CN102125835A - Manganese-supported cylindrical bismuth oxide photocatalyst capable of degrading 2,4,6-trichlorophenol in water - Google Patents
Manganese-supported cylindrical bismuth oxide photocatalyst capable of degrading 2,4,6-trichlorophenol in water Download PDFInfo
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- CN102125835A CN102125835A CN201110020267.3A CN201110020267A CN102125835A CN 102125835 A CN102125835 A CN 102125835A CN 201110020267 A CN201110020267 A CN 201110020267A CN 102125835 A CN102125835 A CN 102125835A
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Abstract
The invention discloses a manganese-supported cylindrical bismuth oxide photocatalyst capable of degrading 2,4,6-trichlorophenol (2,4,6-TCP) in water. The preparation of the catalyst adopts the solvent thermal synthesis method; when in synthesis, the molar ratio of all required components is controlled to meet the following formula: manganese sulfate: bismuth nitrate: nitric acid: P-123 block copolymer surfactant=1: (10-16.7): 66.7: (0.267-0.534). The calcination temperature is controlled at 450-550 DEG C. The appearance of the catalyst is cylindrical, the length is 1-3 microns, and the visible light with the wavelength below 550nm can be absorbed. Under the irradiation of a simulated visible light source, the photocatalysis reaction for degrading the 2,4,6-trichlorophenol is used for evaluating the activity of the catalyst, and about 90% of the 2,4,6-trichlorophenol (the concentration is 5mg/L) in a water body can be removed within 2 hours. The prepared manganese-supported cylindrical bismuth oxide photocatalyst has high catalysis efficiency, and the particle size of powder is large, thereby being conducive to recycling and reuse; and the manufacturing method is simple, the cost is low, and the cycle is short, thereby having good industrial application prospects.
Description
Technical field
The present invention relates to a kind of degradation water 2,4 that is used for, the photochemical catalyst of 6-trichlorophenol belongs to the surround lighting catalysis technical field.
Background technology
Chlorophenol (CPs) has good chemistry and heat endurance as a kind of typical persistent organic pollutants, and easily by the food chain enrichment in vivo, ecological environment and human beings'health in serious threat.Wherein, 2,4, (2,4,6-TCP) strong toxicity, and difficult degradation are widely used in fields such as bactericide, herbicide, defoliant, papermaking bleaching and drinking water disinfection to the 6-trichlorophenol.Set up fast, thoroughly, environmental protection to contain the chlorophenol sewage water treatment method significant for guarantee environment water body safety.
Along with the solar energy CHEMICAL DEVELOPMENT, photocatalysis technology with operating cost economy, oxidability thoroughly, advantage such as non-secondary pollution obtained paying close attention to widely in sewage disposal.Common unification compound photochemical catalyst mostly is metal oxide or sulfide, as TiO
2, CdS and WO
3Deng.The most representative TiO
2Because its greater band gap (3.2eV), and ultraviolet light that can only absorbing wavelength λ≤387nm, limited its development in actual applications.At present, most active research field is by method development of new catalyst such as compound, modifications in the photocatalysis, efficiently utilizes organic matter and inorganic matter system in the sunshine degradation water on the one hand, improves catalytic performance; Improve its stability and the rate of recovery on the one hand.
The bismuthino compound has wide research prospect because of the energy gap with special layer structure and suitable size.Many bismuthino compounds all have photocatalytic activity as bismuth oxide, BiOX, bismuth tungstate, bismuth molybdate, bismuthates etc.Wherein bismuth oxide is as a kind of important functional material, medicinal astringent, ceramic colorant, fire-retardant for plastic, high dioptric glass, glass additive and manufacturing of nuclear engineering glass and nuclear reactor fuel not only can be applied to, and highly active photochemical catalyst can also be obtained by the design of crystal structure and band structure is synthetic.Document " Liu Yan, seal can ring Wu Yanfeng, Zhou Aiqiu, Xu Xiaohong. porous β-Bi
2O
3Preparation and Photocatalytic Performance Study [J]. silicate circular, 2010, (04): 751-756 " show the β-Bi of its preparation
2O
3Have the nanoporous lamellar structure, band gap width is 2.72eV, has significantly improved the absorption to visible light, methyl orange capable of being fast degraded, rhodamine B and 4-chlorophenol.
