CN112007633A - La/Bi2WO6Preparation method and application of photocatalyst - Google Patents
La/Bi2WO6Preparation method and application of photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 95
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 238000002360 preparation method Methods 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002244 precipitate Substances 0.000 claims abstract description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000007935 neutral effect Effects 0.000 claims abstract description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 11
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 229960000583 acetic acid Drugs 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 8
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 34
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 16
- 229910001220 stainless steel Inorganic materials 0.000 claims description 16
- 239000010935 stainless steel Substances 0.000 claims description 16
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000002351 wastewater Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 229910001868 water Inorganic materials 0.000 abstract description 9
- 238000001354 calcination Methods 0.000 abstract description 8
- 238000005303 weighing Methods 0.000 abstract description 7
- 239000000047 product Substances 0.000 abstract description 6
- 229910052797 bismuth Inorganic materials 0.000 abstract description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 4
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 abstract description 4
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 abstract 1
- 229910052746 lanthanum Inorganic materials 0.000 description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 230000015556 catabolic process Effects 0.000 description 14
- 238000006731 degradation reaction Methods 0.000 description 14
- 238000001179 sorption measurement Methods 0.000 description 13
- 238000002835 absorbance Methods 0.000 description 7
- 229910020350 Na2WO4 Inorganic materials 0.000 description 6
- 238000003795 desorption Methods 0.000 description 6
- 230000001678 irradiating effect Effects 0.000 description 6
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 6
- 229910052753 mercury Inorganic materials 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005188 flotation Methods 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 241001198704 Aurivillius Species 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 239000002879 Lewis base Substances 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 239000000370 acceptor Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910021644 lanthanide ion Inorganic materials 0.000 description 1
- 150000007527 lewis bases Chemical class 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- 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
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
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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
- 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
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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
- 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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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- 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
- C02F2101/40—Organic compounds containing sulfur
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
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- 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
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Abstract
The invention discloses La/Bi2WO6A preparation method and application of a photocatalyst, belongs to the field of catalysts, and solves the problem of La/Bi prepared by the existing method2WO6The photocatalyst has poor photocatalytic performance. The method comprises the following steps: weighing lanthanum nitrate, adding absolute ethyl alcohol, glacial acetic acid and deionized water, and fully stirring to prepare a uniform and transparent solution A; dissolving bismuth nitrate in HNO3In the water solution, named as B solution; will sixteenDissolving alkyl trimethyl ammonium bromide and sodium tungstate in deionized water, and naming as solution C; dropwise adding the solution A and the solution B into the solution C under magnetic stirring, adjusting the pH to be neutral by using concentrated ammonia water, and violently stirring to obtain a white precipitate; and reacting the mixed solution containing the precipitate at the temperature of 120-160 ℃ for 6-16h, drying, and calcining the sample in a muffle furnace to obtain the target product. The method enhances the photocatalytic performance of bismuth tungstate, has high product purity, and can efficiently degrade ester-105.
Description
Technical Field
The invention belongs to the field of catalysts, and particularly relates to La/Bi2WO6Preparation method and application of photocatalyst
Background
Photocatalytic oxidation has been widely studied and shows great potential application value in organic wastewater treatment, but few studies have been made in the treatment of flotation reagents. Along with the development of the mining industry in China, mine beneficiation wastewater becomes a main source of pollution to mines and the surrounding environment, and particularly, organic flotation reagents remained in the beneficiation wastewater have high toxicity, large environmental pollution and energy shortage and are important practical problems restricting the development of the human society. In recent years, semiconductor photocatalytic oxidation technology has attracted much attention to the degradation of organic pollutants in water and air.
Bi2WO6As an Aurivillius type oxide, the energy gap is 2.7eV, which is in comparison with TiO2The forbidden band width of 3.2eV is narrower than that of TiO2A novel photocatalytic material with strong visible light response capability. However, Bi2WO6The conduction band low potential (ECB) of the photocatalyst causes the reaction of photo-generated electrons and electron acceptors to be ineffective, and increases the recombination of photo-generated carriers, thereby reducing the photocatalytic activity.
