CN102019184A - Preparation method and application of novel perovskite photocatalyst containing bismuth - Google Patents
Preparation method and application of novel perovskite photocatalyst containing bismuth Download PDFInfo
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- CN102019184A CN102019184A CN2010106055673A CN201010605567A CN102019184A CN 102019184 A CN102019184 A CN 102019184A CN 2010106055673 A CN2010106055673 A CN 2010106055673A CN 201010605567 A CN201010605567 A CN 201010605567A CN 102019184 A CN102019184 A CN 102019184A
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Abstract
The invention discloses a preparation method and an application of a novel perovskite photocatalyst containing bismuth. The main preparation technology comprises the following steps: dissolving Bi(NO3)3.5H2O, La(NO3)3.nH2O and Fe(NO3)3.9H2O in nitric acid, then adding citric acid to fully mix, performing thermostatic stirring to obtain transparent viscous gel, placing the transparent viscous gel in a drying oven to dry and obtain dried gel; decomposing the dried gel in a muffle furnace, and roasting with a high temperature furnace to obtain Bi1-xLaxFeO3 catalyst. The preparation method has simple technology and low cost. The catalyst is used in the photocatalytic reaction and is characterized in that the degradation activity of the catalyst to parachlorophenol is high under visible-light irradiation.
Description
Technical field
The present invention relates to a kind of Preparation of catalysts method, refer in particular to a kind of preparation method and application aspect the photocatalytic degradation phenol wastewater thereof of bismuth-containing perovskite type photocatalyst.
Background technology
Coal is the main fossil energy of China, it also is the primary raw material of many important chemical products, along with social economy continues, high speed development, higher growth rate also appears in the demand of China's energy, chemical products in recent years, and Coal Chemical Industry has been occupied critical role in China's energy, chemical production field.Along with country subsists strong increasingly to the control of pollutant emission, Chinese large-sized Coal Chemical Industry base generally is in the water-deficient area in addition, so enhanced sewage is administered, realizes the recycling and zero-emission of waste water, the conserve water resource has become the inexorable trend and the social duty of coal chemical industry enterprises technical development.
Coal chemical industrial waste water mainly is meant the waste water that produces in coal gasification, destructive distillation, purification and chemical products production process.The pollutant levels height of coal chemical industrial waste water, complicated component, intractability is big, and the processing cost height is a kind of industrial wastewater that is difficult to administer most.And phenolic compound is typical pollutant in the coal chemical industrial waste water, and not only difficult degradation but also toxicity are big for they, have potential hazard carcinogenic, teratogenesis.High-concentration phenolic wastewater is mainly recycled with physical-chemical process, and for the processing of low concentration phenol wastewater, mature technique is not arranged also at present.The photochemical catalysis oxidizing process is that a kind of green with good development prospect purifies one of phenol wastewater technology.TiO
2Be to use more a kind of photochemical catalyst in present people's research, but owing to have its greater band gap, a little less than the visible-range response, to shortcomings such as the sunshine utilization rate are low.Therefore, to TiO
2Carry out modification and seek the extensive concern that novel photocatalysis agent Research on Phenol Wastewater Treatment has caused Chinese scholars.
Perovskite composite oxides ABO
3Have special stable crystal structure, make stability of material fine, and raw material sources are extensive, lower cost.At the beginning of the fifties, Parravano etc. have studied the oxidation reaction of CO on perovskite composite oxide the earliest.At the beginning of the seventies, Meadowcroft has reported the La of the composite metal oxide with perovskite structure
0.8Sr
0.2CoO
3, its catalytic oxidation activity can be compared with platinum.From then on, worldwide formed the upsurge of a research perovskite structure metal oxide catalyst, research field constantly enlarges.Perovskite composite oxides is demonstrating its application promise in clinical practice as the novel semi-conductor photochemical catalyst aspect improvement waste water and the exhaust emission in recent years.But up to the present, perovskite oxide is used for catalytic combustion more, and perofskite type oxide is applied to light-catalyzed reaction, and especially the research of aldehydes matter such as photocatalytic degradation parachlorophenol is also very few.
