CN114392767A - Method for preparing PDA/BWO and reducing hexavalent chromium by photocatalysis - Google Patents
Method for preparing PDA/BWO and reducing hexavalent chromium by photocatalysis Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 15
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 238000007146 photocatalysis Methods 0.000 title claims description 5
- 239000011651 chromium Substances 0.000 claims abstract description 50
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- 230000009467 reduction Effects 0.000 claims abstract description 14
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 13
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- 239000002244 precipitate Substances 0.000 claims description 9
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 7
- 239000011941 photocatalyst Substances 0.000 claims description 7
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- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 3
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 5
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
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- B01J31/063—Polymers comprising a characteristic microstructure
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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
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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- 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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- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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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
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Abstract
The invention discloses a method for preparing PDA/BWO and carrying out photocatalytic reduction on hexavalent chromium [ Cr (VI) ], which comprises the steps of firstly synthesizing a bismuth auto-doped bismuth tungstate material (BWO) by a hydrothermal method, and then forming a ligand-metal charge transfer complex (the dopamine content is between 1 and 5 percent) on the surface of the BWO by a normal-temperature stirring method, thereby forming the PDA/BWO composite material with a core-shell structure. The PDA/BWO composite material has a narrow band gap, high separation efficiency of electron-hole pairs, excellent reduction effect on Cr (VI) under the irradiation of visible light, reduction rate as high as 99.7 percent, and removal rate of total chromium of 72.3 percent.
Description
Technical Field
The invention belongs to the technical field of environmental and chemical engineering, relates to reduction of hexavalent chromium, and particularly relates to a method for reducing hexavalent chromium in a water body by photocatalysis.
Background
Chromium is a common and indispensable material in our daily life, and is widely applied to the fields of leather making, electroplating, spinning and the like. In nature, it exists mainly in two oxidation states, hexavalent chromium [ Cr (VI)]And trivalent chromium [ Cr (III)]. Cr (vi) is extremely toxic and carcinogenic even at very low concentrations, causing harm to human health, resulting in a variety of diseases such as liver damage, pulmonary congestion, fetal abnormalities, and cancer. Prolonged occupational exposure to Cr (VI) can lead to bronchial systemsCancer and respiratory tract cancer. According to the regulations of the World Health Organization (WHO), the maximum allowable concentration of Cr (VI) discharged to the inland river and the maximum allowable concentration of Cr (VI) in the drinking water are respectively 0.1mg L-1And 0.05mg L-1. Cr (III) is an important trace element necessary for human metabolism, and Cr (III) can form hydroxide with hydroxyl, so that insoluble Cr (OH) is easily generated in alkaline water3Precipitates, adsorbs on soil particles, and shows low mobility. Therefore, the method for reducing the highly toxic Cr (VI) into Cr (III) is a promising method for treating the wastewater containing Cr (VI).
Although the traditional technologies for removing Cr (VI), such as adsorption, membrane filtration, electrochemical precipitation, biological methods, etc., have been widely studied, most of these methods have the disadvantages of low efficiency, high energy consumption, secondary pollution, high cost, etc., which severely limits their application in the treatment of chromium-containing wastewater. Therefore, it is important to develop a green and efficient material to effectively remove cr (vi) in an aqueous environment. The photocatalysis technology is widely concerned as a wastewater treatment, atmosphere purification and solar energy development technology with wide prospect due to the advantages of no toxicity, safety, low cost, high efficiency and the like. It is based on the irradiation of high-energy photons on a semiconductor to generate electron-hole pairs, thereby inducing a photoredox reaction, wherein Cr (VI) can be reduced into Cr (III) under the action of electrons.
In a novel semiconductor photocatalyst, bismuth tungstate (Bi)2WO6) As one of the most popular bismuth-based compounds, Bi is used because of its unique crystal structure and band structure2WO6The photocatalyst has excellent pollutant photocatalytic degradation performance. However, since Bi2WO6High recombination rate of electron-hole pairs and low photocatalytic activity caused by easy agglomeration, and Bi is required2WO6And (4) carrying out modification. Various modification methods have been developed, including doping of metallic and non-metallic elements, morphology control, construction of heterojunctions, dye sensitization and Ligand-to-metal charge transfer (LMCT), among others. Wherein Polydopamine (PDA) and bismuth are self-doped with Bi by an LMCT method2WO6(noted BWO) surface-Forming Complex (PDA/BWO)Lowering the band gap of BWO and improving the electron-hole pair separation efficiency of BWO. However, no preparation method for forming a composite on the BWO surface by PDA and no technology and patent for photocatalytic reduction of Cr (VI) in water are available at present.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method and application of a photocatalyst for reducing Cr (VI) in water, and more particularly relates to a method for utilizing PDA (PDA) to load bismuth to dope Bi automatically2WO6The new material of (2) is used as a photocatalyst in a method for reducing Cr (VI) in water under the irradiation of visible light.