Doping elements are introduced into catalyst crystal lattices to form surface defects, a new impurity level is formed to regulate forbidden bandwidth, and photon-generated carrier recombination can be inhibited. The lanthanide ion 4f orbital is easy to combine with various Lewis bases (such as alcohol, aldehyde, amine and the like), and is widely used as a doping modifier of semiconductor photocatalytic materials. Xu et al study of Gd, Eu, Sm or La doped Bi2WO6Degrading RhB performance under visible light photocatalysis, La doping Bi2WO6The sample has the best dark adsorption capacity and higher photocatalytic performance.
The existing preparation of La/Bi2WO6The method of the photocatalyst uses lanthanum chloride as a lanthanum source, and has the defect of high cost. La/Bi obtained by using the method2WO6The optimal doping amount of the photocatalyst La is 5%, and the photocatalytic performance of the photocatalyst La is still to be further improved. Secondly, the existing preparation methods require high pressuresThe reaction is carried out under the condition, the requirement on the reaction is high, and high-pressure conditions are required.
Disclosure of Invention
The object of the present invention is to provide La/Bi2WO6A preparation method of a photocatalyst, aiming at solving the problem of La/Bi prepared by the existing method2WO6The photocatalyst has poor photocatalytic performance and high preparation cost.
Another object of the present invention is to provide La/Bi2WO6The application of the photocatalyst is used for solving the problem of residual pesticide ester-105 in the beneficiation wastewater.
The technical scheme of the invention is as follows: La/Bi2WO6The preparation method of the photocatalyst comprises the following steps:
step one, weighing lanthanum nitrate (La (NO)3)3·6H2O), adding absolute ethyl alcohol, glacial acetic acid and deionized water, and fully stirring to prepare a uniform and transparent solution A;
step two, bismuth nitrate (Bi (NO)3)3·5H2O) dissolved in HNO3In an aqueous solution, the solution is named as B solution;
step three, Cetyl Trimethyl Ammonium Bromide (CTAB) and sodium tungstate (Na)2WO4·2H2O) is dissolved in deionized water, and the solution is named as solution C;
step four, dropwise adding the solution A and the solution B into the solution C under magnetic stirring to obtain a precursor solution, and adding strong ammonia water (NH)3·H2O) adjusting the pH value of the precursor solution to be neutral, and violently stirring for 0.5-3h to obtain white precipitate;
step five, transferring the mixed solution containing the precipitate obtained in the step four into a stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the stainless steel reaction kettle into an oven, reacting for 6-16h at the temperature of 120-160 ℃, alternately washing for a plurality of times by deionized water and absolute ethyl alcohol after the reaction is finished and cooled to room temperature, drying for 5-10h at the temperature of 40-50 ℃, and then calcining the sample in a muffle furnace at the temperature of 300-800 ℃ for 3-10h to remove surface residues to obtain La/Bi2WO6A photocatalyst.
As a further improvement of the present invention, the processFormed La/Bi2WO6In the photocatalyst, La accounts for 1.0-5.0% of the total mass of the catalyst
Preferably, La comprises 2.0% of the total mass of the catalyst.
As a further improvement of the invention, in step two, HNO3The mass concentration of the aqueous solution is 2-4 mol/L.
As a further improvement of the invention, in the fourth step, the volume fraction of the concentrated ammonia water is 50%.
As a further improvement of the invention, the ratio of the amount of Bi element substance in the second step to the amount of W element substance in the third step is 2: 1.
As a further improvement of the invention, in the third step, the addition amount of the hexadecyl trimethyl ammonium bromide is 2.4 to 2.5 percent of the mass of the sodium tungstate.
La/Bi2WO6The application of the photocatalyst in reducing ester-105 in beneficiation wastewater.
The invention has the beneficial effects that:
1. the preparation method adopts a hydrothermal synthesis method, the method is simple and easy to operate, the energy consumption of room-temperature synthesis is low, the used reagents and equipment are few, the reaction condition is mild, the target product can be generated without high layering, the synthesis time is short, and the method is suitable for expanded production;
2. the preparation method uses lanthanum nitrate as a lanthanum source, is cheap and easy to obtain, has the price of one fourth of lanthanum chloride, and greatly reduces the cost;
3. according to the preparation method, a Cetyl Trimethyl Ammonium Bromide (CTAB) surfactant is added, so that the bismuth tungstate is easier to form layering in synthesis, and the compact nano flower-shaped structure enhances the photocatalytic performance of the bismuth tungstate;
4. according to the preparation method disclosed by the invention, the dried product is subjected to high-temperature calcination in the muffle furnace, residues (such as unreacted bismuth nitrate, CTAB and other solvents which are not completely reacted or excessive) on the surface of a sample can be removed, the product purity is improved, and the degradation rate of the product to ester-105 is improved by 5% under the condition of the same dosage;
5.La/Bi2WO6the photocatalyst is quickly realized under the irradiation of visible lightThe separation of photogenerated electrons and holes is realized, the ester-105 can be efficiently degraded, and the degradation rate is higher than 90% in 30min under the irradiation of visible light.
