zinc oxide nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride prepared in example 1 are dispersed in 2mL of water to obtain a dispersion liquid, and the dispersion liquid is spin-dripped on quartz glass and subjected to heat treatment at 60 ℃ for 2 hours to obtain the photocatalyst-based film. 5mL of CH 3 CN is added at the bottom of a photocatalytic reaction tank container, a quartz column is used for separating CH 3 CN liquid at the bottom from a photocatalyst base film, then a reaction system is vacuumized, and then high-purity sulfur hexafluoride gas with the purity of 99.999% is filled into the reaction system to reach normal pressure. Then circulating water at 60 ℃ is introduced, a 300W xenon lamp is used for simulating a solar light source, and a certain amount of 1-fluoropropene is obtained after irradiation for 10 hours. FIG. 16 is a nuclear magnetism fluorine spectrum of the prepared zinc oxide ultrathin nanosheets capable of photo-catalytically converting sulfur hexafluoride to obtain the product 1-fluoropropene.
Example 4
A preparation method of zinc oxide ultrathin nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride comprises the following steps: 6g of sodium dodecyl benzene sulfonate was dissolved in 25mL of water and ethanol at a volume ratio of 4:1, 1.5g of zinc chloride is added into the mixed solvent, and the mixture is stirred for 2 hours at the temperature of 15 ℃ and the rotation speed of 1200 r/min, and then 6.2mL of tetramethyl ammonium hydroxide aqueous solution with the mass fraction of 25% and 6mL of water and ethanol with the volume ratio of 2:1, and stirring at a speed of 1200 rpm at 15 ℃ for 1.5 hours. After the reaction, centrifuging, washing the obtained powder with ethanol and water in sequence, and freeze-drying at the temperature of-50 ℃ to-30 ℃ for two days. And (3) placing the dried powder in a muffle furnace at 700 ℃, calcining for 1 hour in an air atmosphere, obtaining powder, namely the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride, and storing the zinc oxide ultrathin nanosheets in a dryer for later use. Fig. 17 is an XRD diffraction pattern of the obtained ultra-thin zinc oxide nano-sheet capable of photocatalytically converting sulfur hexafluoride, and fig. 18 is a Transmission Electron Microscope (TEM) image thereof.
Example 5
The only difference from example 3 is that: the palladium-supported zinc oxide ultrathin nanosheets in example 2 are used for replacing the zinc oxide ultrathin nanosheets capable of photo-catalytically converting sulfur hexafluoride in example 3 to catalyze sulfur hexafluoride, fig. 19 is a nuclear magnetic resonance spectrum of 1-fluoropropene obtained by photo-catalytically converting sulfur hexafluoride by the palladium-supported zinc oxide ultrathin nanosheets, and the nuclear magnetic resonance spectrum of example 3 in comparison with fig. 16 shows that the performance of catalyzing sulfur hexafluoride to convert 1-fluoropropene is superior to that of example 3.
Example 6
A preparation method of zinc oxide ultrathin nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride comprises the following steps: 6g of sodium dodecyl benzene sulfonate was dissolved in 25mL of water and ethanol at a volume ratio of 4:1, 1.5g of zinc chloride is added into the mixed solvent, and the mixture is stirred for 1.5 hours at the temperature of 10 ℃ and the rotation speed of 1200 r/min, and then 6.2mL of tetramethyl ammonium hydroxide aqueous solution with the mass fraction of 25% and 6mL of water and ethanol with the volume ratio of 2:1, and stirring at a speed of 1200 rpm at 15 ℃ for 2 hours. After the reaction, centrifuging, washing the obtained powder with ethanol and water in sequence, and freeze-drying at the temperature of-50 ℃ to-30 ℃ for two days. And (3) placing the dried powder in a muffle furnace at 800 ℃, calcining for 1 hour in an air atmosphere, obtaining powder which is the ultrathin zinc oxide nano-sheet capable of carrying out photocatalytic conversion on sulfur hexafluoride, and storing the ultrathin zinc oxide nano-sheet in a dryer for standby. Fig. 23 is an XRD diffraction pattern of the obtained ultra-thin zinc oxide nano-sheet capable of photocatalytically converting sulfur hexafluoride, and fig. 24 is a Transmission Electron Microscope (TEM) diagram thereof.