For the purpose of the invention, the hydrothermal method is adopted to synthesize the bismuth self-doped Bi2WO6(BWO), preparing the core-shell structure PDA/BWO composite material (the PDA content is between 1 and 5 percent) based on the LMCT method, and systematically researching the activity of Cr (VI) in the PDA/BWO visible light catalytic reduction water body.
The technical scheme adopted by the invention is carried out according to the following steps:
(a) separately weighing Bi (NO)3)3·5H2O and Na2WO4·2H2O (Bi/W molar ratio is controlled to be 2.05-2.20), which is dissolved in a certain amount of 1.2M HNO3And 1.2M NaOH solution;
(b) fully mixing the two solutions obtained in the step (a), magnetically stirring for 1-4h, then placing the mixture into a reaction kettle, and carrying out hydrothermal reaction for 9-24h at the temperature of 150-;
(c) after cooling, repeatedly cleaning the obtained precipitate with absolute ethyl alcohol and distilled water, and then drying for 4-10h to obtain a bismuth auto-doping bismuth tungstate material (recorded as BWO);
(d) preparing a Tris-HCl buffer solution with a certain concentration, and adjusting the pH value to 8.5;
(e) ultrasonically dispersing a certain amount of BWO into a Tris-HCl buffer solution;
(f) then adding a certain amount of dopamine, performing ultrasonic dispersion on the dopamine, and continuously performing magnetic stirring for 10-24 hours;
(g) centrifugally separating the PDA-loaded BWO catalyst formed in the step (f) from a liquid phase, and washing the separated liquid phase with water for 3 to 6 times to obtain a precipitate;
(h) drying the precipitate obtained in the step (g) for 4-10h, and then grinding the dried solid into powder to obtain a dried PDA/BWO catalyst;
(i) will contain Cr (VI) (10-30mg L)-1) Introducing the simulated wastewater into a photocatalytic reactor, adding a certain amount of the catalyst (controlling the concentration of the catalyst to be 0.2-2g L)-1)；
(j) And opening the cooling device and the light source, irradiating the reactor with certain light intensity, and carrying out the photocatalytic reduction of Cr (VI), wherein the Cr (VI) content and the total Cr content in the water body can be reduced after a period of time.
The photocatalytic reduction of Cr (VI) in water is characterized in that:
(1) the optimal conditions for preparing the PDA/BWO composite material are as follows: pH 8.5, Tris-HCl buffer 10mM, BWO 1g L-1The dopamine loading is 5%, and the 5PDA/BWO photocatalyst is obtained by magnetically stirring for 12 hours at normal temperature;
(2) the optimal conditions for photocatalytic reduction of Cr (VI) are as follows: pH 3.0, initial concentration of Cr (VI) 20mg L-15PDA/BWO concentration of 1.0g L-1The illumination intensity is 565mW cm-2。
According to the invention, BWO is prepared by a hydrothermal method with low cost and macroscopically controllable pH induction, and then the PDA-loaded BWO photocatalyst is prepared by a normal-temperature stirring method, so that the BWO band gap is reduced and the electron hole pair separation efficiency is improved. The catalyst has higher Cr (VI) reduction activity under visible light.
Drawings
FIG. 1 is a TEM image of BWO and 5PDA/BWO composite.
FIG. 2 shows the change of Cr (VI), Cr (III) and total Cr concentration in 5PDA/BWO system with time under the irradiation of visible light.
Best mode for carrying out the invention
The following detailed description of the embodiments of the invention is provided for the purpose of illustrating the invention.
Example 1
(1) Separately weighing Bi (NO)3)3·5H2O and Na2WO4·2H2O (Bi/W molar ratio controlled to be 2.15), dissolved in sequence in oneQuantitative 1.2M HNO3And 1.2M NaOH solution.
(2) The two solutions were mixed thoroughly, magnetically stirred for 1h, then placed in a reaction kettle and subjected to hydrothermal reaction at 200 ℃ for 12 h.
