CN117696079B - Nickel oxide composite PbBiO2Br S-type heterojunction catalyst and preparation method and application thereof - Google Patents
Nickel oxide composite PbBiO2Br S-type heterojunction catalyst and preparation method and application thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 10
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000243 solution Substances 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002244 precipitate Substances 0.000 claims abstract description 17
- 229910052724 xenon Inorganic materials 0.000 claims abstract description 15
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 238000005286 illumination Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 230000002195 synergetic effect Effects 0.000 claims abstract description 9
- 150000002815 nickel Chemical class 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000012046 mixed solvent Substances 0.000 claims description 15
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical class [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 150000001621 bismuth Chemical class 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical group [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical group [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 4
- 229940046892 lead acetate Drugs 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229940078494 nickel acetate Drugs 0.000 claims description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical group Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910001451 bismuth ion Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000000527 sonication Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 2
- 230000003197 catalytic effect Effects 0.000 abstract description 26
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 230000000593 degrading effect Effects 0.000 abstract description 7
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 29
- 229940043267 rhodamine b Drugs 0.000 description 29
- 238000006731 degradation reaction Methods 0.000 description 26
- 230000015556 catabolic process Effects 0.000 description 25
- 239000000047 product Substances 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 15
- 230000000694 effects Effects 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 12
- 238000006555 catalytic reaction Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 229910021642 ultra pure water Inorganic materials 0.000 description 7
- 239000012498 ultrapure water Substances 0.000 description 7
- 238000005119 centrifugation Methods 0.000 description 5
- 238000002256 photodeposition Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
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- 230000004044 response Effects 0.000 description 4
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- 239000000843 powder Substances 0.000 description 3
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- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000295 complement effect Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 229910002117 Bi 4Ti3O12 Inorganic materials 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- KQNKJJBFUFKYFX-UHFFFAOYSA-N acetic acid;trihydrate Chemical compound O.O.O.CC(O)=O KQNKJJBFUFKYFX-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 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 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 229940078487 nickel acetate tetrahydrate Drugs 0.000 description 1
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 description 1
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
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- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
- B01J27/13—Platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
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- 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
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
The invention relates to a preparation method of an S-type heterojunction catalyst of nickel oxide composite PbBiO 2 Br, which comprises the steps of preparing PbBiO 2 Br by adopting a hydrothermal method; then PbBiO 2 Br is added into the solution of the soluble divalent nickel salt, and ultrasonic treatment is carried out to form uniform dispersion suspension; and (3) placing the dispersion suspension under a 300-400W xenon lamp for illumination for 1-4 hours, centrifuging after illumination is finished, collecting precipitate, washing the precipitate by using a deionized water and ethanol mixed solution, and drying to obtain the NiO/PbBiO 2 Br heterojunction catalyst. The preparation method is simple, and the prepared S-shaped heterojunction catalyst has high-efficiency photocatalysis, piezocatalysis and photo-piezoelectricity synergistic catalytic activity, can be used for efficiently catalyzing and degrading organic pollutants in water, and solves the problems that the method for improving the catalytic activity through morphology control in the prior art is difficult and is not suitable for large-scale production and application.
Description
Technical Field
The invention relates to the technical field of catalyst and organic matter degradation, in particular to an S-shaped heterojunction catalyst and a preparation method and application thereof.