Contain the Bi compound and have unique character: contain Bi
3+The metal oxide energy gap is very narrow, and its valence band is made up of Bi-6s and two tracks of O-2p, and this is different from common semiconductor visible light catalyst (generally forming valence band by the 2p track), and this just characteristics cause the great interest of people.Many researchers will contain the Bi compound and be applied in the light-catalyzed reaction, and will be less but the perovskite degraded that contains Bi contains the research of phenol material, so the synthetic A position of this patent contains the perovskite catalyst of Bi, and investigate the activity of its visible light photocatalytic degradation parachlorophenol.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method and application thereof of novel bismuth-containing perovskite type photocatalyst.Adopt sol-gel process, with Fe (NO
3)
39H
2O, Bi (NO
3)
35H
2O and La (NO
3)
3NH
2O, complexing agent is a citric acid, and solvent is 2mol/L salpeter solution and deionized water, has prepared a kind of novel bismuth-containing perovskite composite oxide photochemical catalyst, this catalyst is applied to photocatalysis to degrade organic matter reaction, the parachlorophenol of can degrading under visible light.
The technical problem to be solved in the present invention is realized by following scheme: a kind of preparation method of novel bismuth-containing perovskite type photocatalyst and application thereof take by weighing Fe (NO
3)
39H
2O, Bi (NO
3)
35H
2O, La (NO
3)
3NH
2O is dissolved in the 2mol/L salpeter solution, makes clear solution, wherein Fe (NO
3)
39H
2O and Bi (NO
3)
35H
2O, La (NO
3)
3NH
2The amount of substance ratio of O and used 2mol/L nitric acid is 1: 0.1-0.98: 0.02-0.9: 20; Take by weighing citric acid it is dissolved in the deionized water, be mixed with the citric acid solution of 0.5mol/L, wherein Fe (NO
3)
39H
2O is 1: 4 with the ratio of the amount of substance of citric acid; The citric acid solution of preparation is added in the clear solution, at room temperature stir 10min it is fully mixed, stir at 70 ℃ of constant temperature water baths then, transpiring moisture obtains transparent thick colloid; The transparent thick colloid that obtains is placed in the baking oven, get xerogel with dry 24h under 100 ℃ of air atmosphere conditions, afterwards xerogel is decomposed 3h with 500 ℃ of condition roastings in Muffle furnace and gets the former powder of oxide, again under air atmosphere with 700 ℃ of condition roasting 3h, make Bi at last
1-xLa
xFeO
3Catalyst, obtained catalyst B i
1-xLa
xFeO
3The span of middle x is 0.02-0.9.
Technique scheme is described, in the prepared clear solution, and Fe (NO
3)
39H
2O and Bi (NO
3)
35H
2O, La (NO
3)
3NH
2The amount of substance of O and used 2mol/L nitric acid is than preferred 1: 0.5-0.95: 0.05-0.5: 20, and prepared Bi under this condition
1-xLa
xFeO
3X is 0.05-0.5 in the catalyst; Most preferably be 1: 0.9: 0.1: 20, prepared Bi under this condition
1-xLa
xFeO
3X is 0.1 in the catalyst.
The catalyst of the present invention's preparation is applied to obtain result preferably in the photocatalysis to degrade organic matter reaction.Concrete experimental implementation adopts SGY-I type multifunctional light chemical reactor.Visible light source adopts metal halide lamp.Basic reaction condition is: the initial concentration of parachlorophenol is 20mg/L, and catalyst amount is 1g/L, electromagnetic agitation, and container bottom blasts air in certain amount in the illumination reaction process, and the dischargeable capacity of reactor is 250mL.Carry out before the light-catalyzed reaction, earlier suspension is stirred 30min under dark reaction, make parachlorophenol reach abundant absorption at catalyst surface.The reaction solution temperature is controlled at 16-18 ℃, timing sampling, visible light illumination 5h, solution centrifugal separation 15min after reaction finishes (5000 commentaries on classics/min), survey its filtrate in the absorbance that 280nm (parachlorophenol) locates with UV-7504PC type ultraviolet-visible spectrophotometer then, know the change in concentration of parachlorophenol according to the variation of absorbance by inference.With
(A
0Be the initial absorbance of the parachlorophenol aqueous solution, A is the absorbance of the parachlorophenol aqueous solution in the illumination process) expression parachlorophenol the light degradation rate.Utilize above-mentioned measuring method and condition, the degradation rate of this catalyst activity being estimated discovery parachlorophenol after its 5 hours is 94.6%.