Ubiquitously utilize that solar energy efficient is low, inactivation is fast and is easy to deficiency such as loss at photochemical catalyst, by means of the doping vario-property of metallic element in the preparation process, the photocatalysis performance of bismuth oxide and stability can be further improved.Document " OsterlohF E.Inorganic Materials as Catalysts for Photochemical Splitting of Water[J] .Chemical Materials; 2008; 20:35-54 " studies show that the bismuth system oxide material after element modified such as doping V, Mo and Pb had better catalytic effect and continuation before mixing, and embody certain visible light-responded.Document " Zhang Xia rues Gong Qian, Wei Chaohai recklessly. the preparation of manganese doped nano titanium dioxide and visible light catalytic performance [J] thereof. and chemical industry progress, 2010, (06): 1071-1079 " think that a small amount of Mn ion in doping back can enter TiO
2Perhaps be present in TiO
2In the gap, make TiO
2Valence band and conduction band between produce intermediate level, light induced electron and hole can produce transition by this intermediate level, excitation energy is reduced to visible-range, can expand the visible absorption zone of catalyst.
Less about the bibliographical information that synthesizes manganese load bismuth oxide catalysis material at present, need further research on the basis of rationally controlling reaction condition, to strengthen ability that it activates visible light, improve catalytic efficiency and recycling rate of waterused.
Summary of the invention
The purpose of this invention is to provide in a kind of degradation water 2,4, the manganese load column bismuth oxide photochemical catalyst of 6-trichlorophenol.This catalyst has advantages such as photocatalytic activity height, particle size are big, loose structure, the chlorophenols organic pollution in the water body of can degrading effectively.This Preparation of catalysts process is simple, and operating condition is easy to control, and the gained catalyst particle size is a micron order, has improved and has reclaimed repeatability; Because its fabrication cycle is short, with low cost, this technology has the favorable industrial application prospect aspect the processing organic wastewater simultaneously.
This catalyst adopts the preparation of solvent thermal synthesis method, with manganese sulfate and bismuth nitrate is raw material, Pluronic P-123 (block interpolymers surfactant, its structural formula PEO (20)-PPO (70)-PEO (20), mean molecule quantity is 5750) as structure directing agent, nitric acid is hydrolyst, and required each component mol ratio is controlled to be manganese sulfate when synthetic: bismuth nitrate: nitric acid: Pluronic P-123=1: 10～16.7: 66.7: 0.267～0.534.Technical scheme of the present invention is as follows:
A kind ofly can be used in the water 2,4, the preparation method of the manganese load column bismuth oxide photochemical catalyst of 6-trichlorophenol degraded mainly is divided into solvent thermal synthesis process and last handling process.The presoma that at first prepares the manganese bismuth composite oxide by the solvent thermal synthesis method, the sequential processes precursor powder that adopt calcining thereafter, cools off and mill prepares manganese load column bismuth oxide photochemical catalyst.Step comprises:
1) solvent thermal synthesis process: the Pluronic P-123 block interpolymers surfactant of 0.008～0.016 mol is dissolved in the salpeter solution of 2 mol; Continue under the stirring five water bismuth nitrates to be dissolved in the above-mentioned solution, regulate bismuth nitrate concentration in 0.3～0.5 mol; Continue to stir, making a gesture of measuring according to the mole of manganese and bismuth is manganese sulfate to be joined in 1: 10～1: 16.7 in the solution of above-mentioned bismuth nitrate, obtains the canescence precursor solution after stirring; After with its ageing 3 hours under the stirring at room condition, be transferred to and contain in 100 milliliters of stainless steel autoclaves of teflon-lined, be positioned in the vacuum drying chamber airtight crystallization after the sealing 24 hours, temperature remains on 150 ℃.Crystallization process is cooled to room temperature with its product manganese bismuth compound after finishing, suction filtration is removed excessive moisture, and use deionized water to wash sediment on the gained filter paper repeatedly to remove residual Pluronic P-123, at last the sediment on the filter paper is placed 120 ℃ environment dry, promptly make the presoma of manganese load bismuth oxide;
2) last handling process: the precursor powder of gained was placed in the Muffle furnace with 450～550 ℃ high-temperature calcination after 3 hours, through cooling, grind, promptly obtain manganese load column bismuth oxide photochemical catalyst.