Background
Currently, organic pollutants in the environment are degraded mainly by biological, physical or chemical methods. In contrast, photocatalytic technology, which can utilize clean and renewable solar energy to achieve reactions such as pollutant degradation and hydrogen production under mild conditions, is considered to be an ideal solution to environmental pollution and energy-related challenges. Piezoelectric catalysis is a catalysis technology which is only recently attracting attention and utilizes mechanical vibration to induce charges on the surface of piezoelectric materials to trigger catalytic reaction. Piezocatalysis technology is considered to be an effective complement to photocatalysis because it can use mechanical energy abundant in the environment and operate in the dark. Interestingly, some studies revealed that there is a synergistic effect between piezocatalysis and photocatalysis. The catalytic efficiency of the catalyst can be significantly improved if ultrasonic vibration is applied simultaneously during the irradiation. For example, shalma et al (ACS omega, 2022,7,7595-7605) found that the alternating built-in electric field generated by NaNbO 3 nanorods under periodic vibration effectively inhibited the recombination of photogenerated charges, superior to single piezocatalysis and photocatalysis. Children et al (Nano Energy, 2023, 108, 108202) prepared Bi 4Ti3O12 with oxygen vacancies and observed 3.7-fold and 2.0-fold superior piezoelectricity-photo catalytic activity in RhB degradation than single photo-and piezoelectricity catalysis, respectively. Therefore, the piezoelectric-photocatalytic technology is expected to play an important role in the field of organic pollutant degradation.
Since it was reported in 1988 that NiO and Cu 2 O materials piezocatalytically decompose water, a number of piezoelectric catalysts including ZnO, KTa xNb1-xO3、SrTiO3 and Pb (Zr xTi1-x)O3 was reported and applied to dye degradation, hydrogen production, nitrogen fixation and carbon dioxide reduction) were typical piezoelectric materials with asymmetric centers responsible for their piezoelectric effect.
Disclosure of Invention
First, the technical problem to be solved
In view of the defects and shortcomings of the prior art, the invention provides a preparation method of an S-shaped heterojunction catalyst of nickel oxide composite PbBiO 2 Br, which is simple, has photocatalytic and piezoelectric catalytic activities, can be used for efficiently catalyzing and degrading organic pollutants in water, and solves the problems that the method for improving the catalytic activity through morphology control in the prior art is difficult and is not suitable for large-scale production and application.
(II) technical scheme
In a first aspect, the invention provides a method for preparing an S-type heterojunction catalyst of nickel oxide composite PbBiO 2 Br, which comprises the following steps:
S1, preparing PbBiO 2 Br
Dispersing soluble divalent lead salt, soluble trivalent bismuth salt and soluble bromine salt in a mixed solvent of deionized water and ethylene glycol according to a molar ratio of 1-1.05:1-1.05:1-1.05, and stirring until the mixture is uniformly dispersed, wherein the volume ratio of deionized water to ethylene glycol in the mixed solvent is 15-22:1; slowly dripping the obtained solution into excessive sodium hydroxide or potassium hydroxide solution under stirring, regulating the pH of a reaction system to 12.5-13.5 by using nitric acid, transferring into a high-pressure reaction kettle, carrying out hydrothermal reaction at 135-145 ℃ for 10-16h, cooling to room temperature after the reaction is finished, separating a precipitate, washing the precipitate by using a deionized water and ethanol mixed solution, and drying to obtain PbBiO 2 Br;
s2, preparing NiO/PbBiO 2 Br heterojunction catalyst
Dispersing soluble divalent nickel salt in a mixed solvent of water and methanol, adding PbBiO 2 Br prepared in the step S1 into the mixed solvent, and performing ultrasonic treatment to form uniform dispersion suspension; and (3) placing the dispersion suspension under a 300-400W xenon lamp for illumination for 1-4 hours, centrifuging after illumination is finished, collecting precipitate, washing the precipitate by using a deionized water and ethanol mixed solution, and drying to obtain the NiO/PbBiO 2 Br heterojunction catalyst.
According to a preferred embodiment of the invention, the molar ratio of PbBiO 2 Br to nickel salt in S2 is 1-1.1:1.
According to the preferred embodiment of the invention, in S2, the soluble divalent nickel salt is nickel acetate or hydrate thereof, and after the soluble divalent nickel salt is dispersed in a mixed solvent of water and methanol, a dispersion liquid with the concentration of 0.02-0.04mol/L is obtained, and then PbBiO 2 Br is added; the volume ratio of water to methanol in the water mixed solvent is 25-35:10.
In accordance with a preferred embodiment of the present invention, in S2, the power of the sonication is 120W sonicator for 30 minutes to form a uniform dispersion suspension.