Example 7
A preparation method of zinc oxide ultrathin nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride comprises the following steps: 6g of sodium dodecyl benzene sulfonate was dissolved in 25mL of water and ethanol at a volume ratio of 4:1, 1.5g of zinc chloride is added into the mixed solvent, and the mixture is stirred for 1.5 hours at the temperature of 10 ℃ and the rotation speed of 1200 r/min, and then 6.2mL of tetramethyl ammonium hydroxide aqueous solution with the mass fraction of 25% and 6mL of water and ethanol with the volume ratio of 2:1, and stirring at a speed of 1200 rpm at 15 ℃ for 2 hours. After the reaction, centrifuging, washing the obtained powder with ethanol and water in sequence, and freeze-drying at the temperature of-50 ℃ to-30 ℃ for two days. And (3) placing the dried powder in a muffle furnace at 600 ℃, calcining for 1 hour in an air atmosphere, obtaining powder, namely the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride, and storing the zinc oxide ultrathin nanosheets in a dryer for later use. Fig. 25 is an XRD diffraction pattern of the obtained ultra-thin zinc oxide nano-sheet capable of photocatalytically converting sulfur hexafluoride, and fig. 26 is a Transmission Electron Microscope (TEM) image thereof.
Example 8
10Mg of the ultrathin zinc oxide nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride prepared in example 7 are dispersed in 2mL of water to obtain a dispersion liquid, and the dispersion liquid is spin-dripped on quartz glass and subjected to heat treatment at 60 ℃ for 2 hours to obtain the photocatalyst-based film. 5mL of CH 3 CN is added at the bottom of a photocatalytic reaction tank container, a quartz column is used for separating CH 3 CN liquid at the bottom from a photocatalyst base film, then a reaction system is vacuumized, and then high-purity sulfur hexafluoride gas with the purity of 99.999% is filled into the reaction system to reach normal pressure. Then circulating water at 60 ℃ is introduced, a 300W xenon lamp is used for simulating a solar light source, and a certain amount of 1-fluoropropene is obtained after irradiation for 10 hours. FIG. 27 is a nuclear magnetic resonance spectrum of 1-fluoropropene obtained by photocatalytically converting sulfur hexafluoride with ultra-thin nanosheets of zinc oxide capable of photocatalytically converting sulfur hexafluoride prepared in example 7.
Example 9
10Mg of the ultrathin zinc oxide nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride prepared in example 6 are dispersed in 2mL of water to obtain a dispersion liquid, and the dispersion liquid is spin-dripped on quartz glass and subjected to heat treatment at 60 ℃ for 2 hours to obtain the photocatalyst-based film. 5mL of CH 3 CN is added at the bottom of a photocatalytic reaction tank container, a quartz column is used for separating CH 3 CN liquid at the bottom from a photocatalyst base film, then a reaction system is vacuumized, and then high-purity sulfur hexafluoride gas with the purity of 99.999% is filled into the reaction system to reach normal pressure. Then circulating water at 60 ℃ is introduced, a 300W xenon lamp is used for simulating a solar light source, and a certain amount of 1-fluoropropene is obtained after irradiation for 10 hours. FIG. 28 is a nuclear magnetic resonance spectrum of 1-fluoropropene obtained by photocatalytically converting sulfur hexafluoride with ultra-thin nanosheets of zinc oxide capable of photocatalytically converting sulfur hexafluoride prepared in example 6.
Comparative example 1
1.225G of zinc chloride was dissolved in 25 mL volumes of water and ethanol in a ratio of 4:1, stirring at a temperature of 15 ℃ for 2 hours at a rotation speed of 800 revolutions per minute, and adding 6.2mL of a tetramethyl ammonium hydroxide aqueous solution with a mass fraction of 25% and 6mL of water and ethanol with a volume ratio of 2:1, and stirring at a speed of 800 rpm at 15 ℃ for 1.5 hours. After the reaction, centrifuging, washing the obtained powder with ethanol and water in sequence, and freeze-drying at the temperature of-50 ℃ to-30 ℃ for two days. The dried powder was placed in a 700 ℃ muffle furnace and calcined for 1 hour in an air atmosphere, and the obtained powder was tested, and as can be seen from fig. 5 and 6, the obtained product was not a zinc oxide ultrathin nanosheet.
Comparative example 2
5.576G of sodium dodecylbenzenesulfonate were dissolved in 25mL of water and ethanol in a volume ratio of 4:1, 1.225g of zinc chloride is added into the mixed solvent, and the mixture is stirred in an ice-water mixture at a speed of 800 revolutions per minute for 2 hours, and 6.2mL of tetramethyl ammonium hydroxide aqueous solution with a mass fraction of 25% and 6mL of water and ethanol with a volume ratio of 2:1, and stirring at 800 rpm under an ice-water mixture for 1.5 hours. After the reaction, centrifuging, washing the obtained powder with ethanol and water in sequence, and freeze-drying at the temperature of-50 ℃ to-30 ℃ for two days. And (3) placing the dried powder in a muffle furnace at 700 ℃ and calcining for 1 hour in an air atmosphere to obtain a powder product. Fig. 11 XRD diffraction pattern illustrates the phase of the composite material as hexagonal zinc oxide, but the Transmission Electron Microscope (TEM) of the powder of fig. 12 shows the morphology as packed chips, not ultra-thin nanoplatelets.