Drawings
FIG. 1 shows La/Bi of the present invention2WO6A flow chart of a preparation process of the photocatalyst;
FIG. 2 shows La/Bi contents of La doping amounts different from those of examples 1 to 5 and comparative example 12WO6The degradation effect of the ester-105 solution is shown.
Detailed Description
The flow chart of the preparation process of the invention is shown in figure 1. The present invention will be described in detail with reference to specific embodiments. The following examples respectively prepare La/Bi with La doping amounts of wt 1.0%, wt 1.5%, wt 2.0%, wt 3.0%, wt 5.0%2WO6Respectively named as wt 1.0% La/Bi2WO6、wt1.5％La/Bi2WO6、wt2.0％La/Bi2WO6、wt3.0％La/Bi2WO6、wt5.0％La/Bi2WO6。
Examples 1,
wt1.0％La/Bi2WO6The preparation of (1):
step one, weighing 0.035g La (NO)3)3·6H2Adding 10mL of absolute ethyl alcohol, 2mL of glacial acetic acid and 2mL of deionized water into O (the La accounts for 1.0 wt%), and fully stirring to prepare a uniform and transparent solution A;
step two, 2.43g of Bi (NO)3)3·5H2O is dissolved in 10mL of 4mol/L HNO3In an aqueous solution, the solution is named as B solution;
step three, 0.02g of hexadecyl trimethyl ammonium bromide (CTAB) and 0.83g of Na2WO4·2H2Dissolving O in 50mL of deionized water, and naming the solution as solution C;
step four, slowly dripping the solution A and the solution B into the solution C under magnetic stirring to obtain a precursor solution, and adding 50 percent by volume of concentrated ammonia water (NH)3·H2O) adjusting the pH of the precursor solution to be neutral, and violently stirring for 0.5h to obtain whitePrecipitating;
and step five, transferring the mixed solution containing the precipitate obtained in the step four into a stainless steel reaction kettle with a lining of 100mL of polytetrafluoroethylene, placing the stainless steel reaction kettle into an oven, reacting for 16h at 80 ℃, alternately washing for several times by deionized water and absolute ethyl alcohol after the reaction is finished and cooled to room temperature, drying for 10h at 40 ℃, and then calcining the sample in a muffle furnace for 10h at 300 ℃ to remove surface residues.
The application comprises the following steps: 0.2g of wt 1.0% La/Bi2WO6Dispersing the photocatalyst into 50mL of 50mg/L ester-105 solution, adjusting the pH value to be neutral by using HCl and NaOH aqueous solution, placing the reaction system in a photochemical reactor, stirring in the dark for adsorption, stirring in the dark for 30min to reach adsorption and desorption equilibrium, irradiating by using a 300W mercury lamp, starting timing, taking samples every 10min, and measuring the absorbance of the supernatant at the position of which the lambda is 276 nm.
The absorbance was converted into concentration according to Lambert-beer's law, and the change in the concentration of ester-105 before and after the light irradiation and the degradation rate thereof (see the following formula) were calculated to evaluate La/Bi2WO6Photocatalytic activity of (1).
In the formula: eta is the degradation rate of ester-105, C0Concentration of the pre-ester-105 solution to light, CtThe concentration of the ester-105 solution after illumination.
The degradation rate is 94.21 percent after illumination for 30 min.