According to a preferred embodiment of the invention, in S2, the dispersion is exposed to a 350W xenon lamp for 1 hour, 1.5 hours, 2 hours or 2.5 hours, more preferably 2 hours.
According to a preferred embodiment of the present invention, in S1, the soluble divalent lead salt is lead acetate or a hydrate thereof, the soluble trivalent bismuth salt is bismuth nitrate or a hydrate thereof, and the soluble bromine salt is sodium bromide.
According to the preferred embodiment of the invention, in S1, the dispersion concentration of the soluble divalent lead salt, the soluble trivalent bismuth salt and the soluble bromine salt in the mixed solvent of deionized water and ethylene glycol is respectively 0.07-0.1mol/L; the molar amount of the solute in the sodium hydroxide or potassium hydroxide solution is 20 times or more, preferably 50 to 100 times, the sum of the molar amounts of lead ions and bismuth ions.
According to the preferred embodiment of the invention, in S1, after the dripping of the obtained solution to sodium hydroxide or potassium hydroxide solution is completed, nitric acid is used for adjusting the pH value of the reaction system to 13, the reaction system is transferred into a high-pressure reaction kettle for hydrothermal reaction at 140 ℃ for 12 hours, after the reaction is completed, the reaction system is cooled to room temperature, the precipitate is separated, and the precipitate is washed for 3 times by using a mixed solution of deionized water and ethanol, and then PbBiO 2 Br is obtained after drying.
In a second aspect, the present invention provides a nickel oxide composite PbBiO 2 Br S-type heterojunction catalyst prepared by the preparation method of any one of the above embodiments.
In a third aspect, the present invention provides a method for the catalytic degradation of organic matter in water, comprising: the S-type heterojunction catalyst of nickel oxide composite PbBiO 2 Br is put into water, and ultrasonic vibration and/or illumination are applied to the water, so that organic matters in the water are degraded.
(III) beneficial effects
According to the invention, niO is synthesized in situ and is combined to PbBiO 2 Br through a photo-deposition method, so that the S-type heterojunction composite material NiO/PbBiO 2 Br is constructed, the composite material has high-efficiency photocatalytic and piezocatalytic activities, and the rate of piezocatalytic degradation of RhB is more than 31 times of the rate constant of single NiO catalytic degradation. Experiments also find that although PbBiO 2 Br also shows certain piezocatalysis characteristics, the rate of piezocatalysis degradation of the S-type heterojunction composite material is 12.4 times of the rate constant of single PbBiO 2 Br catalytic degradation. In addition, under the synergistic effect of light and ultrasound, the degradation rate of RhB is 1.2 times and 1.35 times of that of single photocatalysis and piezocatalysis respectively when the S-type heterojunction composite material is used as a catalyst. This demonstrates that the photocatalysis and piezocatalysis of the S-type heterojunction composite material also have a synergistic effect.
According to the preparation method, pbBiO 2 Br is firstly applied to synthesis of the piezoelectric or photo-piezoelectric synergistic catalyst, and the piezoelectric catalysis and photo-piezoelectric synergistic catalytic activity of PbBiO 2 Br are further improved by adopting NiO nanoparticle modification. The NiO nano particles are synthesized in situ and deposited on the surface of PbBiO 2 Br, an S-type heterojunction is constructed between the bonding interface of NiO and PbBiO 2 Br, the S-type heterojunction does not lose the redox capacity of electrons and holes while promoting the separation of carriers (the action mechanism does not improve the separation efficiency of carriers by capturing electrons, so that the reduction capacity of electrons is not reduced), and excellent piezoelectric and photoelectrocatalytic activities are obtained.
The preparation method of the NiO/PbBiO 2 Br S-type heterojunction catalyst is only carried out by a common hydrothermal combined photo-deposition method, and compared with a morphology control method, the preparation method has the advantages of simple operation, easily obtained raw materials, mild conditions and easy control, and is suitable for large-scale production and application.
Drawings
FIG. 1 is a Raman diagram of the product prepared in example 3 and the products prepared in comparative examples 1-2.
