CN110947420B - Preparation method of modified composite nano photocatalyst - Google Patents
Preparation method of modified composite nano photocatalyst Download PDFInfo
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- CN110947420B CN110947420B CN201911032748.9A CN201911032748A CN110947420B CN 110947420 B CN110947420 B CN 110947420B CN 201911032748 A CN201911032748 A CN 201911032748A CN 110947420 B CN110947420 B CN 110947420B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 62
- 239000002131 composite material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000000725 suspension Substances 0.000 claims abstract description 85
- 239000002244 precipitate Substances 0.000 claims abstract description 68
- 239000000243 solution Substances 0.000 claims abstract description 56
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 22
- 229940074404 sodium succinate Drugs 0.000 claims abstract description 21
- ZDQYSKICYIVCPN-UHFFFAOYSA-L sodium succinate (anhydrous) Chemical compound [Na+].[Na+].[O-]C(=O)CCC([O-])=O ZDQYSKICYIVCPN-UHFFFAOYSA-L 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- -1 sodium succinate modified vanadium pentoxide Chemical class 0.000 claims abstract description 16
- KVBGVZZKJNLNJU-UHFFFAOYSA-N naphthalene-2-sulfonic acid Chemical compound C1=CC=CC2=CC(S(=O)(=O)O)=CC=C21 KVBGVZZKJNLNJU-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 239000011858 nanopowder Substances 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 7
- 229920000767 polyaniline Polymers 0.000 description 7
- 230000002776 aggregation Effects 0.000 description 6
- 238000007578 melt-quenching technique Methods 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- CQPFMGBJSMSXLP-UHFFFAOYSA-M acid orange 7 Chemical compound [Na+].OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 CQPFMGBJSMSXLP-UHFFFAOYSA-M 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 239000003945 anionic surfactant Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005253 cladding Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000987 azo dye Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/36—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of vanadium, niobium or tantalum
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Abstract
The present disclosure discloses a preparation method of a modified composite nano photocatalyst, which belongs to the field of catalytic materials. The preparation method comprises the following steps: heating the vanadium pentoxide nanometer powder to a molten state to obtain a vanadium pentoxide melt; adding the vanadium pentoxide melt into an aqueous solution of sodium succinate, and vigorously stirring to obtain a sodium succinate modified vanadium pentoxide suspension; centrifuging the succinic acid ester sodium salt modified vanadium pentoxide suspension to obtain a precipitate; drying the precipitate, adding the precipitate into beta-naphthalene sulfonic acid solution, and performing ultrasonic dispersion to obtain a first suspension; mixing the first suspension with an aniline solution, and performing first cooling to obtain a second suspension; mixing the second suspension with an ammonium persulfate solution, and performing ice bath for the second time to obtain a third suspension; and purifying the third suspension to obtain the modified composite nano photocatalyst. The modified composite nano photocatalyst prepared by the preparation method has good dispersibility.
Description
Technical Field
The present disclosure relates to the field of preparation of catalytic materials, and in particular, to a method for preparing a modified composite nano photocatalyst.
Background
The composite nano photocatalytic material starts in the 80 s as a research hotspot. V (V) 2 O 5 (vanadium pentoxide) is a colorant and catalyst widely used in industry, and is widely used due to its characteristics of being not easily poisoned and being inexpensive. At the same time V 2 O 5 Based on its good stability and suitable semiconductor bandgap width, is considered to be a good choice for the next generation photocatalytic material.
At present, V can be prepared by a melt quenching method 2 O 5 However, during the preparation, V 2 O 5 Nano-powder of (a)The bulk tends to agglomerate, which affects the V 2 O 5 Performance of the photocatalyst.