Examples 2,
wt1.5％La/Bi2WO6The preparation of (1):
step one, weighing 0.053g of La (NO)3)3·6H2Adding 10mL of absolute ethyl alcohol, 2mL of glacial acetic acid and 2mL of deionized water into O (the La accounts for 1.5 wt%), and fully stirring to prepare a uniform and transparent solution A;
step two, 2.43g of Bi (NO)3)3·5H2O is dissolved in 10mL of 4mol/L HNO3In an aqueous solution, the solution is named as B solution;
step three, then 0.02g of cetyltrimethylammonium bromide (CTAB) and 0.83g of Na2WO4·2H2Dissolving O in 50mL of deionized water, and naming the solution as solution C;
step four, slowly dripping the solution A and the solution B into the solution C under magnetic stirring to obtain a precursor solution, and adding 50 percent by volume of concentrated ammonia water (NH)3·H2O) adjusting the pH value of the precursor solution to be neutral, and violently stirring for 1h to obtain white precipitate;
and step five, transferring the mixed solution containing the precipitate obtained in the step four into a stainless steel reaction kettle with a lining of 100mL of polytetrafluoroethylene, placing the stainless steel reaction kettle into an oven, reacting for 14h at 100 ℃, alternately washing the mixture for several times by deionized water and absolute ethyl alcohol after the reaction is finished and cooled to room temperature, drying the mixture for 7h at 45 ℃, and then calcining the sample in a muffle furnace for 8h at 400 ℃ to remove surface residues.
The application comprises the following steps: 0.2g of wt 1.5% La/Bi2WO6Dispersing the photocatalyst into 50mL of 50mg/L ester-105 solution, adjusting the pH value to be neutral by using HCl and NaOH aqueous solution, placing the reaction system in a photochemical reactor, stirring in the dark for adsorption, stirring in the dark for 30min to reach adsorption and desorption equilibrium, irradiating by using a 300W mercury lamp, starting timing, taking samples every 10min, and measuring the absorbance of the supernatant at the position of which the lambda is 276 nm. The light irradiation is carried out for 30min, and the degradation rate is 95.11 percent.
Examples 3,
wt2.0％La/Bi2WO6The preparation of (1):
step one, weighing 0.07g of La (NO)3)3·6H2Adding 10mL of absolute ethyl alcohol, 2mL of glacial acetic acid and 2mL of deionized water into O (according to the La being wt 2.0%), and fully stirring to prepare a uniform and transparent solution A;
step two, 2.43g of Bi (NO)3)3·5H2O is dissolved in 10mL of 4mol/L HNO3In an aqueous solution, the solution is named as B solution;
step three, then 0.02g of cetyltrimethylammonium bromide (CTAB) and 0.83g of Na2WO4·2H2Dissolving O in 50mL of deionized water, and naming the solution as solution C;
step four, slowly dripping the solution A and the solution B into the solution C under magnetic stirring to obtain a precursor solution, and adding 50 percent by volume of concentrated ammonia water (NH)3·H2O) adjusting the pH value of the precursor solution to be neutral, and violently stirring for 1.5h to obtain white precipitate;
and step five, transferring the mixed solution containing the precipitate obtained in the step four into a stainless steel reaction kettle with a lining of 100mL of polytetrafluoroethylene, placing the stainless steel reaction kettle into an oven, reacting for 8 hours at 120 ℃, alternately washing for several times by deionized water and absolute ethyl alcohol after the reaction is finished and cooled to room temperature, drying for 5 hours at 50 ℃, and then calcining the sample for 3 hours at 500 ℃ in a muffle furnace to remove surface residues.
The application comprises the following steps: 0.2g of wt 2.0% La/Bi2WO6Dispersing the photocatalyst into 50mL of 50mg/L ester-105 solution, adjusting the pH value to be neutral by using HCl and NaOH aqueous solution, placing the reaction system in a photochemical reactor, stirring in the dark for adsorption, stirring in the dark for 30min to reach adsorption and desorption equilibrium, irradiating by using a 300W mercury lamp, starting timing, taking samples every 10min, and measuring the absorbance of the supernatant at the position of which the lambda is 276 nm. The degradation rate is 97.33 percent after illumination for 30 min.
