CN110935437A - Synthetic method of Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water - Google Patents
Synthetic method of Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water Download PDFInfo
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- bismuth vanadate
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 57
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000002096 quantum dot Substances 0.000 title claims abstract description 41
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- FUSNMLFNXJSCDI-UHFFFAOYSA-N tolnaftate Chemical compound C=1C=C2C=CC=CC2=CC=1OC(=S)N(C)C1=CC=CC(C)=C1 FUSNMLFNXJSCDI-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 230000003301 hydrolyzing effect Effects 0.000 title claims description 21
- 238000010189 synthetic method Methods 0.000 title claims description 4
- 238000000034 method Methods 0.000 claims abstract description 19
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 13
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 80
- 239000008367 deionised water Substances 0.000 claims description 37
- 229910021641 deionized water Inorganic materials 0.000 claims description 37
- 239000000243 solution Substances 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 21
- FWPIDFUJEMBDLS-UHFFFAOYSA-L tin(II) chloride dihydrate Chemical compound O.O.Cl[Sn]Cl FWPIDFUJEMBDLS-UHFFFAOYSA-L 0.000 claims description 20
- -1 bismuth vanadate quantum dots Chemical class 0.000 claims description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- IHIXIJGXTJIKRB-UHFFFAOYSA-N trisodium vanadate Chemical compound [Na+].[Na+].[Na+].[O-][V]([O-])([O-])=O IHIXIJGXTJIKRB-UHFFFAOYSA-N 0.000 claims description 3
- GPIHAUAAQOAXNW-UHFFFAOYSA-N O.O.O.O.O.O.O.O.O.O.O.O.[Na] Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Na] GPIHAUAAQOAXNW-UHFFFAOYSA-N 0.000 claims 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 238000000354 decomposition reaction Methods 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 229910001887 tin oxide Inorganic materials 0.000 abstract 2
- 230000000694 effects Effects 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004065 semiconductor Substances 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
-
- 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
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- B01J35/39—
-
- 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
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/661—Chalcogenides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
- C09K11/7457—Vanadates; Chromates; Molybdates; Tungstates
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a method for synthesizing a Z-type tri-tin oxide/bismuth vanadate quantum dot composite photocatalyst capable of fully decomposing water, relates to the field of photocatalysts, and aims to solve the problem that the full decomposition of water under visible light catalysis cannot be realized due to the fact that oxygen cannot be generated by tri-tin oxide due to the existence of polyvalent tin. The method has the advantages of simple process and low cost, and the obtained Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst can realize full water decomposition under the catalysis of visible light.
Description
Technical Field
The invention relates to the field of photocatalysts, in particular to a synthetic method of a Z-shaped stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water.
Background
The visible light semiconductor catalysis technology is emphasized due to the outstanding advantages of simple operation, mild reaction conditions, no secondary pollution, high sunlight utilization rate and the like. Tin tetraoxide is a visible light photocatalyst, and the proper conduction band valence band position of the tin tetraoxide is very suitable for completely decomposing water. However, because the stannic oxide is a multi-component oxide, the interior of the stannic oxide can only produce hydrogen but not oxygen due to the existence of the divalent tin, so that the stannic oxide can not completely decompose water at present.
Disclosure of Invention
The invention aims to solve the problem that the existing stannic oxide can not realize the complete water decomposition under visible light catalysis due to the fact that oxygen can not be generated due to the existence of polyvalent tin, and provides a method for synthesizing a Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst for the complete water decomposition by utilizing a simple hydrothermal process.
