CN107185521A - A kind of catalysis material and preparation method thereof - Google Patents

A kind of catalysis material and preparation method thereof Download PDF

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Publication number
CN107185521A
CN107185521A CN201710356041.8A CN201710356041A CN107185521A CN 107185521 A CN107185521 A CN 107185521A CN 201710356041 A CN201710356041 A CN 201710356041A CN 107185521 A CN107185521 A CN 107185521A
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China
Prior art keywords
catalysis material
preparation
sodium tungstate
mixed solution
washed
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CN201710356041.8A
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Inventor
张雅恒
黄金城
翟任凯
李建鑫
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Yangcheng Institute of Technology
Yancheng Institute of Technology
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Yangcheng Institute of Technology
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Priority to CN201710356041.8A priority Critical patent/CN107185521A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts 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
    • B01J23/24Chromium, molybdenum or tungsten
    • B01J23/31Chromium, molybdenum or tungsten combined with bismuth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02Impregnation, coating or precipitation
    • B01J37/03Precipitation; Co-precipitation
    • B01J37/031Precipitation
    • B01J37/033Using Hydrolysis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/40Organic compounds containing sulfur
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Catalysts (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention provides a kind of catalysis material and preparation method thereof, the molecular formula of the catalysis material is Pr/Bi2WO6, Pr and Bi mol ratio are 0.5 2.0:100;Its preparation method is first to add to sodium tungstate to obtain sodium tungstate solution in deionized water, praseodymium nitrate and bismuth nitrate is added to mixed solution is obtained in deionized water;Under agitation, sodium tungstate solution is added drop-wise in mixed solution, obtains milky suspension, and adjust pH to 2, be subsequently placed in autoclave, reacted;The pale yellow precipitate that reaction is produced is collected, is washed with deionized, then is washed with absolute ethyl alcohol, dries, that is, obtains catalysis material.The catalysis material of the present invention is the Bi after loose structure, doping Pr2WO6Red shift occurs for ABSORPTION EDGE, and the utilization rate to visible ray is improved.

Description

A kind of catalysis material and preparation method thereof
Technical field
The invention belongs to catalysis material technical field, and in particular to a kind of catalysis material responded with high visible And preparation method thereof.
Background technology
In recent years, semiconductor light-catalyst is received due to its application potential in terms of environmental improvement and solar energy conversion Extensive concern.In these semiconductors, because bismuth tungstate(Bi2WO6)The band gap of relative narrower, under visible light illumination with good Good photocatalysis performance and be proved to be most promising semiconductor catalyst.
Bi2WO6It is a kind of Ca-Ti ore type semiconductor, the electron transition that is stimulated after illumination produces electron hole pair, electron hole To redox ability it is extremely strong, easily occur redox reaction with organic matter and high-molecular compound.Bi2WO6Forbidden band Width is 2.75ev,, can quilt in W atom 5d tracks formation conduction band in 6s and O atom 2p hybridized orbit the formation valence band of Bi atoms Excited by visible light, can have higher photocatalytic activity under visible light.
Find in actual applications, pure Bi2WO6The photo-generate electron-hole recombination rate of catalyst is higher, and electron hole is not yet Just it has been combined when producing free radical, has made the reduction of its photocatalytic activity.Rare earth element has the energy level enriched and 4f electron transitions Characteristic, is also easy to produce polyelectron configuration, there is special optical property, in Photocatalyst and construction novel photocatalyst system Aspect has good application.In Bi2WO6The middle appropriate rare earth element of doping, in effectively reduction semiconductor photoproduction electron-hole recombinations On the basis of, the utilization rate of carrier is improved, optimizes Bi2WO6Photocatalytic activity, have good effect.
The content of the invention
The technical problem of solution:It is an object of the invention to prepare it is a kind of with high visible respond catalysis material and Its preparation method.
Technical scheme:A kind of catalysis material, its molecular formula is Pr/Bi2WO6, Pr and Bi mol ratio are 0.5-2.0: 100。
Further, the crystal structure of the catalysis material is the (Bi by being alternately present2O2)2+Layer and it is octahedral (WO6)6-Accumulation is formed.
The preparation method of above-mentioned catalysis material, comprises the following steps:
Step 1, sodium tungstate is added to and sodium tungstate solution is obtained in deionized water, praseodymium nitrate and bismuth nitrate are added in deionized water Obtain mixed solution;
Step 2, under agitation, sodium tungstate solution is added drop-wise in mixed solution, obtains milky suspension, and adjust pH To 2;
Step 3, step 2 gained mixed solution is placed in autoclave, reacted;
Step 4, the pale yellow precipitate that reaction is produced is collected, be washed with deionized, then washed with absolute ethyl alcohol, dried, produce To catalysis material.
Further, nitre acid for adjusting pH is used in step 2.
Further, in step 3 reaction temperature be 120-200 DEG C, the time be 12h.
Further, drying condition is 60 DEG C, 6h in step 4.
Beneficial effect:
1. the catalysis material of the present invention is loose structure, the Bi after doping Pr2WO6Red shift occurs for ABSORPTION EDGE, to visible ray Utilization rate is improved;
2. Pr doping is 1%, Pr/Bi2WO6The energy gap of sample is 2.56eV, wider than the forbidden band undoped with sample Degree narrows, degradation rate highest;
3. raw material is cheap, prepare simply, it is all very environmentally friendly when preparing and using.
Brief description of the drawings
The Pr/Bi that Fig. 1 is different doping Pr in embodiment 12WO6UV-vis DRS collection of illustrative plates;
The Pr/Bi that Fig. 2 is different doping Pr in embodiment 12WO6The influence of photocatalytic degradation methylene blue.
Embodiment
Embodiment 1
Step 1, the sodium tungstate for weighing 2.5mmol is dissolved in 15mL deionized waters, weighs a certain amount of praseodymium nitrate and bismuth nitrate It is dissolved in 50mL deionized waters and forms mixed solution(The molar percentage of praseodymium and bismuth is respectively 0%, 0.5%, 1.0%, 1.5%, 2.0%, tungsten:Praseodymium+bismuth=1:2);
Step 2, under continuous stirring, sodium tungstate solution is slowly dropped in mixed solution, obtains milky suspension, be used in combination Nitre acid for adjusting pH value is to 2;
Step 3, step 2 gained mixed solution is placed in 100mL autoclaves, reactor loading is 70% or so, Room temperature is cooled to after reacting 12h at a temperature of 120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C;
Step 4, the pale yellow precipitate that reaction is produced is collected, washs for several times, is done in 60 DEG C of baking oven through deionized water and ethanol Dry 6 hours, obtain Pr/Bi2WO6
As shown in figure 1, present invention gained Pr/Bi2WO6Red shift occurs for ABSORPTION EDGE;It is computed obtaining, when Pr doping is When 1%, Pr/Bi2WO6Energy gap be 2.56eV.
Performance test
The methylene blue solution for preparing 10mg/L makees target degradation product, and light source is used as using 500W mercury lamps.Weigh 25mg Pr/ Bi2WO6Add in 100mL methylene blue solutions, first darkroom is stirred 0.5 hour, system is reached that adsorption-desorption is balanced.
Lamp source is opened, a sample was taken every 25 minutes, 5mL is extracted every time, and is removed with centrifuge after suspended particulate, to molten Liquid carries out absorbance test.
As shown in Fig. 2 present invention gained Pr/Bi2WO6It is higher to the degradation rate of visible ray;When Pr doping is 1%, Pr/Bi2WO6Degradation rate highest.