FIG. 2 is an XRD pattern for the product prepared in example 3 and the product prepared in comparative examples 1-2.
Fig. 3 is a TEM image of the product prepared in example 3.
FIG. 4 is an XPS plot of the product prepared in example 3 versus the product prepared in comparative examples 1-2.
FIG. 5 is a comparison of the activity of the catalysts of examples 1-4 and comparative examples 1-2 in piezocatalytically degrading RhB.
FIG. 6 is a first order kinetic fit of the catalysts of examples 1-4 and comparative examples 1-2 during piezocatalytically degrading RhB.
Fig. 7 is a cycle test chart of the catalyst prepared in example 3 in piezocatalytically degrading RhB.
FIG. 8 is a comparison of catalytic activity of the catalyst prepared in example 3 in piezo-electric catalysis, photo-piezo co-catalysis degradation of RhB.
FIG. 9 is a graph comparing piezoelectric response currents of the catalyst prepared in example 3 and the catalysts of comparative examples 1 to 2.
Detailed Description
The invention will be better explained by the following detailed description of the embodiments with reference to the drawings.
According to the invention, niO nano particles are loaded on the surface of PbBiO 2 Br by a photo-deposition method, so that an S-type heterojunction structure is constructed, and the oxidation-reduction capability of electrons and holes is not lost while the separation of carriers is promoted, thereby obtaining excellent activity of piezoelectricity to catalyze and degrade organic matters. Further research also proves that NiO/PbBiO 2 Br also has photo-piezoelectric synergistic catalytic activity, and the catalytic activity of NiO/PbBiO 2 Br can be initiated under the drive of light and/or ultrasonic vibration so as to catalyze the degradation of organic matters.
The present invention will be described in detail with reference to preferred embodiments thereof. The S-type heterojunction catalyst of NiO/PbBiO 2 Br in the following examples can be recorded as xNiO/PbBiO 2 Br, x represents the duration of the light deposition treatment under a xenon lamp in the synthesis process, and x is 1-4h.
Example 1
The method for preparing the S-type heterojunction catalyst in the embodiment is as follows:
(1) Preparation PbBiO 2 Br
First, 20.0g of sodium hydroxide was weighed and dissolved in 30ml of ultrapure water to obtain a sodium hydroxide solution.
Then 1.4552 g (0.003 mol) bismuth nitrate pentahydrate, 1.1380g (0.003 mol) lead acetate trihydrate and 0.3086g (0.003 mol) sodium bromide were weighed out respectively, and dispersed in a mixed solvent composed of 40ml deionized water and 2ml ethylene glycol, and magnetically stirred for 0.5 hours to obtain a mixed solution containing bismuth nitrate and lead acetate. Then, the mixed solution is slowly dripped into the sodium hydroxide solution prepared before under stirring, after the dripping is finished, 6.0mol/L nitric acid solution is used to make the pH value of the solution be 13, after magnetic stirring is carried out for 0.5h, the solution is transferred into a stainless steel autoclave with a polytetrafluoroethylene lining of 100ml, and ultrapure water is added to make the total volume of the suspension be 80ml; and carrying out hydrothermal reaction for 12 hours at 140 ℃, pouring out supernatant after the reaction is finished and cooled to room temperature, collecting sediment at the bottom, centrifugally washing the sediment for 3 times by adopting a mixed solution of ultrapure water and ethanol, and then putting the sediment into an oven for drying for 12 hours at 60 o C to obtain a target product PbBiO 2 Br.
(2) Preparation of catalyst NiO/PbBiO 2 Br
0.2822G of nickel acetate tetrahydrate was weighed and dissolved in a mixed solution composed of 30ml of ultrapure water and 10ml of methanol to obtain a nickel acetate solution. 1.0g of the NiO/PbBiO 2 Br powder of the catalyst prepared in the step (1) is weighed and added into the nickel acetate solution, and the mixture is placed into a 120W ultrasonic machine for ultrasonic treatment for 30min to form uniform suspension, and the uniform suspension is placed under a 350W xenon lamp for illumination for 1 hour. After the illumination is finished, the precipitate is collected by a centrifuge. And (3) centrifugally washing for 3 times by using a mixed solution of ultrapure water and alcohol, putting into a vacuum oven, and drying for 12 hours under the vacuum environment of 60 o ℃ to obtain the target product 1-NiO/PbBiO 2 Br catalyst.
