CN107930615B - Method for preparing heterojunction composite photocatalyst - Google Patents
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910002905 Bi4V2O11 Inorganic materials 0.000 claims abstract description 23
- 238000004729 solvothermal method Methods 0.000 claims abstract description 8
- 230000000593 degrading effect Effects 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 4
- 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 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 239000003242 anti bacterial agent Substances 0.000 claims description 2
- 229940088710 antibiotic agent Drugs 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000004005 microsphere Substances 0.000 claims description 2
- 239000004098 Tetracycline Substances 0.000 abstract description 14
- 229960002180 tetracycline Drugs 0.000 abstract description 14
- 229930101283 tetracycline Natural products 0.000 abstract description 14
- 235000019364 tetracycline Nutrition 0.000 abstract description 14
- 150000003522 tetracyclines Chemical class 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- OFVLGDICTFRJMM-WESIUVDSSA-N tetracycline Chemical compound C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O OFVLGDICTFRJMM-WESIUVDSSA-N 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 229910052723 transition metal Inorganic materials 0.000 abstract description 3
- -1 transition metal vanadate Chemical class 0.000 abstract description 3
- 230000003115 biocidal effect Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 9
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 229910052797 bismuth Inorganic materials 0.000 description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 230000006798 recombination Effects 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012286 potassium permanganate Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Images
Classifications
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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
- B01J23/16—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—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention relates to transition metal vanadate, in particular to a method for preparing Bi4V2O11A method for preparing an RGO heterojunction composite photocatalyst. The invention synthesizes Bi at low temperature by solvothermal method4V2O11/RGO heterojunction photocatalyst, and RGO and Bi with different proportions4V2O11The catalytic activity and stability of the prepared photocatalyst are examined by degrading Tetracycline (TC) through photocatalysis, which is a common antibiotic.
Description
Technical Field
The invention relates to transition metal vanadate, in particular to a method for synthesizing Bi by taking ammonium metavanadate, pentahydrate bismuth nitrate, urea, ammonia water, concentrated sulfuric acid, graphite powder, potassium permanganate, hydrogen peroxide, hydrochloric acid and deionized water as raw materials4V2O11A method for preparing an RGO heterojunction composite photocatalyst. The preparation method is characterized by simple preparation process and good visible light catalytic performance of the product.
Technical Field
Recently, bismuth vanadate (Bi)4V2O11) Due to its excellent chemical and thermal stability, it has become a hot spot for research in the field of photocatalysis. Bismuth vanadate, a visible light responsive semiconductor material, has been widely used for photocatalytic degradation of organic pollutants and photodecomposition of water. At present, most of methods for preparing bismuth vanadate are solid-phase synthesis methods, namely products (monoclinic, orthorhombic and tetragonal) with different crystal phases can be obtained by high-temperature calcination. However, the solid phase method has high energy consumption, and the bismuth vanadate obtained by the method has large size and poor dispersibility, so that the practical application of the bismuth vanadate in production and life is limited. In addition, Bi4V2O11The electron holes are easy to recombine, the light stability is poor, and the effect of degrading organic pollutants is poor. Therefore, it is a practical work to improve the photocatalyst performance by increasing the electron-hole separation rate (inhibiting electron-hole recombination) of bismuth vanadate. The construction of a heterojunction is one of the important means to improve the efficiency of electron and hole separation. Due to the special energy band structure and carrier transmission characteristic of the heterojunction, the recombination of electrons and holes can be effectively inhibited in the photocatalytic reaction, and the photocatalyst is improvedThe catalytic performance of (2). Reduced Graphene Oxide (RGO) is of great interest due to its excellent electrical conductivity, thermal and chemical stability. Currently, Reduced Graphene Oxide (RGO) can be obtained by reducing Graphene Oxide (GO) by a solvothermal method. Therefore, the introduction of RGO by solvothermal method can effectively improve Bi4V2O11Electron hole recombination. In addition, there is no disclosure of Bi4V2O11And the construction of RGO heterojunction and the research report of applying the RGO heterojunction to photocatalytic degradation of antibiotics.
The invention synthesizes Bi at low temperature by solvothermal method4V2O11/RGO heterojunction photocatalyst, and RGO and Bi with different proportions4V2O11The catalytic activity and stability of the prepared photocatalyst are examined by degrading Tetracycline (TC) through photocatalysis, which is a common antibiotic.
Disclosure of Invention
The invention aims to provide a transition metal vanadate-based high-efficiency photocatalyst prepared by a two-step method, and a method for realizing photocatalytic degradation of tetracycline heterojunction composite photocatalyst under visible light.