The invention relates to a synthesis method of a Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water, which is carried out according to the following steps:
dissolving stannous chloride dihydrate in deionized water, adjusting the pH value to 13, stirring for 30min, and then carrying out ultrasonic treatment for 5 min; adding the treated solution into a high-pressure reaction kettle, carrying out hydrothermal reaction for 12-20h at the temperature of 160-200 ℃, cooling to room temperature, filtering, alternately washing the obtained precipitate for three times by using distilled water and absolute ethyl alcohol, drying for 12h at the temperature of 60-100 ℃, and grinding to obtain the stannic oxide;
dissolving sodium oleate in deionized water, stirring for 30min, adding bismuth nitrate pentahydrate into the solution, and stirring for 30min to obtain a solution A; dissolving sodium orthovanadate dodecahydrate in deionized water, stirring for 30min, adding the solution A, stirring until the solution A is dissolved to obtain a milky solution, adding the milky solution into a high-pressure reaction kettle, carrying out hydrothermal reaction at 90-110 ℃ for 10-14h, cooling to room temperature, filtering, alternately washing the obtained precipitate with n-hexane and absolute ethyl alcohol for three times, drying at 80 ℃ for 12h, and grinding to obtain bismuth vanadate quantum dots;
thirdly, adding the stannic oxide obtained in the first step into deionized water, and carrying out ultrasonic treatment for 10min to obtain a mixed solution; adding the bismuth vanadate quantum dots obtained in the step two into the mixed solution, performing ultrasonic treatment for 10min, stirring for 30min, adding into a high-pressure reaction kettle, performing hydrothermal reaction for 3-5h at the temperature of 100-120 ℃, cooling to room temperature, filtering, washing the obtained precipitate with distilled water and absolute ethyl alcohol once respectively, drying for 12h at the temperature of 80 ℃, and grinding to obtain the Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of completely hydrolyzing water;
wherein the mass volume ratio of the stannous chloride dihydrate to the deionized water is 5-9 g:120 mL; the mass-to-volume ratio of the sodium oleate to the deionized water is 0.5481-0.9135 g: 40 mL; the molar ratio of the bismuth nitrate pentahydrate to the sodium oleate is 1: 2-4; the mass-volume ratio of the sodium dodecavanadate to the deionized water is 0.2401-0.4001 g: 40 mL; the mass volume ratio of the stannic oxide to the deionized water is 0.1-0.3 g: 20 mL; the mass ratio of the bismuth vanadate quantum dots to the stannic oxide is 1: 3 to 9.
The invention has the following beneficial effects:
the Z system is constructed by compounding the material with proper forbidden band width and the tin tetraoxide, and the problem is hopeful to be solved, so that the aim of decomposing water by the tin tetraoxide can be fulfilled.
According to the invention, bismuth vanadate quantum dots with a proper forbidden band width are introduced, and the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst is prepared by a simple hydrothermal method, so that the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of fully decomposing water is obtained. The method for synthesizing the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst has the advantages of mild reaction conditions, simple process and excellent performance of the obtained catalyst, and is suitable for industrial production.
The stannic oxide in the Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water is in a triclinic phase, and the bismuth vanadate quantum dot is in a monoclinic phase, so that the stannic oxide and the bismuth vanadate quantum dot are in a good composite state. As can be seen from the figure IV, in the process of decomposing water by visible light catalysis, the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst obtained by the invention shows excellent activity of decomposing water completely, and the hydrogen production rate is far higher than that of single tri-tin tetroxide, which indicates that the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst obtained by the invention can realize complete decomposition of water and has good activity.
Drawings
Fig. 1 is an XRD chart of the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst obtained in the sixteenth embodiment;
FIG. 2 is a Raman diagram of the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst obtained in the sixteenth embodiment;
FIG. 3 is a TEM image of the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst obtained in the sixteenth embodiment;
FIG. 4 is a diagram illustrating the activity of the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst obtained in the sixteenth embodiment in decomposing water; wherein A is a hydrogen production curve and B is an oxygen production curve.