(3) After cooling, repeatedly cleaning with absolute ethyl alcohol and distilled water, and finally drying for 6 hours to obtain a bismuth auto-doping bismuth tungstate material (recorded as BWO);
(4) preparing 200mL of 10mM Tris-HCl buffer solution, and adjusting the pH value to 8.5;
(5) weighing 0.2g BWO, and ultrasonically dispersing into the solution in the step (4);
(6) weighing 10mg of dopamine, ultrasonically dispersing into the mixed solution obtained in the step (5), and continuously magnetically stirring for 12 hours;
(7) and (4) centrifugally separating the PDA-loaded BWO catalyst formed in the step (6) from the liquid phase. Washing with distilled water for 4 times to obtain precipitate;
(8) drying the precipitate obtained in the step (7) for 6h, and then grinding the dried solid into powder to obtain a dried 5PDA/BWO catalyst;
(9) will contain Cr (VI) (20mg L)-1) Introducing the simulated wastewater into a photocatalytic reactor, and adding 1g L-1The pH of the 5PDA/BWO catalyst is adjusted to 3.0, and the mixture is stirred for 30min in a dark state so as to reach the equilibrium of adsorption and desorption;
(10) the cooling device and light source were turned on at 565mW cm-2Under the light intensity of the light source, the light-catalyzed reduction reaction of Cr (VI) is carried out, the reduction rate of the Cr (VI) is up to 99.7 percent after 90min, and the total removal rate of Cr is 72.3 percent.
The 5PDA/BWO composite material prepared by the invention has high Cr (VI) reduction rate and total chromium removal rate in the photocatalytic reduction water, and in addition, the preparation method of the catalyst is simple and safe.
The above description is an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent flow transformations made by the present specification, or directly or indirectly applied to other related technologies, are included in the scope of the present invention.
Claims (2)
1. A method for preparing PDA/BWO and reducing hexavalent chromium [ Cr (VI) ] by photocatalysis comprises the following steps:
(a) separately weighing Bi (NO)3)3·5H2O and Na2WO4·2H2O (Bi/W molar ratio is controlled to be 2.05-2.20), which is dissolved in a certain amount of 1.2M HNO3And 1.2M NaOH solution;
(b) fully mixing the two solutions obtained in the step (a), magnetically stirring for 1-4h, then placing the mixture into a reaction kettle, and carrying out hydrothermal reaction for 9-24h at the temperature of 150-;
(c) after cooling, repeatedly cleaning the obtained precipitate with absolute ethyl alcohol and distilled water, and then drying for 4-10h to obtain a bismuth auto-doping bismuth tungstate material (recorded as BWO);
(d) preparing a Tris-HCl buffer solution with a certain concentration, and adjusting the pH value to 8.0-9.0;
(e) ultrasonically dispersing a certain amount of BWO into a Tris-HCl buffer solution;
(f) then adding a certain amount of dopamine, performing ultrasonic dispersion on the dopamine, and continuously performing magnetic stirring for 10-24 hours;
(g) centrifugally separating the PDA-loaded BWO catalyst formed in the step (f) from a liquid phase, and washing the separated liquid phase with water for 3 to 6 times to obtain a precipitate;
(h) drying the precipitate obtained in the step (g) for 4-10h, and then grinding the dried solid into powder to obtain a dried PDA/BWO catalyst;
(i) will contain Cr (VI) (10-30mg L)-1) Introducing the simulated wastewater into a photocatalytic reactor, adding a certain amount of the catalyst (controlling the concentration of the catalyst to be 0.2-2g L)-1)；
(j) And opening the cooling device and the light source, irradiating the reactor with certain light intensity, and carrying out the photocatalytic reduction of Cr (VI), wherein the Cr (VI) content and the total Cr content in the water body can be reduced after a period of time.
2. The method for photocatalytic reduction of Cr (VI) in water according to claim 1, wherein:
(1) the optimal conditions for preparing the PDA/BWO composite material are as follows: pH 8.5, Tris-HCl buffer 10mM, BWO 1g L-1Plural ofThe dopamine loading is 5%, and the 5PDA/BWO photocatalyst is obtained by magnetically stirring for 12 hours at normal temperature;
(2) the optimal conditions for photocatalytic reduction of Cr (VI) are as follows: pH 3.0, initial concentration of Cr (VI) 20mg L-15PDA/BWO concentration of 1.0g L-1The illumination intensity is 565mW cm-2。
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