Disclosure of Invention
The embodiment of the disclosure provides a preparation method of a modified composite nano photocatalyst, which can effectively prevent vanadium pentoxide nanopowder from generating aggregation and agglomeration effects in the melt quenching process by using sodium succinate as an anionic surfactant. The technical scheme is as follows:
the embodiment of the disclosure provides a preparation method of a modified composite nano photocatalyst, which comprises the following steps:
heating the vanadium pentoxide nanometer powder to a molten state to obtain a vanadium pentoxide melt;
adding the vanadium pentoxide melt into an aqueous solution of sodium succinate, and vigorously stirring to obtain a sodium succinate modified vanadium pentoxide suspension;
centrifuging the succinic acid ester sodium salt modified vanadium pentoxide suspension to obtain a precipitate;
drying the precipitate, adding the precipitate into beta-naphthalene sulfonic acid solution, and performing ultrasonic dispersion to obtain a first suspension;
mixing the first suspension with an aniline solution, and performing first cooling to obtain a second suspension;
mixing the second suspension with an ammonium persulfate solution, and performing ice bath for the second time to obtain a third suspension;
and purifying the third suspension to obtain the modified composite nano photocatalyst.
Specifically, the concentration of the aqueous solution of the sodium succinate salt is 0.05mol/L, and the weight-volume ratio of the vanadium pentoxide melt to the aqueous solution of the sodium succinate salt is (1-5) g/100mL.
Specifically, the concentration of the beta-naphthalene sulfonic acid solution is 0.2mol/L, and the weight-volume ratio of the vanadium pentoxide melt to the beta-naphthalene sulfonic acid solution is (1-4) g/500mL.
Specifically, the concentration of the aniline solution is 0.4mol/L, and the weight-volume ratio of the precipitate to the aniline solution is (0.4-4) g/100mL.
Specifically, the precipitate was dried in an oven at 70 ℃ for 4h.
Specifically, the concentration of the ammonium persulfate solution is 0.4mol/L, and the second suspension is mixed with an equal volume of the ammonium persulfate solution.
Specifically, the first ice bath time was 2h.
Specifically, the second ice bath time is 8-24 hours.
Specifically, the method for purifying the third suspension comprises the following steps: and filtering the third suspension to obtain a precipitate, washing the precipitate with ethanol and deionized water respectively, and drying the washed precipitate.
Further, the precipitate after washing was dried at 80℃for 10 hours.
The technical scheme provided by the embodiment of the disclosure has the beneficial effects that: according to the preparation method of the modified composite nano photocatalyst provided by the embodiment of the disclosure, sodium succinate is used as an anionic surfactant, hydrogen bond connection can be effectively generated with the surface of the quenched and solidified particles of the vanadium pentoxide melt, and the interfacial cladding generated by the sodium succinate can effectively prevent aggregation and agglomeration effects generated after the vanadium pentoxide nano powder is subjected to melt quenching, so that the prepared modified composite nano photocatalyst is ensured to have good dispersibility, and further the photochemical performance of the modified composite nano photocatalyst is ensured.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present disclosure, the drawings required for the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present disclosure, and other drawings may be obtained according to these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is an infrared spectrum analysis chart of a modified composite nano-photocatalyst provided in an embodiment of the present disclosure before a photocatalytic reaction;
FIG. 2 is an infrared spectrum analysis of a modified composite nano-photocatalyst provided in an embodiment of the present disclosure after a photocatalytic reaction;
FIG. 3 is a scanning electron microscope analysis chart of a modified composite nano-photocatalyst provided by an embodiment of the present disclosure;
FIG. 4 is a graph of a scanning electron microscope analysis of a comparative example acquisition photocatalyst provided in the comparative example of the present disclosure;
FIG. 5 is a graph showing the results of photocatalytic degradation of orange II with the modified composite nano-photocatalyst of the embodiment of the present disclosure and the photocatalyst provided in the comparative example, wherein 1 is polyaniline, 2 is the photocatalyst provided in the comparative example, and 3 is the modified composite nano-photocatalyst provided in the first embodiment of the present disclosure;
fig. 6 is a comparative graph of methyl orange results of the modified composite nano-photocatalyst of the embodiment of the present disclosure and the photocatalyst provided in the comparative example, in which 4 is polyaniline, 5 is the photocatalyst provided in the comparative example, and 6 is the modified composite nano-photocatalyst provided in the first embodiment of the present disclosure.
Detailed Description
For the purposes of clarity, technical solutions and advantages of the present disclosure, the following further details the embodiments of the present disclosure with reference to the accompanying drawings.