Examples 4,
wt3.0％La/Bi2WO6The preparation of (1):
step one, weighing 0.105g of La (NO)3)3·6H2Adding 10mL of absolute ethyl alcohol, 2mL of glacial acetic acid and 2mL of deionized water into O (according to the La weight ratio of 3.0 percent), and fully stirring to prepare a uniform and transparent solution A;
step two, 2.43g of Bi (NO)3)3·5H2O is dissolved in 10mL of 4mol/L HNO3In an aqueous solution, the solution is named as B solution;
step three, 0.02g of hexadecyl trimethyl ammonium bromide (CTAB) and 0.83g of Na2WO4·2H2Dissolving O in 50mL of deionized water, and naming the solution as solution C;
step four, slowly dripping the solution A and the solution B into the solution C under magnetic stirring to obtain a precursor solution, and adding 50 percent by volume of concentrated ammonia water (NH)3·H2O) adjusting the pH value of the precursor solution to be neutral, and violently stirring for 3 hours to obtain white precipitate;
and step five, transferring the mixed solution containing the precipitate obtained in the step four into a stainless steel reaction kettle with a lining of 100mL of polytetrafluoroethylene, placing the stainless steel reaction kettle into an oven, reacting for 6 hours at 140 ℃, alternately washing the mixture for several times by deionized water and absolute ethyl alcohol after the reaction is finished and cooled to room temperature, drying the mixture for 5 hours at 50 ℃, and then calcining the sample for 3 hours at 800 ℃ in a muffle furnace to remove surface residues.
The application comprises the following steps: 0.2g of wt 3.0% La/Bi2WO6Dispersing the photocatalyst into 50mL of 50mg/L ester-105 solution, adjusting the pH value to be neutral by using HCl and NaOH aqueous solution, placing the reaction system in a photochemical reactor, stirring in the dark for adsorption, stirring in the dark for 30min to reach adsorption and desorption equilibrium, irradiating by using a 300W mercury lamp, starting timing, taking samples every 10min, and measuring the absorbance of the supernatant at the position of which the lambda is 276 nm. The light irradiation is carried out for 30min, and the degradation rate is 96.14 percent.
Examples 5,
wt5.0％La/Bi2WO6The preparation of (1):
step one, weighing 0.175g of La (NO)3)3·6H2Adding 10mL of absolute ethyl alcohol, 2mL of glacial acetic acid and 2mL of deionized water into O (according to the La weight ratio of 5.0 percent), and fully stirring to prepare a uniform and transparent solution A;
step two, 2.43g of Bi (NO)3)3·5H2O is dissolved in 10mL of 4mol/L HNO3In an aqueous solution, the solution is named as B solution;
step three, then 0.02g of cetyltrimethylammonium bromide (CTAB) and 0.83g of Na2WO4·2H2Dissolving O in 50mL of deionized water, and naming the solution as solution C;
step four, slowly dripping the solution A and the solution B into the solution C under magnetic stirring to obtain a precursor solution, and adding 50 percent by volume of concentrated ammonia water (NH)3·H2O) adjusting the pH value of the precursor solution to be neutral, and violently stirring for 3 hours to obtain white precipitate;
and step five, transferring the mixed solution containing the precipitate obtained in the step four into a stainless steel reaction kettle with a lining of 100mL of polytetrafluoroethylene, placing the stainless steel reaction kettle into an oven, reacting for 4 hours at 160 ℃, alternately washing the mixture for several times by deionized water and absolute ethyl alcohol after the reaction is finished and cooled to room temperature, drying the mixture for 5 hours at 50 ℃, and then calcining the sample for 3 hours at 800 ℃ in a muffle furnace to remove surface residues.
The application comprises the following steps: 0.2g of wt 5.0% La/Bi2WO6Dispersing the photocatalyst into 50mL of 50mg/L ester-105 solution, adjusting the pH value to be neutral by using HCl and NaOH aqueous solution, placing the reaction system in a photochemical reactor, stirring in the dark for adsorption, stirring in the dark for 30min to reach adsorption and desorption equilibrium, irradiating by using a 300W mercury lamp, starting timing, taking samples every 10min, and measuring the absorbance of the supernatant at the position of which the lambda is 276 nm. The degradation rate is 94.87 percent after illumination for 30 min.
Comparative examples 1,
The doped amount of La in this comparative example was 0, which was named as wt 0.0% La/Bi2WO6。
wt0.0％La/Bi2WO6The preparation of (1):
step one, 2.43g of Bi (NO)3)3·5H2O is dissolved in 10mL of 4mol/L HNO3In an aqueous solution, the solution is named as A solution;
step two, then 0.02g of cetyltrimethylammonium bromide (CTAB) and 0.83g of Na2WO4·2H2Dissolving O in 50mL of deionized water, and naming the solution as B;
step three, slowly dripping the solution B into the solution A under magnetic stirring to obtain a precursor solution, and adding 50% by volume of concentrated ammonia water (NH)3·H2O) adjusting the pH value of the precursor solution to be neutral, and violently stirring for 1.5h to obtain white precipitate;
and step four, transferring the mixed solution containing the precipitate obtained in the step three to a stainless steel reaction kettle with a lining of 100mL of polytetrafluoroethylene, placing the stainless steel reaction kettle in an oven, reacting for 12 hours at 160 ℃, alternately washing for several times by deionized water and absolute ethyl alcohol after the reaction is finished and cooled to room temperature, drying for 7 hours at 80 ℃, and then calcining the sample in a muffle furnace for 3 hours at 500 ℃ to remove surface residues.