Advantage of the present invention is that preparation method's technology is simple, and is with low cost, and the catalyst structure of preparing is a kind of perovskite structure, can respond under visible light as photochemical catalyst, has catalytic activity preferably.Photochemical catalyst provided by the invention is compared with existing catalyst, has following essential characteristics:
1. catalyst is complexing agent with the citric acid, adopts the sol-gel process preparation, and simple to operate, with low cost, roasting has formed single-phase perovskite catalyst Bi in air atmosphere
1-xLa
xFeO
3
2.Bi
1-xLa
xFeO
3The catalyst parachlorophenol of can under visible light, degrading;
3. with Bi
1-xLa
xFeO
3Catalyst is applied to have photocatalytic activity preferably in the experiment of photocatalytic degradation parachlorophenol.
Description of drawings
Fig. 1 is the process chart of preparation new catalyst
Fig. 2 is embodiment 1 obtained Bi
0.9La
0.1FeO
3The XRD figure spectrum of perovskite type photocatalyst
The catalyst thing phase that adopts D8ADVANCE type powder x-ray diffraction instrument to detect is by the position (being respectively 23 °, 32 °, 40 °, 52 °, 58 °, 68 °) in the XRD figure spectrum with relative intensity as can be known, catalyst B i
0.9La
0.1FeO
3Be the perovskite phase
Fig. 3 is embodiment 1 obtained Bi
0.9La
0.1FeO
3The active figure of the photocatalytic degradation parachlorophenol of perovskite type photocatalyst
Fig. 4 is embodiment 2 obtained Bi
0.95La
0.05FeO
3The XRD figure spectrum of perovskite type photocatalyst
The catalyst thing phase that adopts D8ADVANCE type powder x-ray diffraction instrument to detect is by the position (being respectively 23 °, 32 °, 40 °, 52 °, 58 °, 68 °) in the XRD figure spectrum with relative intensity as can be known, catalyst B i
0.95La
0.05FeO
3Be the perovskite phase
Fig. 5 is embodiment 2 obtained Bi
0.95La
0.05FeO
3The active figure of the photocatalytic degradation parachlorophenol of perovskite type photocatalyst
Fig. 6 is embodiment 3 obtained Bi
0.5La
0.5FeO
3The XRD figure spectrum of perovskite type photocatalyst
The catalyst thing phase that adopts D8ADVANCE type powder x-ray diffraction instrument to detect is by the position (being respectively 23 °, 32 °, 40 °, 52 °, 58 °, 68 °) in the XRD figure spectrum with relative intensity as can be known, catalyst B i
0.5La
0.5FeO
3Be the perovskite phase
Fig. 7 is embodiment 3 obtained Bi
0.5La
0.5FeO
3The active figure of the photocatalytic degradation parachlorophenol of perovskite type photocatalyst
Fig. 8 is embodiment 4 obtained Bi
0.2La
0.8FeO
3The XRD figure spectrum of perovskite type photocatalyst
The catalyst thing phase that adopts D8ADVANCE type powder x-ray diffraction instrument to detect is by the position (being respectively 23 °, 32 °, 40 °, 52 °, 58 °, 68 °) in the XRD figure spectrum with relative intensity as can be known, catalyst B i
0.2La
0.8FeO
3Be the perovskite phase
Fig. 9 is embodiment 4 obtained Bi
0.2La
0.8FeO
3The active figure of the photocatalytic degradation parachlorophenol of perovskite type photocatalyst
The specific embodiment
Embodiment 1: take by weighing 8.7313g Bi (NO
3)
35H
2O, 0.6498g La (NO
3)
3NH
2O and 8.08g Fe (NO
3)
39H
2O is dissolved in the 200mL 2mol/L salpeter solution, obtains clear solution; Take by weighing the 16.8112g citric acid and join and be dissolved in the 160mL deionized water, join after the dissolving in the clear solution, in 70 ℃ of following waters bath with thermostatic control and stir, transpiring moisture obtains transparent thick colloid.With the gained colloid in baking oven under 100 ℃ of air atmospheres dry 24h get xerogel, 500 ℃ of roasting 3h get the former powder of oxide in Muffle furnace then, 700 ℃ of roasting 3h make Bi at last under air atmosphere