Example 2
This example is the same as step (1) of example 1, with only a slight difference in step (2), specifically, the "350W xenon lamp under light for 1 hour" is adjusted to: and (3) irradiating for 1.5 hours under a 350W xenon lamp to obtain the target product 1.5-NiO/PbBiO 2 Br catalyst.
Example 3
This example is the same as step (1) of example 1, with only a slight difference in step (2), specifically, the "350W xenon lamp under light for 1 hour" is adjusted to: and (3) irradiating for 2 hours under a 350W xenon lamp to obtain the target product 2-NiO/PbBiO 2 Br catalyst.
Example 4
This example is the same as step (1) of example 1, with only a slight difference in step (2), specifically, the "350W xenon lamp under light for 1 hour" is adjusted to: and (3) irradiating for 2.5 hours under a 350W xenon lamp to obtain the target product 2.5-NiO/PbBiO 2 Br catalyst.
Comparative example 1
The desired product PbBiO 2 Br was prepared according to step (1) of example 1.
Comparative example 2
4.7538G of NiCl 2·6H2 O and 2.00g of NaOH were weighed out and dissolved in 30ml of ultrapure water, respectively, to obtain clear solutions. The NiCl 2 solution was added dropwise to the NaOH solution, and the precipitate was separated by centrifugation after magnetically stirring for 1.0 h. The precipitate was washed by centrifugation 3 times with a mixture of ultrapure water and ethanol, and then dried in an oven at 60 o C for 12 hours. Finally, the powder is roasted for 2 hours at 500 o ℃ to obtain the target product NiO.
Referring to fig. 1-4, it can be seen from the XRD patterns of the products of fig. 2 that due to the low NiO content, only the PbBiO 2 Br diffraction peak was observed in the XRD pattern, but both NiO and PbBiO 2 Br were already present in the product of example 3 as demonstrated in the Raman pattern of fig. 1. In combination with the TEM image of the product of example 3 shown in FIG. 3, it can be seen that nano NiO powder (which is shown as a distinct floc from the layered nanoplatelets in the TEM image) was deposited on the surface of the layered PbBiO 2 Br nanoplatelets (the nanoplatelets have a thickness of about 0.293 nm), which was also confirmed by XPS analysis. The XPS spectra of the product prepared in example 3 and the products prepared in comparative examples 1-2 are shown in FIG. 4, which shows that both NiO and PbBiO 2 Br are already present in the product of example 3. The test results prove that the invention successfully prepares the NiO modified PbBiO 2 Br composite catalyst; by further analyzing the energy band structures of NiO and PbBiO 2 Br in detail, and combining experimental results, it is confirmed that an S-type heterojunction structure is formed between NiO and PbBiO 2 Br.
To verify the catalytic activity of the products prepared in the examples of the present invention, the following experiments were designed.
Experiment 1: piezoelectric catalytic degradation RhB experiment
The experimental method comprises the following steps: preparing rhodamine B (RhB) aqueous solution with the concentration of 10mg/L in a beaker; the catalysts of examples 1-4 and comparative examples 1-2 were weighed 0.10g each, put into 50ml of rhodamine B aqueous solution, magnetically stirred for 60min, and then put into a 120W ultrasonic cleaner to conduct piezoelectricity catalytic degradation experiment. The total duration of the piezoelectricity catalytic degradation activity test is 1.5 hours, 3mL of reaction solution is sucked every 15min, and the absorbance at 554nm is measured by an ultraviolet-visible spectrophotometer after centrifugation.