0 is added.2g of wt 0.0% La/Bi2WO6Dispersing the photocatalyst into 50mL of 50mg/L ester-105 solution, adjusting the pH value to be neutral by using HCl and NaOH aqueous solution, placing the reaction system in a photochemical reactor, stirring in the dark for adsorption, stirring in the dark for 30min to reach adsorption and desorption equilibrium, irradiating by using a 300W mercury lamp, starting timing, taking samples every 10min, and measuring the absorbance of the supernatant at the position of which the lambda is 276 nm. The light irradiation is carried out for 30min, and the degradation rate is 85.15 percent.
La/Bi of different La doping amounts in examples 1 to 5 and comparative example 12WO6The degradation effect on the ester-105 solution is shown in FIG. 2. As can be seen from FIG. 2, doping a certain proportion of La into the catalyst bismuth tungstate is beneficial to improving the photocatalytic performance, and experiments have investigated that the doping amount of La is La/Bi with the percentage of wt 1.0%, wt 1.5%, wt 2.0%, wt 3.0% and wt 5.0%2WO6The influence of the photocatalyst on the degradation rate of the ester-105 solution shows that the photocatalytic performance is best when the optimal doping amount of La is 2 wt%.
Claims (8)
1.La/Bi2WO6The preparation method of the photocatalyst is characterized by comprising the following steps:
step one, lanthanum nitrate is weighed, absolute ethyl alcohol, glacial acetic acid and deionized water are added, and the mixture is fully stirred to prepare a uniform and transparent solution A;
step two, dissolving bismuth nitrate in HNO3In an aqueous solution, the solution is named as B solution;
dissolving cetyl trimethyl ammonium bromide and sodium tungstate into deionized water, and naming the solution as solution C;
step four, dropwise adding the solution A and the solution B into the solution C under magnetic stirring to obtain a precursor solution, adjusting the pH of the precursor solution to be neutral by using strong ammonia water, and violently stirring for 0.5-3h to obtain a white precipitate;
transferring the mixed solution containing the precipitate obtained in the step four into a stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the stainless steel reaction kettle into a drying oven, reacting for 4-16h at 80-160 ℃, alternately washing for several times by using deionized water and absolute ethyl alcohol after the reaction is finished and the temperature is cooled to room temperature, drying for 5-10h at 40-50 ℃, and then dryingCalcining the sample in a muffle furnace at the temperature of 300-800 ℃ for 3-10h to remove surface residues to obtain La/Bi2WO6A photocatalyst.
2. La/Bi according to claim 12WO6The preparation method of the photocatalyst is characterized by comprising the following steps: the prepared La/Bi2WO6In the photocatalyst, La accounts for 1.0-5.0% of the total mass of the catalyst.
3. La/Bi according to claim 22WO6The preparation method of the photocatalyst is characterized by comprising the following steps: la accounted for 2.0% of the total mass of the catalyst.
4. La/Bi according to any one of claims 1 to 32WO6The preparation method of the photocatalyst is characterized by comprising the following steps: in step two, HNO3The mass concentration of the aqueous solution is 2-4 mol/L.
5. La/Bi according to claim 42WO6The preparation method of the photocatalyst is characterized by comprising the following steps: in the fourth step, the volume fraction of the concentrated ammonia water is 50%.
6. La/Bi according to claim 52WO6The preparation method of the photocatalyst is characterized by comprising the following steps: the ratio of the amount of Bi element substance in the second step to the amount of W element substance in the third step is 2: 1.
7. La/Bi according to claim 62WO6The preparation method of the photocatalyst is characterized by comprising the following steps: in the third step, the addition amount of the hexadecyl trimethyl ammonium bromide is 2.4 to 2.5 percent of the mass of the sodium tungstate.
8.La/Bi2WO6The application of the photocatalyst in reducing ester-105 in beneficiation wastewater.
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