The invention is realized by the following steps:
(1) preparation of GO: weighing 1g of graphite powder, placing the graphite powder in a beaker, weighing a proper amount of concentrated sulfuric acid, slowly adding the concentrated sulfuric acid into the beaker, and stirring in an ice bath (not higher than 5 ℃); slowly adding potassium permanganate in several times, controlling the reaction temperature to be not more than 20 ℃, and continuously stirring for 1 h; removing the ice bath, gradually increasing the temperature to about 35 ℃, and stirring for 2 h; after the color is changed into brown, slowly adding 300ml of deionized water, stirring for 30min, and then slowly adding hydrogen peroxide to ensure that the solution is changed into bright yellow; and (3) cooling the solution to room temperature, washing with a large amount of dilute hydrochloric acid solution and deionized water, and finally drying in an oven to obtain Graphene Oxide (GO).
(2) Weighing GO, adding the GO into an ethylene glycol solution, and performing ultrasonic dispersion; uniformly stirring, adding bismuth nitrate pentahydrate, performing ultrasonic dispersion, adding ammonium metavanadate and urea, and adjusting the pH value of the suspension to 7.5 by using a dilute ammonia solution; the suspension is filled in a reaction kettle and placed inCarrying out solvothermal reaction in an oven at 180 ℃ for 24 hours; washing and drying the obtained precipitate to obtain a sample Bi4V2O11an/RGO photocatalyst.
The concentration of the dilute ammonia solution is 14 wt%.
The Bi4V2O11In the/RGO photocatalyst, wherein RGO and Bi4V2O11The mass ratio of (A) to (B) is 0.01-0.08: 1.0.
further, RGO and Bi4V2O11Is 0.04: 1.0.
(3) the invention adopts solvothermal method to synthesize Bi at low temperature4V2O11the/RGO heterojunction composite photocatalyst has low energy consumption; the obtained sample has regular appearance and better dispersibility.
(4) Bi prepared by the invention4V2O11the/RGO heterojunction composite photocatalyst effectively inhibits the recombination of photo-generated electron holes and improves the photocatalytic activity.
(5) Performing structural analysis on the product by means of X-ray diffraction (XRD), Raman (Raman), electron microscope Scanning (SEM) and the like; performing a photocatalytic degradation experiment by taking tetracycline as a target pollutant, and measuring absorbance by an ultraviolet-visible spectrophotometer to evaluate the photocatalytic activity of the tetracycline; and the stability of the photocatalyst is explored through a cycle experiment.
Drawings
FIG. 1 shows Bi thus prepared4V2O11And Bi4V2O11XRD diffractogram of/RGO-4% (BR 4%) and Bi4V2O11GO and Bi4V2O11Raman spectrum of/RGO complex product.
FIG. 2 shows Bi thus prepared4V2O11Scanning electron micrograph (a) of (a) and scanning electron micrograph (b) of BR 4% of the heterojunction composite photocatalyst.
FIG. 3 shows Bi4V2O11And (3) a degradation curve of the/RGO heterojunction composite photocatalyst to TC in visible light for 60 min.
FIG. 4 is a cycle experiment of a BR 4% heterojunction composite photocatalyst on TC degradation activity test within 60min of illumination.
Detailed Description
Example 1Bi4V2O11Preparation of/RGO heterojunction composite photocatalyst (taking BR 4% as an example)
(1) Preparation of GO: GO is prepared by an improved Hummers method, 1g of graphite powder is weighed and placed in a beaker, 60ml of concentrated sulfuric acid is weighed and slowly added into the beaker, and the mixture is stirred in an ice bath (not higher than 5 ℃); then slowly adding 3g of potassium permanganate, controlling the reaction temperature not to exceed 20 ℃, and continuously stirring for 1 h; removing the ice bath, gradually increasing the temperature to about 35 ℃, and stirring for 2 h; after the color is changed into brown, slowly adding 300ml of deionized water, stirring for 30min, and then slowly adding hydrogen peroxide to ensure that the solution is changed into bright yellow; and (3) cooling the solution to room temperature, washing the solution by using a large amount of dilute hydrochloric acid solution (concentrated hydrochloric acid: water volume ratio is 1:10) and deionized water, and finally drying the solution in a 60 ℃ oven to obtain Graphene Oxide (GO).
(2)Bi4V2O11Preparation of/RGO: weighing 30mg of GO, adding the GO into 30ml of ethylene glycol solution, and performing ultrasonic dispersion; after the solution is stirred uniformly, 0.67mm of bismuth nitrate pentahydrate is weighed and added into the solution, after ultrasonic dispersion, 0.67mm of ammonium metavanadate and 0.5g of urea are added, and stirring is carried out for 30 min; then, the pH value of the solution is adjusted to 7.5 by using dilute ammonia solution with the concentration of 14 wt%; transferring the suspension into a 50ml reaction kettle, and placing the reaction kettle in an oven at 180 ℃ for solvothermal reaction for 24 hours; after cooling to room temperature, the precipitate was collected, washed twice each with deionized water and absolute ethanol, and dried in an oven at 60 ℃ for 12h to give the final product.