Detailed Description
The first embodiment is as follows: the synthesis method of the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water in the embodiment is carried out according to the following steps:
dissolving stannous chloride dihydrate in deionized water, adjusting the pH value to 13, stirring for 30min, and then carrying out ultrasonic treatment for 5 min; adding the treated solution into a high-pressure reaction kettle, carrying out hydrothermal reaction for 12-20h at the temperature of 160-200 ℃, cooling to room temperature, filtering, alternately washing the obtained precipitate for three times by using distilled water and absolute ethyl alcohol, drying for 12h at the temperature of 60-100 ℃, and grinding to obtain the stannic oxide;
dissolving sodium oleate in deionized water, stirring for 30min, adding bismuth nitrate pentahydrate into the solution, and stirring for 30min to obtain a solution A; dissolving sodium orthovanadate dodecahydrate in deionized water, stirring for 30min, adding the solution A, stirring until the solution A is dissolved to obtain a milky solution, adding the milky solution into a high-pressure reaction kettle, carrying out hydrothermal reaction at 90-110 ℃ for 10-14h, cooling to room temperature, filtering, alternately washing the obtained precipitate with n-hexane and absolute ethyl alcohol for three times, drying at 80 ℃ for 12h, and grinding to obtain bismuth vanadate quantum dots;
thirdly, adding the stannic oxide obtained in the first step into deionized water, and carrying out ultrasonic treatment for 10min to obtain a mixed solution; adding the bismuth vanadate quantum dots obtained in the step two into the mixed solution, performing ultrasonic treatment for 10min, stirring for 30min, adding into a high-pressure reaction kettle, performing hydrothermal reaction for 3-5h at the temperature of 100-120 ℃, cooling to room temperature, filtering, washing the obtained precipitate with distilled water and absolute ethyl alcohol once respectively, drying for 12h at the temperature of 80 ℃, and grinding to obtain the Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of completely hydrolyzing water;
wherein the mass volume ratio of the stannous chloride dihydrate to the deionized water is 5-9 g:120 mL; the mass-to-volume ratio of the sodium oleate to the deionized water is 0.5481-0.9135 g: 40 mL; the molar ratio of the bismuth nitrate pentahydrate to the sodium oleate is 1: 2-4; the mass-volume ratio of the sodium dodecavanadate to the deionized water is 0.2401-0.4001 g: 40 mL; the mass volume ratio of the stannic oxide to the deionized water is 0.1-0.3 g: 20 mL; the mass ratio of the bismuth vanadate quantum dots to the stannic oxide is 1: 3 to 9.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the pH is adjusted to 13 with 0.05-0.2M sodium hydroxide solution. The rest is the same as the first embodiment.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the mass volume ratio of the stannous chloride dihydrate to the deionized water is 8g:120 mL. The rest is the same as the first embodiment.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the mass volume ratio of the stannous chloride dihydrate to the deionized water is 7g:120 mL. The rest is the same as the first embodiment.
The fifth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: in the first step, the hydrothermal reaction is carried out for 16h at 180 ℃. The rest is the same as the first embodiment.
The sixth specific implementation mode: the first difference between the present embodiment and the specific embodiment is: in the first step, the drying temperature is 80 ℃. The rest is the same as the first embodiment.
The seventh embodiment: the first difference between the present embodiment and the specific embodiment is: the mass-to-volume ratio of the sodium oleate to the deionized water is 0.7301 g: 40 mL. The rest is the same as the first embodiment.
The specific implementation mode is eight: the first difference between the present embodiment and the specific embodiment is: the molar ratio of the bismuth nitrate pentahydrate to the sodium oleate is 1: 3. the rest is the same as the first embodiment.
The specific implementation method nine: the first difference between the present embodiment and the specific embodiment is: the mass-volume ratio of the sodium dodecavanadate to the deionized water is 0.3201 g: 40 mL. The rest is the same as the first embodiment.
The detailed implementation mode is ten: the first difference between the present embodiment and the specific embodiment is: the mass ratio of the bismuth vanadate quantum dots to the stannic oxide is 1: 4. the rest is the same as the first embodiment.