Example 1
The embodiment of the disclosure provides a preparation method of a modified composite nano photocatalyst, which comprises the following steps:
heating vanadium pentoxide nanopowder with purity of 99.9% to molten state at 850 ℃ to obtain vanadium pentoxide melt;
adding 1.0g of vanadium pentoxide melt into 100mL of 0.05mol/L sodium succinate aqueous solution at 25 ℃ and vigorously stirring for 24 hours by using a magnetic stirrer to obtain sodium succinate modified vanadium pentoxide suspension;
centrifuging the succinic acid ester sodium salt modified vanadium pentoxide suspension at 3000rpm for 10min to obtain precipitate;
drying the precipitate, adding 1g of the dried precipitate into 500mL of beta-naphthalene sulfonic acid solution with the concentration of 0.2mol/L, and performing ultrasonic dispersion for 1h to obtain a first suspension;
mixing 200mL of the first suspension with 100mL of aniline solution with the concentration of 0.4mol/L, namely, the weight-volume ratio of the precipitate to the aniline solution is 0.4g/100mL, and performing first cooling to obtain a second suspension;
mixing the second suspension with an ammonium persulfate solution, and performing ice bath for the second time to obtain a third suspension;
and purifying the third suspension to obtain the modified composite nano photocatalyst, namely the vanadium pentoxide-polyaniline photocatalyst.
Specifically, the precipitate was dried in an oven at 70 ℃ for 4h.
Specifically, the concentration of the ammonium persulfate solution was 0.4mol/L, and the second suspension was mixed with an equal volume of the ammonium persulfate solution.
Specifically, the first ice bath time was 2h.
Specifically, the second ice bath time is 8-24 hours.
Specifically, the method for purifying the third suspension comprises the following steps: and filtering the third suspension to obtain a precipitate, washing the precipitate with ethanol and deionized water respectively, and transferring the washed precipitate into a beaker for drying.
Further, the washed precipitate was dried at 80℃for 10 hours.
As shown in fig. 1 and fig. 2, comparing fig. 1 and fig. 2, the result of infrared spectrum analysis of the modified composite nano-photocatalyst obtained in the first embodiment of the present disclosure shows that the modified composite nano-photocatalyst does not have obvious change before and after the reaction, which indicates that the modified composite nano-photocatalyst maintains its chemical stability while treating the organic dye by photocatalysis, and can be reused for multiple times, so that the modified composite nano-photocatalyst has higher economical efficiency.
Example two
The embodiment of the disclosure provides a preparation method of a modified composite nano photocatalyst, which comprises the following steps:
heating vanadium pentoxide nanopowder with purity of 99.9% to molten state at 850 ℃ to obtain vanadium pentoxide melt;
adding 2g of vanadium pentoxide melt into 100mL of water solution of sodium succinate with the concentration of 0.05mol/L at 25 ℃, and vigorously stirring for 24 hours by using a magnetic stirrer to obtain sodium succinate modified vanadium pentoxide suspension;
centrifuging the succinic acid ester sodium salt modified vanadium pentoxide suspension at 3000rpm for 10min to obtain precipitate;
drying the precipitate, adding 1g of the dried precipitate into 500mL of beta-naphthalene sulfonic acid solution with the concentration of 0.2mol/L, and performing ultrasonic dispersion for 1h to obtain a first suspension;
mixing 400mL of the first suspension with 100mL of aniline solution with the concentration of 0.4mol/L, namely, the weight-volume ratio of the precipitate to the aniline solution is 0.8g/100mL, and performing first cooling to obtain a second suspension;
mixing the second suspension with an ammonium persulfate solution, and performing ice bath for the second time to obtain a third suspension;
and purifying the third suspension to obtain the modified composite nano photocatalyst.
Specifically, the precipitate was dried in an oven at 70 ℃ for 4h.
Specifically, the concentration of the ammonium persulfate solution was 0.4mol/L, and the second suspension was mixed with an equal volume of the ammonium persulfate solution.
Specifically, the first ice bath time was 2h.
Specifically, the second ice bath time is 8-24 hours.
Specifically, the method for purifying the third suspension comprises the following steps: and filtering the third suspension to obtain a precipitate, washing the precipitate with ethanol and deionized water respectively, and transferring the washed precipitate into a beaker for drying.
Further, the washed precipitate was dried at 80℃for 10 hours.