Claims (6)

1. a kind of catalysis material, it is characterised in that:Molecular formula is Pr/Bi2WO6, Pr and Bi mol ratio are 0.5-2.0:100.
2. catalysis material according to claim 1, it is characterised in that:The crystal structure of the catalysis material is by handing over For (the Bi of appearance2O2)2+Layer and octahedral (WO6)6-Accumulation is formed.
3. the preparation method of the catalysis material described in claim 1, it is characterised in that:Comprise the following steps:
Step 1, sodium tungstate is added to and sodium tungstate solution is obtained in deionized water, praseodymium nitrate and bismuth nitrate are added in deionized water Obtain mixed solution;
Step 2, under agitation, sodium tungstate solution is added drop-wise in mixed solution, obtains milky suspension, and adjust pH To 2;
Step 3, step 2 gained mixed solution is placed in autoclave, reacted;
Step 4, the pale yellow precipitate that reaction is produced is collected, be washed with deionized, then washed with absolute ethyl alcohol, dried, produce To catalysis material.
4. the preparation method of catalysis material according to claim 3, it is characterised in that:Adjusted in step 2 using nitric acid pH。
5. the preparation method of catalysis material according to claim 3, it is characterised in that:Reaction temperature is in step 3 120-200 DEG C, the time be 12h.
6. the preparation method of catalysis material according to claim 3, it is characterised in that:Drying condition is 60 in step 4 ℃、6h。
CN201710356041.8A 2017-05-19 2017-05-19 A kind of catalysis material and preparation method thereof Pending CN107185521A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107983336A (en) * 2017-12-11 2018-05-04 湖北大学 A kind of praseodymium doped bismuth tungstate light urges agent and preparation method thereof
CN108355646A (en) * 2017-12-29 2018-08-03 盐城工学院 A kind of preparation method of bismuth based compound nano-photocatalyst

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103638923A (en) * 2013-09-12 2014-03-19 陕西科技大学 Rare earth element Nd-doped Bi2WO6 composite photocatalyst, preparation method therefor and applications thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103638923A (en) * 2013-09-12 2014-03-19 陕西科技大学 Rare earth element Nd-doped Bi2WO6 composite photocatalyst, preparation method therefor and applications thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CHUNYING WANG等: ""Photocatalytic degradation of two different types of dyes by synthesized La/Bi2WO6"", 《RSC ADVANCES》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107983336A (en) * 2017-12-11 2018-05-04 湖北大学 A kind of praseodymium doped bismuth tungstate light urges agent and preparation method thereof
CN108355646A (en) * 2017-12-29 2018-08-03 盐城工学院 A kind of preparation method of bismuth based compound nano-photocatalyst
CN108355646B (en) * 2017-12-29 2021-04-06 盐城工学院 Preparation method of bismuth compound nano photocatalyst

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Application publication date: 20170922

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