The concrete implementation mode eleven: the first difference between the present embodiment and the specific embodiment is: and the hydrothermal temperature in the step two is 100 ℃, and the hydrothermal time is 12 h. The rest is the same as the first embodiment.
The specific implementation mode twelve: the first difference between the present embodiment and the specific embodiment is: and step three, the hydrothermal temperature is 110 ℃, and the hydrothermal time is 4 hours. The rest is the same as the first embodiment.
The beneficial effects of the present invention are demonstrated by the following examples:
example 1
The method for synthesizing the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of being used for fully decomposing water by using the simple hydrothermal process is realized by the following steps:
firstly, dissolving 7g of stannous chloride dihydrate in 120ml of deionized water, dissolving 0.1M of sodium hydroxide in the deionized water to adjust the pH value to 13, stirring for 30min, carrying out ultrasonic treatment for 5min, adding the solution into a high-pressure reaction kettle, covering a kettle cover, carrying out hydrothermal reaction for 16h at 180 ℃, cooling to room temperature, filtering, alternately washing the obtained precipitate with distilled water and absolute ethyl alcohol for three times, drying for 12h at 80 ℃, and grinding to obtain the stannic oxide.
Secondly, 0.7301g of sodium oleate is dissolved in 40ml of deionized water, the mixture is stirred for 30min, and then 0.388g of bismuth nitrate pentahydrate is added into the solution, and the solution is stirred for 30min, so as to obtain a solution I. 0.3201g of sodium dodecavanadate is dissolved in 40ml of deionized water, the solution is stirred for 30min, the solution is added into the solution I, the stirring is carried out until the solution is dissolved, a milky solution is obtained, the solution is added into a high-pressure reaction kettle, a kettle cover is covered, the hydrothermal reaction is carried out for 12h at the temperature of 100 ℃, the solution is cooled to the room temperature, the filtration is carried out, the obtained precipitate is alternately washed for three times by normal hexane and absolute ethyl alcohol, the drying is carried out for 12h at the temperature of 80 ℃, and the grinding is carried out, thus obtaining the bismuth vanadate quantum dots.
And thirdly, adding 0.2g of the stannic oxide obtained in the first step into 20ml of deionized water, carrying out ultrasonic treatment for 10min, then adding 0.05g of the bismuth vanadate quantum dots obtained in the second step into the solution, carrying out ultrasonic treatment for 10min, and stirring for 30 min. Adding the solution into a high-pressure reaction kettle, covering the kettle cover, carrying out hydrothermal reaction for 4h at the temperature of 110 ℃, cooling to room temperature, filtering, washing the obtained precipitate with distilled water and absolute ethyl alcohol once respectively, drying for 12h at the temperature of 80 ℃, and grinding to obtain the stannic oxide/bismuth vanadate quantum dot capable of fully hydrolyzing water.