The experimental results are shown in FIG. 5. C represents the residual rhodamine B concentration, C0 represents the initial concentration of rhodamine B, and smaller C/C0 represents higher degradation rate of rhodamine B. From the graph, after degradation for 1.5 hours, the degradation rate sequence of each catalyst for degrading rhodamine B is as follows: example 3 > example 2 > example 4 > example 1 > comparative example 2. This shows that the catalysts provided in examples 1-4 all had higher piezocatalytic activity than those provided in comparative examples 1-2, wherein the residual amount of RhB (C/C 0) was the lowest in the catalyst group of example 3, i.e., the piezocatalytic activity of the target product was related to the treatment time of the NiO photo-deposition on PbBiO 2 Br surface, and the product with the optimal catalytic activity was obtained at 2h of photo-deposition.
With further reference to fig. 6, it can be observed that the degradation process of RhB corresponds to the first order reaction kinetics. Of these, example 3 had the best piezoelectric catalytic activity, and the degradation rate constant for RhB reached 3.11.h -1, which was 12.4 times the catalytic rate constant for PbBiO 2 Br in comparative example 1 and 31.1 times the catalytic rate constant for NiO in comparative example 2. The catalyst prepared in example 3 was subjected to a cyclic test for piezocatalytically degrading RhB, the test results are shown in FIG. 7: after five cycles (2.5 h each), the catalytic activity of the catalyst remained essentially unchanged, indicating that the catalyst material had very high stability.
Experiment 2: photocatalytic degradation of Luo Mingdan RhB in Water
The experimental method comprises the following steps: rhodamine B (RhB) solution with the concentration of 10mg/L is prepared. 0.10g of the catalyst prepared in example 3 was weighed, added to 50mL of rhodamine B solution to be degraded, magnetically stirred for 60min, and placed in a beaker under a 350W xenon lamp for photocatalytic degradation of RhB. The total duration of the photocatalytic degradation activity test is 1.5 hours, 3mL of the reaction solution is sucked every 15min, and after centrifugation, the absorbance at 554nm is measured by an ultraviolet-visible spectrophotometer.
Experiment 3: photo-piezoelectricity catalytic degradation Luo Mingdan RhB in water
The experimental method comprises the following steps: rhodamine B (RhB) solution with the concentration of 10mg/L is prepared. 0.10g of the catalyst prepared in example 3 is weighed, added into 50mL of rhodamine B solution to be degraded, magnetically stirred for 60min, and the beaker is simultaneously placed in a 120W ultrasonic cleaner and under 350W xenon lamp illumination to perform a photo-piezoelectric catalytic degradation RhB experiment. The total duration of the photo-piezoelectricity catalytic degradation activity test is 1.5 hours, 3mL of reaction solution is absorbed every 15min, and after centrifugation, the absorbance at 554nm is measured by an ultraviolet-visible spectrophotometer.
The results of the above experiments 2-3 are shown in FIG. 8. From the figure, the catalyst provided in example 3 also shows excellent photocatalytic activity, and the photocatalytic degradation rate reaches 3.5h -1. If the example 3 is placed under the environment of illumination and ultrasonic vibration, higher catalytic efficiency can be obtained, and the degradation rate constant reaches 4.2.h -1 which are 1.2 times and 1.35 times of the degradation rate constant of photocatalysis and piezocatalysis respectively; this is mainly due to the synergistic effect of light and ultrasound induced catalysis, which cannot be produced by directly mixing NiO with PbBiO 2 Br.