Example 2Bi4V2O11Characterization analysis of/RGO heterojunction composite photocatalyst
After RGO introduction, Bi is added as shown in FIG. 14V2O11The XRD characteristic peak of (A) is weakened and Bi in a Raman spectrogram is combined4V2O11the/RGO has both GO and Bi4V2O11Characteristic peak characteristics of (1). This result demonstrates that we successfully produced Bi4V2O11the/RGO heterojunction composite photocatalyst.
As shown in FIG. 2, (a) shows pure Bi4V2O11Microspheres, (b) RGO coating pure Bi can be seen4V2O11Of (2) is provided.
As shown in FIG. 3, Bi of different ratios can be seen4V2O11The basic condition that the/RGO heterojunction composite photocatalyst degrades tetracycline within 60min under visible light.
As shown in FIG. 4, the stability experiment of BR-4% photocatalyst for tetracycline degradation can be seen.
Example 3Bi4V2O11Visible light catalytic activity experiment of/RGO heterojunction composite photocatalyst
(1) Tetracycline with the concentration of 10mg/L is prepared, and the prepared solution is placed in a dark place.
(2) Weighing 50mg Bi4V2O11Placing the/RGO heterojunction composite photocatalyst into a photocatalytic reactor, adding 100mL of the target degradation liquid prepared in the step (1), magnetically stirring for 40min under a dark condition until the composite photocatalyst is uniformly dispersed, opening a water source and a light source, and performing a photocatalytic degradation experiment.
(3) And absorbing the photocatalytic degradation liquid in the reactor every 10min, and absorbing the supernatant liquid for measuring the absorbance after centrifugation.
(4) As can be seen from FIG. 3, the photocatalyst prepared has excellent visible light catalytic activity, especially RGO and Bi4V2O11Sample with a molar ratio of 0.04:1.0 showed the best tetracycline degrading activity than pure Bi4V2O11Much higher.
Example 4Bi4V2O11Visible light catalytic stability experiment of/RGO heterojunction composite photocatalyst
(1) Tetracycline with the concentration of 10mg/L is prepared, and the prepared solution is placed in a dark place.
(2) Weighing 50mg of BR 4% heterojunction composite photocatalyst, placing the photocatalyst into a photocatalytic reactor, adding 100mL of the target degradation liquid prepared in the step (1), magnetically stirring the photocatalyst for 40min in the dark condition, opening a water source and a light source after the composite photocatalyst is uniformly dispersed, and carrying out a photocatalytic degradation experiment.
(3) And absorbing the photocatalytic degradation liquid in the reactor every 10min, and absorbing the supernatant liquid for measuring the absorbance after centrifugation. And (4) recovering the centrifugal precipitate, centrifuging, washing, and drying in a 60 ℃ oven for the next circulation experiment.
(4) As can be seen from fig. 4, the prepared photocatalyst has excellent visible light photocatalytic stability.
Claims (3)
1. Method for preparing heterojunction composite photocatalyst, wherein the heterojunction composite photocatalyst is Bi4V2O11the/RGO heterojunction composite photocatalyst is characterized by comprising the following specific steps: weighing GO, adding the GO into an ethylene glycol solution, and performing ultrasonic dispersion; uniformly stirring, adding bismuth nitrate pentahydrate, performing ultrasonic dispersion, adding ammonium metavanadate and urea, and adjusting the pH value of the suspension to 7.5 by using a dilute ammonia solution; putting the suspension into a reaction kettle, and putting the reaction kettle into an oven at 180 ℃ for solvothermal reaction for 24 hours; washing and drying the obtained precipitate to obtain a sample Bi4V2O11An RGO heterojunction composite photocatalyst; RGO and Bi4V2O11Is 0.04:1.0 RGO coating pure Bi4V2O11The surface of the microspheres.
2. The method for preparing the heterojunction composite photocatalyst of claim 1, wherein the concentration of the dilute ammonia solution is 14 wt%.
3. Use of the heterojunction composite photocatalyst prepared by the method as claimed in any one of claims 1 to 2, for catalytically degrading antibiotics under visible light.
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| CN102698735A (en) * | 2012-05-18 | 2012-10-03 | 北京工业大学 | Method of preparing flower-ball shaped Bi4V2O11 visible-light catalyst |
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| CN102698735A (en) * | 2012-05-18 | 2012-10-03 | 北京工业大学 | Method of preparing flower-ball shaped Bi4V2O11 visible-light catalyst |
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| Title |
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| Preparation and characterization of sphere-shaped BiVO4/reduced grapheme oxide photocatalyst for an augemented natural sunlight photocatalytic activity;Chongfei Yu et al.,;《Journal of Alloys and Compounds》;20160331;第677卷;219-227 * |
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