Comparative example 3
5.576G of sodium dodecylbenzenesulfonate were dissolved in 25mL of water and ethanol in a volume ratio of 4:1, 1.225g of zinc chloride is added into the mixed solvent, and the mixture is stirred for 2 hours at the temperature of 15 ℃ and the rotation speed of 800 r/min, and 6.2mL of tetramethyl ammonium hydroxide aqueous solution with the mass fraction of 25% and 6mL of water and ethanol with the volume ratio of 2:1, and stirring at a temperature of 15 ℃ at a speed of 800 revolutions per minute for 1.5 hours. After the reaction, centrifuging, washing the obtained powder with ethanol and water in sequence, and freeze-drying at the temperature of-50 ℃ to-30 ℃ for two days. And (3) placing the dried powder in a muffle furnace at 300 ℃ and calcining for 1 hour in an air atmosphere to obtain a powder product. Fig. 13 XRD diffraction pattern shows that the phase of the composite material is hexagonal zinc oxide, but fig. 14 Transmission Electron Microscopy (TEM) of the powder shows that the resulting zinc oxide flakes are thicker and contaminated.
Comparative example 4
10Mg of the zinc oxide powder obtained in comparative example 2 was dispersed in 2mL of water to obtain a dispersion, and the dispersion was spin-dropped on quartz glass and heat-treated at 60℃for 2 hours to obtain a photocatalyst-based film. 5mL of CH 3 CN is added at the bottom of a photocatalytic reaction tank container, a quartz column is used for separating CH 3 CN liquid at the bottom from a photocatalyst base film, then a reaction system is vacuumized, and then high-purity sulfur hexafluoride gas with the purity of 99.999% is filled into the reaction system to reach normal pressure. Then, circulating water at 60 ℃ is introduced, a 300W xenon lamp is used for simulating a solar light source, the solar light source is irradiated for 10 hours, fig. 15 shows the nuclear magnetic resonance fluorine spectrum of a liquid phase product after the reaction, and as can be seen from fig. 15, no product is obtained, which shows that the material has no catalytic performance.
Comparative example 5
5ML of CH 3 CN is added at the bottom of a photocatalytic reaction tank container, a quartz column is used for separating CH 3 CN liquid at the bottom from blank quartz glass, then the reaction system is vacuumized, and then high-purity sulfur hexafluoride gas with the purity of 99.999% is filled into the reaction system to reach normal pressure. Then, circulating water at 60 ℃ is introduced, a 300W xenon lamp is used for simulating a solar light source, and sulfur hexafluoride cannot be converted after 10 hours of irradiation.
Comparative example 6
The only difference from example 3 is that: DMF was used instead of CH 3 CN in example 3, and no product was formed in the liquid phase.
Comparative example 7
The only difference from example 3 is that: the powder obtained in comparative example 1 is used for replacing the zinc oxide ultrathin nanosheets capable of photo-catalytically converting sulfur hexafluoride obtained in example 1 to be used as a catalyst for catalyzing sulfur hexafluoride, and the nuclear magnetic resonance fluorine spectrum of a liquid phase product obtained after the reaction in FIG. 20 shows that no sulfur hexafluoride conversion product 1-fluoropropene is generated.
Comparative example 8
The only difference from example 3 is that: the powder obtained in comparative example 3 is used for replacing the zinc oxide ultrathin nanosheets capable of photo-catalytically converting sulfur hexafluoride obtained in example 1 to be used as a catalyst for catalyzing sulfur hexafluoride, and the nuclear magnetic resonance fluorine spectrum of a liquid phase product obtained after the reaction in FIG. 21 shows that no sulfur hexafluoride conversion product 1-fluoropropene is generated.