In this invention, the preparation process 1 of manganese load column bismuth oxide photochemical catalyst) solvent is selected the nitric acid of 2 mol in, can with the effective complexing of five water bismuth nitrates, hydrolysis is relaxed more, obtain compound colloidal sol uniformly; 2) high-temperature calcination 3 hours in 450～550 ℃ Muffle furnace of manganese load bismuth oxide precursor powder makes manganese load bismuth oxide obtain further crystallization in.
The manganese load column bismuth oxide photocatalyst activity evaluation method of the present invention's preparation is as follows:
1) be the ratio of 20 grams per liters according to catalyst and reactant liquor volume, take by weighing a certain amount of manganese load column bismuth oxide photochemical catalyst powder and 2,4,6-trichlorophenol solution adds in the Photoreactor, and 2,4, the 6-TCP initial concentration of solution is 5 mg/litre;
2) under the lucifuge condition ultrasonic about 20 minutes, catalyst is scattered in fully forms emulsion in the solution, and it is saturated to reach absorption;
3) open xenon lamp (simulated solar spectrum, 500 watts of power; Model C EL-S500, religion Jin Yuan Science and Technology Ltd. in Beijing, Beijing) irradiation, photocatalytic degradation reaction timing begins.Wherein entire reaction course is carried out under ultrasound condition, makes reactant liquor and catalyst mix even, in the outside circulator bath control system that inserts of Photoreactor, makes reacting liquid temperature remain on 25～35 ℃, timing sampling simultaneously;
4) reaction finishes the back centrifugal reaction solution to reclaim catalyst granules, also with high performance liquid chromatograph (HPLC) the day part sample concentration is analyzed behind the centrifugal sample, calculates the reaction degradation rate.Wherein degradation rate (%) computational methods are (organic matter removal concentration/organic matter initial concentration) * 100%.
Description of drawings
Fig. 1 is a manganese load column bismuth oxide photochemical catalyst scanning electron microscope image;
Fig. 2 is the X-ray diffraction spectrogram of manganese load column bismuth oxide photochemical catalyst;
Fig. 3 is the ultraviolet-visible light diffuse reflection spectrum of manganese load column bismuth oxide photochemical catalyst;
Fig. 4 is the manganese load column bismuth oxide photochemical catalyst and the bismuth oxide powder light degradation 2,4 of the present invention's preparation, the degradation rate time history plot of 6-TCP.
The specific embodiment
Embodiment 1
Weigh in the balance and get 6.96 gram Pluronic P-123 block interpolymers surfactants and place beaker, add the nitric acid (HNO of 100 milliliter of 2 mol
3) solution, stir by magnetic stirring apparatus, treat that Pluronic P-123 is dissolved in nitric acid fully and forms after the water white solution, add 19.73 grams, the five water bismuth nitrate (Bi (NO that take by weighing in advance
3)
35H
2O), proceed to stir.After treating the solution clarification, add 0.51 gram manganese sulfate (MnSO
4H
2O), continue to be stirred to manganese sulfate and dissolve fully, this moment, solution existed with linen even solation.Continuing to make the ageing at room temperature of this colloidal sol about 3 hours under the state that stirs, obtain the precursor solution of rose; This solution is transferred to has in the teflon-lined stainless steel autoclave, will be put in 150 ℃ the vacuum drying chamber crystallization after the autoclave sealing 24 hours; Take out autoclave and be cooled to room temperature, from polytetrafluoroethyllining lining, take out plural gel afterwards and carry out suction filtration, the sediment that washes gained with deionized water repeatedly residues in the Pluronic P-123 on surface with flush away, the solids of suction filtration gained is placed 120 ℃ environment evaporate to dryness, obtain precursor powder; At last this precursor powder was calcined 3 hours in 450 ℃ Muffle furnace, can be obtained manganese load column bismuth oxide photochemical catalyst, be designated as sample 1#.This photochemical catalyst pattern is a column, and length is about 3 microns, but the ultraviolet-visible light diffuse reflection spectrum shows the visible light that its absorbing wavelength 550 nanometers are following.