Example III
The embodiment of the disclosure provides a preparation method of a modified composite nano photocatalyst, which comprises the following steps:
heating vanadium pentoxide nanopowder with purity of 99.9% to molten state at 850 ℃ to obtain vanadium pentoxide melt;
adding 4g of vanadium pentoxide melt into 100mL of water solution of sodium succinate with the concentration of 0.05mol/L at 25 ℃, and vigorously stirring for 24 hours by using a magnetic stirrer to obtain sodium succinate modified vanadium pentoxide suspension;
centrifuging the succinic acid ester sodium salt modified vanadium pentoxide suspension at 3000rpm for 10min to obtain precipitate;
drying the precipitate, adding 4g of the dried precipitate into 500mL of beta-naphthalene sulfonic acid solution with the concentration of 0.2mol/L, and performing ultrasonic dispersion for 1h to obtain a first suspension;
mixing 500mL of the first suspension with 100mL of aniline solution with the concentration of 0.4mol/L, namely, the weight-volume ratio of the precipitate to the aniline solution is 4g/100mL, and performing first cooling to obtain a second suspension;
mixing the second suspension with an ammonium persulfate solution, and performing ice bath for the second time to obtain a third suspension;
and purifying the third suspension to obtain the modified composite nano photocatalyst.
Specifically, the precipitate was dried in an oven at 70 ℃ for 4h.
Specifically, the concentration of the ammonium persulfate solution was 0.4mol/L, and the second suspension was mixed with an equal volume of the ammonium persulfate solution.
Specifically, the first ice bath time was 2h.
Specifically, the second ice bath time is 8-24 hours.
Specifically, the method for purifying the third suspension comprises the following steps: and filtering the third suspension to obtain a precipitate, washing the precipitate with ethanol and deionized water respectively, and transferring the washed precipitate into a beaker for drying.
Further, the washed precipitate was dried at 80℃for 10 hours.
Example IV
The embodiment of the disclosure provides a preparation method of a modified composite nano photocatalyst, which comprises the following steps:
heating vanadium pentoxide nanopowder with purity of 99.9% to molten state at 850 ℃ to obtain vanadium pentoxide melt;
adding 1.0g of vanadium pentoxide melt into 100mL of 0.05mol/L sodium succinate aqueous solution at 25 ℃ and vigorously stirring for 24 hours by using a magnetic stirrer to obtain sodium succinate modified vanadium pentoxide suspension;
centrifuging the succinic acid ester sodium salt modified vanadium pentoxide suspension at 3000rpm for 10min to obtain precipitate;
drying the precipitate, adding 4g of the dried precipitate into 500mL of beta-naphthalene sulfonic acid solution with the concentration of 0.2mol/L, and performing ultrasonic dispersion to obtain a first suspension;
mixing 500mL of the first suspension with 100mL of aniline solution with the concentration of 0.4mol/L, namely, the weight-volume ratio of the precipitate to the aniline solution is 4g/100mL, and performing first cooling to obtain a second suspension;
mixing the second suspension with an ammonium persulfate solution, and performing ice bath for the second time to obtain a third suspension;
and purifying the third suspension to obtain the modified composite nano photocatalyst.
Specifically, the precipitate was dried in an oven at 70 ℃ for 4h.
Specifically, the concentration of the ammonium persulfate solution was 0.4mol/L, and the second suspension was mixed with an equal volume of the ammonium persulfate solution.
Specifically, the first ice bath time was 2h.
Specifically, the second ice bath time is 8-24 hours.
Specifically, the method for purifying the third suspension comprises the following steps: and filtering the third suspension to obtain a precipitate, washing the precipitate with ethanol and deionized water respectively, and transferring the washed precipitate into a beaker for drying.
Further, the washed precipitate was dried at 80℃for 10 hours.