The piezoelectric response currents of the catalyst products of example 3 and comparative examples 1-2 were further tested, and the test results are shown in the response photocurrent spectra shown in fig. 9, and it can be seen from the graph that the catalyst provided in example 3 has higher response photocurrent, which indicates that the recombination of NiO and PbBiO 2 Br makes the catalyst have higher carrier separation capability, so that the life of photo-generated electrons is prolonged, more electrons are promoted to participate in photocatalytic and piezocatalytic reactions, and finally the NiO/PbBiO 2 Br catalyst shows excellent photocatalytic and piezocatalytic activities. And the complementary effect between photocatalysis and piezocatalysis makes NiO/PbBiO 2 Br show more excellent activity under illumination and ultrasonic vibration.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; 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 or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (9)
1. The application of the S-type heterojunction compound of nickel oxide composite PbBiO 2 Br as a photoelectric-piezoelectric synergistic catalyst is characterized in that the preparation method of the S-type heterojunction compound of nickel oxide composite PbBiO 2 Br is as follows:
S1, preparing PbBiO 2 Br
Dispersing soluble divalent lead salt, soluble trivalent bismuth salt and soluble bromine salt in a mixed solvent of deionized water and ethylene glycol according to a molar ratio of 1-1.05:1-1.05:1-1.05, and stirring until the mixture is uniformly dispersed, wherein the volume ratio of deionized water to ethylene glycol in the mixed solvent is 15-22:1; slowly dripping the obtained solution into excessive sodium hydroxide or potassium hydroxide solution under stirring, regulating the pH of a reaction system to 12.5-13.5 by using nitric acid, transferring into a high-pressure reaction kettle, carrying out hydrothermal reaction at 135-145 ℃ for 10-16h, cooling to room temperature after the reaction is finished, separating a precipitate, washing the precipitate by using a deionized water and ethanol mixed solution, and drying to obtain PbBiO 2 Br;
s2, preparing NiO/PbBiO 2 Br heterojunction catalyst
Dispersing soluble divalent nickel salt in a mixed solvent of water and methanol, adding PbBiO 2 Br prepared in the step S1 into the mixed solvent, and performing ultrasonic treatment to form uniform dispersion suspension; and (3) placing the dispersion suspension under a 300-400W xenon lamp for illumination for 1-4 hours, centrifuging after illumination is finished, collecting precipitate, washing the precipitate by using a deionized water and ethanol mixed solution, and drying to obtain the NiO/PbBiO 2 Br heterojunction catalyst.
2. Use according to claim 1, characterized in that in S2 the molar ratio PbBiO 2 Br to nickel salt is 1-1.1:1.
3. The use according to claim 1, wherein in S2, the soluble divalent nickel salt is nickel acetate or a hydrate thereof, which is dispersed in a mixed solvent of water and methanol to obtain a dispersion having a concentration of 0.02 to 0.04mol/L, and then PbBiO 2 Br is added; the volume ratio of water to methanol in the water mixed solvent is 25-35:10.
4. Use according to claim 1, characterized in that in S2 the power of the sonication is 120W sonicator for 30min to form a uniform dispersion.
5. Use according to claim 1, characterized in that in S2 the dispersion is subjected to a 350W xenon lamp for 2 hours.
6. Use according to claim 1, characterized in that in S1 the soluble divalent lead salt is lead acetate or a hydrate thereof, the soluble trivalent bismuth salt is bismuth nitrate or a hydrate thereof, and the soluble bromine salt is sodium bromide.
7. The use according to claim 1, wherein in S1, the dispersion concentration of the soluble divalent lead salt, the soluble trivalent bismuth salt and the soluble bromine salt in the mixed solvent of deionized water and ethylene glycol is 0.07 to 0.1mol/L, respectively; the molar amount of the solute in the sodium hydroxide or potassium hydroxide solution is more than 20 times of the sum of the molar amounts of lead ions and bismuth ions.
8. The method according to claim 1, wherein in S1, after the solution is added dropwise to sodium hydroxide or potassium hydroxide solution, the pH of the reaction system is adjusted to 13 by nitric acid, the reaction system is transferred into a high-pressure reaction kettle and subjected to hydrothermal reaction at 140 ℃ for 12 hours, after the reaction is finished, the reaction system is cooled to room temperature, the precipitate is separated, and the precipitate is washed for 3 times by using a mixed solution of deionized water and ethanol, and then PbBiO 2 Br is obtained after drying.
9. The use according to claim 1, wherein the S-type heterojunction composite of nickel oxide composite PbBiO 2 Br prepared in step S2 is put into water, ultrasonic vibration and light irradiation are applied to the water, and simultaneously organic matters in the water are degraded by means of piezocatalysis and photoelectrocatalysis.
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