As can be seen from fig. 1, in the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of completely decomposing water obtained in this embodiment, the tri-tin tetroxide in the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of completely decomposing water is a triclinic phase, and the bismuth vanadate quantum dot is a monoclinic phase. As can be seen from fig. 2, the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water has characteristic peaks of tri-tin tetroxide and bismuth vanadate quantum dots, and the two show good composite states. As can be seen from FIG. 3, the stannic oxide is of a nanosheet structure, and bismuth vanadate quantum dots with a particle size of about 5nm are uniformly supported thereon. As can be seen from fig. 4, in the process of decomposing water by visible light catalysis, the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst obtained in this embodiment exhibits excellent activity of decomposing water completely, and the hydrogen production rate is much higher than that of a single tri-tin tetroxide, which indicates that the Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst obtained in this embodiment can realize complete decomposition of water and has good activity.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
The present invention is not limited to the above description of the embodiments, and those skilled in the art should, in light of the present disclosure, appreciate that many changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (10)
1. A synthetic method of a Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of completely hydrolyzing water is characterized by comprising the following steps of:
dissolving stannous chloride dihydrate in deionized water, adjusting the pH value to 13, stirring for 30min, and then carrying out ultrasonic treatment for 5 min; adding the treated solution into a high-pressure reaction kettle, carrying out hydrothermal reaction for 12-20h at the temperature of 160-200 ℃, cooling to room temperature, filtering, alternately washing the obtained precipitate for three times by using distilled water and absolute ethyl alcohol, drying for 12h at the temperature of 60-100 ℃, and grinding to obtain the stannic oxide;
dissolving sodium oleate in deionized water, stirring for 30min, adding bismuth nitrate pentahydrate into the solution, and stirring for 30min to obtain a solution A; dissolving sodium orthovanadate dodecahydrate in deionized water, stirring for 30min, adding the solution A, stirring until the solution A is dissolved to obtain a milky solution, adding the milky solution into a high-pressure reaction kettle, carrying out hydrothermal reaction at 90-110 ℃ for 10-14h, cooling to room temperature, filtering, alternately washing the obtained precipitate with n-hexane and absolute ethyl alcohol for three times, drying at 80 ℃ for 12h, and grinding to obtain bismuth vanadate quantum dots;
thirdly, adding the stannic oxide obtained in the first step into deionized water, and carrying out ultrasonic treatment for 10min to obtain a mixed solution; adding the bismuth vanadate quantum dots obtained in the step two into the mixed solution, performing ultrasonic treatment for 10min, stirring for 30min, adding into a high-pressure reaction kettle, performing hydrothermal reaction for 3-5h at the temperature of 100-120 ℃, cooling to room temperature, filtering, washing the obtained precipitate with distilled water and absolute ethyl alcohol once respectively, drying for 12h at the temperature of 80 ℃, and grinding to obtain the Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of completely hydrolyzing water;
wherein the mass volume ratio of the stannous chloride dihydrate to the deionized water is 5-9 g:120 mL; the mass-to-volume ratio of the sodium oleate to the deionized water is 0.5481-0.9135 g: 40 mL; the molar ratio of the bismuth nitrate pentahydrate to the sodium oleate is 1: 2-4; the mass-volume ratio of the sodium dodecavanadate to the deionized water is 0.2401-0.4001 g: 40 mL; the mass volume ratio of the stannic oxide to the deionized water is 0.1-0.3 g: 20 mL; the mass ratio of the bismuth vanadate quantum dots to the stannic oxide is 1: 3 to 9.
2. The method for synthesizing the Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water according to claim 1, wherein the pH is adjusted to 13 by using 0.05-0.2M sodium hydroxide solution.
3. The method for synthesizing the Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of completely hydrolyzing water according to claim 1, wherein the mass-to-volume ratio of stannous chloride dihydrate to deionized water is 7g:120 mL.
4. The method for synthesizing a Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water according to claim 1, wherein the reaction is performed in step one under hydrothermal conditions at 180 ℃ for 16 h.
5. The method for synthesizing the Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water according to claim 1, wherein the drying temperature in the first step is 80 ℃.
6. The method for synthesizing the Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of completely hydrolyzing water according to claim 1, wherein the mass-to-volume ratio of sodium oleate to deionized water is 0.7301 g: 40 mL.
7. The method for synthesizing a Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of completely hydrolyzing water according to claim 1, wherein the molar ratio of bismuth nitrate pentahydrate to sodium oleate is 1: 3.
8. the method for synthesizing the Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of completely hydrolyzing water according to claim 1, wherein the mass-to-volume ratio of sodium dodecahydrate to deionized water is 0.3201 g: 40 mL.
9. The method for synthesizing the Z-type stannic oxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water according to claim 1, wherein the mass-to-volume ratio of stannic oxide to deionized water is 0.2 g: 20 mL.
10. The method for synthesizing a Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water according to claim 1, wherein the mass ratio of bismuth vanadate quantum dots to tri-tin tetroxide is 1: 4.
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