Comparative example 9
5.576G of sodium dodecyl benzene sulfonate is dissolved in 25mL of a mixed solvent with the volume ratio of water to ethanol being 4:1, 1.225g of zinc chloride is added, and the mixture is stirred at the temperature of 15 ℃ for 2 hours at the speed of 800 revolutions per minute, and 6.2mL of a tetramethyl ammonium hydroxide aqueous solution with the mass fraction of 25% and 6mL of water to ethanol with the volume ratio of 2:1, and stirring at a speed of 800 rpm at 15 ℃ for 1.5 hours. After the reaction, centrifuging, washing the obtained powder with ethanol and water in sequence, and freeze-drying at the temperature of-50 ℃ to-30 ℃ for two days. 10mg of the obtained powder was dispersed in 2mL of water to obtain a dispersion, and the dispersion was spin-dropped on quartz glass and heat-treated at 60℃for 2 hours to obtain a photocatalyst-based film. 5mL of CH 3 CN is added at the bottom of a photocatalytic reaction tank container, a quartz column is used for separating CH 3 CN liquid at the bottom from a photocatalyst base film, then a reaction system is vacuumized, and then high-purity sulfur hexafluoride gas with the purity of 99.999% is filled into the reaction system to reach normal pressure. Then, circulating water at 60 ℃ is introduced, a 300W xenon lamp is used for simulating a solar light source, the solar light source irradiates for 10 hours, and FIG. 22 shows a nuclear magnetic fluorine spectrum after the reaction for 10 hours, wherein the nuclear magnetic fluorine spectrum shows no generation of any product.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of zinc oxide ultrathin nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride is characterized by comprising the following steps: the method comprises the following steps: dissolving sodium dodecyl benzene sulfonate in a mixed solvent of water and ethanol, adding zinc chloride, stirring at the temperature of 10-18 ℃ for the first time, adding a tetramethyl ammonium hydroxide aqueous solution, a mixed solvent of water and ethanol, stirring at the temperature of 10-18 ℃ for the second time, separating solid from liquid, washing, drying and calcining the stirred product in an air atmosphere at the temperature of 600-800 ℃ to obtain the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride.
2. The method for preparing the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride according to claim 1, wherein the method is characterized by comprising the following steps: in the mixed solvent of water and ethanol, the volume ratio of water to ethanol is 2-4: 1.
3. The method for preparing the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride according to claim 1, wherein the method is characterized by comprising the following steps: the mass ratio of the zinc chloride to the sodium dodecyl benzene sulfonate is 1-1.5: 2.5-6.
4. The method for preparing the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride according to claim 1, wherein the method is characterized by comprising the following steps: the mass ratio of the zinc chloride to the tetramethylammonium hydroxide in the tetramethylammonium hydroxide aqueous solution is 1-1.5: 1.23 to 1.86.
5. The method for preparing the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride according to claim 1, wherein the method is characterized by comprising the following steps: the time of the primary stirring is 1.5-2.5 hours; the secondary stirring time is 1.5-2 hours; the calcination time was 1 hour.
6. The method for preparing the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride according to any one of claims 1 to 5, wherein the method comprises the following steps: the method also comprises dispersing the calcined product in water, ultrasonic treating to obtain uniform suspension, adding H 2PdCl4 solution under heating, stirring, washing, and drying.
7. The method for preparing the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride according to any one of claims 1 to 5, wherein the method comprises the following steps: the method comprises the following steps: dissolving sodium dodecyl benzene sulfonate into a mixed solvent of water and ethanol, wherein the dosage ratio of the mixed solvent of sodium dodecyl benzene sulfonate, water and ethanol is 2.5-6 g:25ml of zinc chloride is added, stirring is carried out once at the temperature of 10-18 ℃, and then the mixed solvent of the aqueous solution of tetramethyl ammonium hydroxide, water and ethanol is added, wherein the dosage ratio of the added mixed solvent of the aqueous solution of tetramethyl ammonium hydroxide, water and ethanol to the zinc chloride is 6.2ml:6ml: 1-1.5 g, carrying out secondary stirring at 10-18 ℃, carrying out solid-liquid separation, washing and drying on the stirred product, calcining at 600-800 ℃ in an air atmosphere, dispersing the calcined product in water, carrying out ultrasonic treatment to obtain a uniform suspension, and adding an H 2PdCl4 solution at 100 ℃, wherein the dosage ratio of H 2PdCl4 in the calcined product and the H 2PdCl4 solution is 200mg: and (3) 0.02mmol, washing and drying the obtained product after stirring to obtain the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride.
8. An ultrathin zinc oxide nano-sheet capable of photocatalytically converting sulfur hexafluoride, which is characterized in that: the method for preparing the zinc oxide ultrathin nanosheets capable of carrying out photocatalytic conversion on sulfur hexafluoride according to any one of claims 1-7.
9. Use of the ultra-thin zinc oxide nano-sheet capable of photocatalytically converting sulfur hexafluoride as claimed in claim 8 as a catalyst for photocatalytically converting sulfur hexafluoride to generate fluorine-containing organic substances.
10. The application of the zinc oxide ultrathin nanosheets capable of performing photocatalytic conversion on sulfur hexafluoride as a catalyst to perform photocatalytic conversion on sulfur hexafluoride to generate fluorine-containing organic substances, which is characterized in that: the CH 3 CN and sulfur hexafluoride are used as reaction raw materials to carry out photocatalysis reaction to obtain 1-fluoropropene, and the structural formula of the 1-fluoropropene isThe reaction pressure is normal pressure, the temperature is 60 ℃, the light source is a 300W xenon lamp, and the irradiation time is 10h.
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