Preparation presoma step is with embodiment 1, and wherein Pluronic P-123 is 9.28 grams; Nitric acid (2 mol) is 100 milliliters; Five water bismuth nitrate (Bi (NO
3)
35H
2O) be 24 grams; Manganese sulfate (MnSO
4) be 0.51 gram; 550 ℃ of calcinings of Muffle furnace control temperature are 3 hours in the last handling process.Be designated as sample 2#.This photochemical catalyst pattern is a column, and length is about 2.5 microns, but the ultraviolet-visible light diffuse reflection spectrum shows the visible light that its absorbing wavelength 500 nanometers are following.
Embodiment 3
The presoma preparation process is with embodiment 1, and wherein Pluronic P-123 is 9.28 grams; Nitric acid (2 mol) is 100 milliliters; Five water bismuth nitrate (Bi (NO
3)
35H
2O) be 14.55 grams; Manganese sulfate (MnSO
4) be 0.51 gram; 480 ℃ of calcinings of Muffle furnace control temperature are 3 hours in the last handling process.Be designated as sample 3#.This photochemical catalyst pattern is a column, and length is 1.5～2 microns, but the ultraviolet-visible light diffuse reflection spectrum shows the visible light that its absorbing wavelength 524 nanometers are following.
The presoma preparation process is with embodiment 1, and wherein Pluronic P-123 is 7.83 grams; Nitric acid (2 mol) is 100 milliliters; Five water bismuth nitrate (Bi (NO
3)
35H
2O) be 24 grams; Manganese sulfate (MnSO
4) be 0.51 gram; 450 ℃ of calcinings of Muffle furnace control temperature are 3 hours in the last handling process.Be designated as sample 4#.This photochemical catalyst pattern is a column, and length is about 1.5 microns, but the ultraviolet-visible light diffuse reflection spectrum shows the visible light that its absorbing wavelength 500 nanometers are following.
The presoma preparation process is with embodiment 1, and wherein Pluronic P-123 is 4.64 grams; Nitric acid (2 mol) is 100 milliliters; Five water bismuth nitrate (Bi (NO
3)
35H
2O) be 20.37 grams; Manganese sulfate (MnSO
4) be 0.51 gram; 550 ℃ of calcinings of Muffle furnace control temperature are 3 hours in the last handling process.Be designated as sample 5#.This photochemical catalyst pattern is a column, and length is about 1.2 microns, but the ultraviolet-visible light diffuse reflection spectrum shows the visible light that its absorbing wavelength 530 nanometers are following.
The prepared catalyst of above-mentioned each example is respectively applied for following photocatalytic degradation experiment, investigates the catalytic activity of each catalyst:
Reaction 1: take by weighing 0.1 gram catalyst 1#, adding initial concentration is 2 of 5 mg/litre, 4,100 milliliters of the 6-TCP aqueous solution, pH 8.0, and ultrasonic dispersion was scattered in catalyst fully in about 20 minutes and forms emulsion in the solution under the dark room conditions, and it is saturated to reach absorption, open xenon lamp and carry out light-catalyzed reaction, even in the light-catalyzed reaction process by ultrasonic reactant liquor and the catalyst mix of making, keep the temperature of reactant liquor simultaneously by the circulator bath control system.Timing sampling by centrifugal removal catalyst powder, is got supernatant and is analyzed on high performance liquid chromatograph.
Reaction 2: take by weighing 0.2 gram catalyst 2#, adding initial concentration is 2,4 of 5 mg/litre, 100 milliliters of the 6-TCP aqueous solution, and it is described with reaction 1 that surplus person reacts.
Reaction 3: take by weighing 0.2 gram catalyst 3#, adding initial concentration is 2,4 of 5 mg/litre, 100 milliliters of the 6-TCP aqueous solution, and it is described with reaction 1 that surplus person reacts.
Reaction 4: take by weighing 0.2 gram catalyst 4#, adding initial concentration is 2,4 of 5 mg/litre, 100 milliliters of the 6-TCP aqueous solution, and it is described with reaction 1 that surplus person reacts.
Reaction 5: take by weighing 0.2 gram catalyst 5#, adding initial concentration is 2,4 of 5 mg/litre, 100 milliliters of the 6-TCP aqueous solution, and it is described with reaction 1 that surplus person reacts.
Phase flows: acetonitrile: water=60: 40 (volume ratio, the acetate that adds 1% water volume is regulated pH);
Flow velocity: 1 ml/min;
Chromatographic column: Waters WAT 045905Symmetry C18,5 μ m;
Detect wavelength: 220 nanometers;
Sample size: 20 microlitres.