Example five
The embodiment of the disclosure provides a preparation method of a modified composite nano photocatalyst, which comprises the following steps:
heating vanadium pentoxide nanopowder with purity of 99.9% to molten state at 850 ℃ to obtain vanadium pentoxide melt;
adding 5g of vanadium pentoxide melt into 100mL of water solution of sodium succinate with the concentration of 0.05mol/L at 25 ℃, and vigorously stirring for 24 hours by using a magnetic stirrer to obtain sodium succinate modified vanadium pentoxide suspension;
centrifuging the succinic acid ester sodium salt modified vanadium pentoxide suspension at 3000rpm for 10min to obtain precipitate;
drying the precipitate, adding 2g of the dried precipitate into 500mL of beta-naphthalene sulfonic acid solution with the concentration of 0.2mol/L, and performing ultrasonic dispersion to obtain a first suspension;
mixing 500mL of the first suspension with 500mL of aniline solution with the concentration of 0.4mol/L, namely, the weight-volume ratio of the precipitate to the aniline solution is 0.4g/100mL, and performing first cooling to obtain a second suspension;
mixing the second suspension with an ammonium persulfate solution, and performing ice bath for the second time to obtain a third suspension;
and purifying the third suspension to obtain the modified composite nano photocatalyst.
Specifically, the precipitate was dried in an oven at 70 ℃ for 4h.
Specifically, the concentration of the ammonium persulfate solution was 0.4mol/L, and the second suspension was mixed with an equal volume of the ammonium persulfate solution.
Specifically, the first ice bath time was 2h.
Specifically, the second ice bath time is 8-24 hours.
Specifically, the method for purifying the third suspension comprises the following steps: and filtering the third suspension to obtain a precipitate, washing the precipitate with ethanol and deionized water respectively, and transferring the washed precipitate into a beaker for drying.
Further, the washed precipitate was dried at 80℃for 10 hours.
The result of scanning electron microscope analysis of the modified composite nano-photocatalyst provided in the first embodiment of the present disclosure is shown in fig. 3, and as can be seen from fig. 3, the modified composite nano-photocatalyst has good dispersibility.
Measurement of the specific surface area of the modified composite nano photocatalyst provided in the first embodiment of the present disclosure was 42.3m 2 Per gram, the specific surface area of the photocatalyst provided in the comparative example was measured to be 16.8m 2 And/g. Therefore, the modified composite nano photocatalyst provided in the first embodiment of the disclosure has a larger specific surface area. And the size of single particles is about 25nm, so that the size distribution is relatively uniform.
As a result of scanning electron microscope analysis of the photocatalyst obtained in the comparative example, as shown in fig. 4, it can be seen from comparison of fig. 3 and 4 that the dispersibility of the photocatalyst is not good, and the dispersibility of the modified composite nano-photocatalyst provided in the first embodiment of the present disclosure is superior to that of the photocatalyst provided in the comparative example.
Comparative example
The method for preparing vanadium pentoxide by using the melt quenching method comprises the following specific steps:
heating vanadium pentoxide nanopowder with purity of 99.9% to molten state at 850 ℃ to obtain vanadium pentoxide melt;
adding 5.0g of vanadium pentoxide melt into 50mL of deionized water at 25 ℃, vigorously stirring for 24 hours by using a magnetic stirrer, and finally obtaining a vanadium pentoxide precipitate through centrifugal separation (3000 rpm); and drying the precipitate to obtain vanadium pentoxide powder. The vanadium pentoxide powder is the photocatalyst.
The modified composite nano photocatalyst provided in the first embodiment and the photocatalyst provided in the comparative embodiment are subjected to photocatalytic degradation orange II and methyl orange test respectively, namely, the modified composite nano photocatalyst shows remarkable photocatalytic activity under visible light irradiation through the degradation test of azo dyes. The specific photocatalytic degradation experimental process comprises the following steps: 200ml of orange II is measured by a measuring cylinder, added into a quartz beaker, and vigorously stirred in the dark for 30min to realize adsorption and desorption balance. Then, ultraviolet light (36W high-pressure mercury lamp, purchased from Beijing electric light source research institute) irradiation was performed under stirring, 1 sample was taken every 5min for the first 20min, 1 sample was taken every 20min later, and the photocatalytic time was 4 hours. The test results are shown in fig. 5 and 6, and meanwhile, polyaniline is used as a control, so that the degradation efficiency of the modified composite nano photocatalyst provided in the first embodiment reaches 96.9% and 93.3% respectively in 2h. The photocatalyst provided in the comparative example has degradation efficiencies of 57% and 65% under the same experimental conditions. This is in sharp contrast to the degradation residues of 72% and 91% of polyaniline.