0.9La
0.1FeO
3Catalyst, the prepared catalyst of the present embodiment 20mg/L parachlorophenol simulated wastewater of under visible light, degrading, catalyst amount is under the condition of 1g/L, the photocatalytic degradation rate of different time is as shown in the table:
| Time/h | 0.5 | 1 | 1.5 | 2 | 2.5 | 3 | 4 | 5 |
| Degradation rate/% | 11.8 | 34.4 | 54.1 | 69.5 | 80.4 | 85.8 | 91.3 | 94.6 |
Embodiment 2: implementation condition is with embodiment 1, and different is to take by weighing 9.2163g Bi (NO
3)
35H
2O, 0.3249gLa (NO
3)
3NH
2O and 8.08g Fe (NO
3)
39H
2O is dissolved in the 200mL 2mol/L salpeter solution, obtains clear solution; Make Bi at last
0.95La
0.05FeO
3Catalyst, the prepared catalyst of the present embodiment 20mg/L parachlorophenol simulated wastewater of under visible light, degrading, catalyst amount is under the condition of 1g/L, the photocatalytic degradation rate of different time is as shown in the table:
| Time/h | 0.5 | 1 | 1.5 | 2 | 2.5 | 3 | 4 | 5 |
| Degradation rate/% | 3 | 17.8 | 53.2 | 61.6 | 72.2 | 85.5 | 90 | 91 |
Embodiment 3: implementation condition is with embodiment 1, and different is to take by weighing 4.8507g Bi (NO
3)
35H
2O, 3.2492gLa (NO
3)
3NH
2O and 8.08g Fe (NO
3)
39H
2O is dissolved in the 200mL 2mol/L salpeter solution, obtains clear solution; Make Bi at last
0.5La
0.5FeO
3Catalyst, the prepared catalyst of the present embodiment 20mg/L parachlorophenol simulated wastewater of under visible light, degrading, catalyst amount is under the condition of 1g/L, the photocatalytic degradation rate of different time is as shown in the table:
| Time/h | 0.5 | 1 | 1.5 | 2 | 2.5 | 3 | 4 | 5 |
| Degradation rate/% | 9.4 | 25.6 | 44.3 | 63.4 | 74.8 | 78.5 | 88.9 | 94 |
Embodiment 4: implementation condition is with embodiment 1, and different is to take by weighing 1.9403g Bi (NO
3)
35H
2O, 5.1987gLa (NO
3)
3NH
2O and 8.08g Fe (NO
3)
39H
2O is dissolved in the 200mL 2mol/L salpeter solution, obtains clear solution; Make Bi at last
0.2La
0.8FeO
3Catalyst, the prepared catalyst of the present embodiment 20mg/L parachlorophenol simulated wastewater of under visible light, degrading, catalyst amount is under the condition of 1g/L, the photocatalytic degradation rate of different time is as shown in the table:
| Time/h | 0.5 | 1 | 1.5 | 2 | 2.5 | 3 | 4 | 5 |
| Degradation rate/% | 56.6 | 67.7 | 76 | 82.7 | 86.1 | 86.3 | 91.1 | 89 |
Claims (3)
1. sol-gel process has been adopted in the preparation method of a novel bismuth-containing perovskite type photocatalyst and application thereof, and complexing agent is a citric acid, it is characterized in that: take by weighing Fe (NO
3)
39H
2O, Bi (NO
3)
35H
2O, La (NO
3)
3NH
2O is dissolved in the 2mol/L salpeter solution, makes clear solution, wherein Fe (NO
3)
39H
2O and Bi (NO
3)
35H
2O, La (NO
3)
3NH
2The amount of substance ratio of O and used 2mol/L nitric acid is 1: 0.1-0.98: 0.02-0.9: 20; Take by weighing citric acid it is dissolved in the deionized water, be mixed with the citric acid solution of 0.5mol/L, wherein Fe (NO
3)
39H
2O is 1: 4 with the ratio of the amount of substance of citric acid; The citric acid solution of preparation is added in the clear solution, at room temperature stir 10min it is fully mixed, stir at 70 ℃ of constant temperature water baths then, transpiring moisture obtains transparent thick colloid; The transparent thick colloid that obtains is placed in the baking oven, get xerogel with dry 24h under 100 ℃ of air atmosphere conditions, afterwards xerogel is decomposed 3h with 500 ℃ of condition roastings in Muffle furnace and gets the former powder of oxide, again under air atmosphere with 700 ℃ of condition roasting 3h, make Bi at last
1-xLa
xFeO
3Catalyst, obtained catalyst B i
1-xLa
xFeO
3The span of middle x is 0.02-0.9.