Claims (4)
1. one kind can be used in the degradation water 2,4, the preparation method of the manganese load column bismuth oxide photochemical catalyst of 6-trichlorophenol, and its feature comprises the steps:
1) precursor solution preparation: Pluronic P-123 is dissolved in salpeter solution, under stirring five water bismuth nitrates is dissolved in the above-mentioned solution, control bismuth nitrate concentration is 0.3～0.5 mol; Making a gesture of measuring according to the mole of manganese and bismuth is 1: 10～1: 16.7, manganese sulfate is joined in the solution of above-mentioned bismuth nitrate under stirring, continues stirring until to mix, and obtains the canescence precursor solution;
2) hydro-thermal building-up process: with the ageing at room temperature 3 hours under stirring of canescence precursor solution, transfer to afterwards and contain in the teflon-lined stainless steel autoclave, sealing autoclave, and be placed in 150 ℃ the vacuum drying chamber airtight crystallization 24 hours;
3) catalyst precursor preparation: after from vacuum drying chamber, taking out autoclave, be cooled to room temperature; Take out crystallization product manganese bismuth compound, suction filtration uses sediment several on the deionized water rinsing filter paper, places 120 ℃ environment dry afterwards, promptly gets the presoma of manganese load bismuth oxide catalyst;
4) prepared precursor powder places Muffle furnace with 450～550 ℃ of calcinings 3 hours Preparation of Catalyst: with above-mentioned steps 3), is cooled to room temperature, grinds, and promptly obtains manganese load column bismuth oxide photochemical catalyst.
2. the preparation method of photochemical catalyst according to claim 1, it is characterized in that: the preparation process 1 of manganese load column bismuth oxide photochemical catalyst) described Pluronic P-123 is a nonionic block interpolymers surfactant, structural formula is PEO (20)-PPO (70)-PEO (20), mean molecule quantity is 5750, and its solution concentration is controlled at 0.008～0.016 mol.
3. preparation method as claimed in claim 1, wherein described in the step 1) in the salpeter solution concentration of nitric acid be 2 mol.
4. this photochemical catalyst pattern is a column, and length is 1～3 micron, but the following visible light of absorbing wavelength 550 nanometers.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119151A (en) * | 2016-06-21 | 2016-11-16 | 盐城工学院 | Bacterial strain and method for screening and separating thereof for degraded 2,4,6 trichlorophenol, 2,4,6,-Ts |
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| US6169049B1 (en) * | 1997-04-28 | 2001-01-02 | John P. Witham | Solution coated hydrothermal BaTiO3 for low-temperature firing |
| JP2003260356A (en) * | 2002-03-08 | 2003-09-16 | Univ Waseda | Method for manufacturing h-type layer perovskite photocatalyst and h-type layer perovskite photocatalyst |
| CN101303928A (en) * | 2008-01-14 | 2008-11-12 | 浙江大学 | Cobalt material doping with ferrous acid bismuth multi-iron and preparation method thereof |
| CN101890354A (en) * | 2010-07-27 | 2010-11-24 | 北京师范大学 | Method for preparing bismuth ferrite photocatalyst |
-
2011
- 2011-01-18 CN CN201110020267.3A patent/CN102125835A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6169049B1 (en) * | 1997-04-28 | 2001-01-02 | John P. Witham | Solution coated hydrothermal BaTiO3 for low-temperature firing |
| JP2003260356A (en) * | 2002-03-08 | 2003-09-16 | Univ Waseda | Method for manufacturing h-type layer perovskite photocatalyst and h-type layer perovskite photocatalyst |
| CN101303928A (en) * | 2008-01-14 | 2008-11-12 | 浙江大学 | Cobalt material doping with ferrous acid bismuth multi-iron and preparation method thereof |
| CN101890354A (en) * | 2010-07-27 | 2010-11-24 | 北京师范大学 | Method for preparing bismuth ferrite photocatalyst |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119151A (en) * | 2016-06-21 | 2016-11-16 | 盐城工学院 | Bacterial strain and method for screening and separating thereof for degraded 2,4,6 trichlorophenol, 2,4,6,-Ts |
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Application publication date: 20110720 |