According to the preparation method of the modified composite nano photocatalyst provided by the embodiment of the disclosure, sodium succinate is used as an anionic surfactant, hydrogen bond connection can be effectively generated with the surface of the quenched and solidified particles of the vanadium pentoxide melt, and the interfacial cladding generated by the sodium succinate can effectively prevent aggregation and agglomeration effects generated after the vanadium pentoxide nano powder is subjected to melt quenching, so that the prepared modified composite nano photocatalyst is ensured to have good dispersibility, and further the photochemical performance of the modified composite nano photocatalyst is ensured. In addition, the n-type semiconductor characteristic from vanadium pentoxide and the p-type semiconductor characteristic of polyaniline in the modified composite nano-photocatalyst can generate a photoinduced built-in electric field effect under illumination, so that the photo-generated charges of a phase interface are accelerated to separate, and the overall quantum efficiency is improved, thereby enabling the vanadium pentoxide and the polyaniline in the modified composite nano-photocatalyst to generate a synergistic effect of semiconductor photocatalysis, finally improving the photocatalytic degradation rate, and improving the photocatalytic degradation rate can improve the efficiency of separating and degrading the pollutant by photocatalytic treatment.
The foregoing description of the preferred embodiments of the present disclosure is not intended to limit the disclosure, but rather to enable any modification, equivalent replacement, improvement or the like, which fall within the spirit and principles of the present disclosure.
Claims (9)
1. The preparation method of the modified composite nano photocatalyst is characterized by comprising the following steps of:
heating the vanadium pentoxide nanometer powder to a molten state to obtain a vanadium pentoxide melt;
adding the vanadium pentoxide melt into an aqueous solution of sodium succinate, and vigorously stirring to obtain a sodium succinate modified vanadium pentoxide suspension;
centrifuging the succinic acid ester sodium salt modified vanadium pentoxide suspension to obtain a precipitate;
drying the precipitate, adding the precipitate into beta-naphthalene sulfonic acid solution, and performing ultrasonic dispersion to obtain a first suspension;
mixing the first suspension with an aniline solution, and performing first cooling to obtain a second suspension;
mixing the second suspension with an ammonium persulfate solution, and performing ice bath for the second time to obtain a third suspension;
and purifying the third suspension to obtain the modified composite nano photocatalyst.
2. The preparation method according to claim 1, wherein the concentration of the aqueous solution of the sodium succinate salt is 0.05mol/L, and the weight-to-volume ratio of the vanadium pentoxide melt to the aqueous solution of the sodium succinate salt is (1-5) g/100mL.
3. The preparation method according to claim 1, wherein the concentration of the beta-naphthalene sulfonic acid solution is 0.2mol/L, and the weight-volume ratio of the vanadium pentoxide melt to the beta-naphthalene sulfonic acid solution is (1-4) g/500mL.
4. The method according to claim 1, wherein the concentration of the aniline solution is 0.4mol/L, and the weight-to-volume ratio of the precipitate to the aniline solution is (0.4-4) g/100mL.
5. The method of claim 1, wherein the precipitate is dried in an oven at 70 ℃ for 4 hours.
6. The production method according to claim 1, wherein the concentration of the ammonium persulfate solution is 0.4mol/L, and the second suspension is mixed with an equal volume of the ammonium persulfate solution.
7. The method of claim 1, wherein the second ice bath is performed for 8 to 24 hours.
8. The method of claim 1, wherein the method of purifying the third suspension comprises: and filtering the third suspension to obtain a precipitate, washing the precipitate with ethanol and deionized water respectively, and drying the washed precipitate.
9. The method of claim 8, wherein the washed precipitate is dried at 80 ℃ for 10h.
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| CN1693212A (en) * | 2005-04-25 | 2005-11-09 | 四川大学 | Process for preparing vanadium dioxide nano powder |
| CN109126891A (en) * | 2018-07-09 | 2019-01-04 | 江汉大学 | A kind of preparation method of the polypyrrole nanocluster of the titania additive of modification |
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| CN1693212A (en) * | 2005-04-25 | 2005-11-09 | 四川大学 | Process for preparing vanadium dioxide nano powder |
| CN109126891A (en) * | 2018-07-09 | 2019-01-04 | 江汉大学 | A kind of preparation method of the polypyrrole nanocluster of the titania additive of modification |
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