2. according to claim 1, sol-gel process has been adopted in a kind of preparation method of novel bismuth-containing perovskite type photocatalyst and application thereof, and complexing agent is a citric acid, it is characterized in that: take by weighing Fe (NO
3)
39H
2O, Bi (NO
3)
35H
2O, La (NO
3)
3NH
2O is dissolved in the 2mol/L salpeter solution, makes clear solution, wherein Fe (NO
3)
39H
2O and Bi (NO
3)
35H
2O, La (NO
3)
3NH
2The amount of substance ratio of O and used 2mol/L nitric acid is 1: 0.5-0.95: 0.05-0.5: 20, and obtained catalyst B i
1-xLa
xFeO
3The span of middle x is 0.05-0.5.
3. according to claim 1, sol-gel process has been adopted in a kind of preparation method of novel bismuth-containing perovskite type photocatalyst and application thereof, and complexing agent is a citric acid, it is characterized in that: take by weighing Fe (NO
3)
39H
2O, Bi (NO
3)
35H
2O, La (NO
3)
3NH
2O is dissolved in the 2mol/L salpeter solution, makes clear solution, wherein Fe (NO
3)
39H
2O and Bi (NO
3)
35H
2O, La (NO
3)
3NH
2The amount of substance ratio of O and used 2mol/L nitric acid is 1: 0.9: 0.1: 20, and obtained catalyst B i
1-xLa
xFeO
3Middle x's is 0.1.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030390A (en) * | 2014-06-04 | 2014-09-10 | 上海应用技术学院 | Method for degrading musk ketone under natural light by utilizing titanium dioxide/charcoal hybrid aerogel |
| CN105080553A (en) * | 2015-08-04 | 2015-11-25 | 内蒙古大学 | Method for preparing stanniferous double-perovskite type phenol photocatalytic degradation catalyst |
| CN106040251A (en) * | 2016-06-16 | 2016-10-26 | 内蒙古大学 | Preparation method for sol-gel one-step low-temperature synthesis of pure-phase Bi25F3O40/ZnO photocatalyst |
| CN106622205A (en) * | 2016-12-05 | 2017-05-10 | 聊城大学 | Preparation method of perovskite catalyst |
| CN108404971A (en) * | 2018-03-30 | 2018-08-17 | 东北大学秦皇岛分校 | Composite photo-catalyst and the preparation method and application thereof for handling wastewater containing phenol |
| CN111196721A (en) * | 2020-01-13 | 2020-05-26 | 桂林电子科技大学 | La1-xBixFeO3Rare earth ferrite magnetic material and preparation method thereof |
| CN111892093A (en) * | 2020-08-12 | 2020-11-06 | 桂林电子科技大学 | Microwave absorbing material and preparation method thereof |
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| CN104030390A (en) * | 2014-06-04 | 2014-09-10 | 上海应用技术学院 | Method for degrading musk ketone under natural light by utilizing titanium dioxide/charcoal hybrid aerogel |
| CN105080553A (en) * | 2015-08-04 | 2015-11-25 | 内蒙古大学 | Method for preparing stanniferous double-perovskite type phenol photocatalytic degradation catalyst |
| CN105080553B (en) * | 2015-08-04 | 2017-10-27 | 内蒙古大学 | A kind of preparation method of stanniferous double-perovskite type Photocatalytic Degradation of Phenol catalyst |
| CN106040251A (en) * | 2016-06-16 | 2016-10-26 | 内蒙古大学 | Preparation method for sol-gel one-step low-temperature synthesis of pure-phase Bi25F3O40/ZnO photocatalyst |
| CN106622205A (en) * | 2016-12-05 | 2017-05-10 | 聊城大学 | Preparation method of perovskite catalyst |
| CN108404971A (en) * | 2018-03-30 | 2018-08-17 | 东北大学秦皇岛分校 | Composite photo-catalyst and the preparation method and application thereof for handling wastewater containing phenol |
| CN108404971B (en) * | 2018-03-30 | 2020-12-15 | 东北大学秦皇岛分校 | Composite photocatalyst for treating phenol-containing wastewater and preparation method and application thereof |
| CN111196721A (en) * | 2020-01-13 | 2020-05-26 | 桂林电子科技大学 | La1-xBixFeO3Rare earth ferrite magnetic material and preparation method thereof |
| CN111892093A (en) * | 2020-08-12 | 2020-11-06 | 桂林电子科技大学 | Microwave absorbing material and preparation method thereof |
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