CN108479829A - A kind of preparation of N doping Zinc vanadate photochemical catalyst - Google Patents

A kind of preparation of N doping Zinc vanadate photochemical catalyst Download PDF

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Publication number
CN108479829A
CN108479829A CN201711484368.XA CN201711484368A CN108479829A CN 108479829 A CN108479829 A CN 108479829A CN 201711484368 A CN201711484368 A CN 201711484368A CN 108479829 A CN108479829 A CN 108479829A
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China
Prior art keywords
photochemical catalyst
zinc vanadate
preparation
doping
doping zinc
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Pending
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CN201711484368.XA
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Chinese (zh)
Inventor
马开梅
何平伟
张松利
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Xinghua Precision Casting And Forging Industry Research Institute Co Ltd
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Xinghua Precision Casting And Forging Industry Research Institute Co Ltd
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Priority to CN201711484368.XA priority Critical patent/CN108479829A/en
Publication of CN108479829A publication Critical patent/CN108479829A/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
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24Nitrogen compounds
    • 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
    • B01J37/08Heat 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
    • 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)
  • Toxicology (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Catalysts (AREA)

Abstract

The application in field is administered the invention discloses the preparation method of N doping Zinc vanadate photochemical catalyst and its in environmental contaminants, belongs to material preparation and photocatalysis research field.The characteristics of catalyst, has:Doped energy-band with nitrogen adjusts the forbidden band structure of Zinc vanadate.During preparing photochemical catalyst, using calcination method simple for process, synthesize N doping Zinc vanadate photochemical catalyst.Under N doping effect, N doping Zinc vanadate photochemical catalyst shows high photocatalysis performance, promotes the application of Zinc vanadate photochemical catalyst.

Description

A kind of preparation of N doping Zinc vanadate photochemical catalyst
Technical field
The invention belongs to the preparation of material and its photocatalysis technology fields, relate generally to a kind of N doping Zinc vanadate photocatalysis The preparation of agent and its research of photocatalytic activity.
Background technology
With the enhancing of people's environmental protection consciousness, the problem of water pollution, has received more and more attention.Traditional dirt Method for treating water can not meet the requirement of people.A kind of cleaning is searched out, efficiently, energy-saving and environment-friendly sewage water treatment method, The hot spot direction studied at people.
TiO was found for the first time from 19722Since photocatalytic activity, the research of photocatalysis technology is always Material Field Hot spot direction.Photocatalysis technology by its energy conservation and environmental protection, non-secondary pollution the advantages that for sewage processing provide one it is non- Often good solution route.Conductor photocatalysis material can utilize in inexhaustible, nexhaustible solar energy processing air or Poisonous and harmful substance in person's water improves environment, achievees the purpose that utilization of resources ecology.Currently, a variety of different semiconductor lights Photocatalyst material is widely studied, such as ZnO, g-C3N4Deng, but Zinc vanadate is extensive by its material source, cheap, nothing The hot spot material that the advantages that bio-toxicity is studied as photocatalysis.
But there is also some defects for Zinc vanadate photochemical catalyst, for example, sun light utilization efficiency is low;Absorption to substrate of degrading Poor performance;Quantum efficiency is relatively low, and with high that photo-generate electron-hole recombination rate, these defects all hinder its reality Using.In this background, how to improve the photocatalysis efficiency of Zinc vanadate and widen its photophase range, urged at Zinc vanadate light The research emphasis of agent.
In recent years, element doping is modified method acquisition people and widely pays close attention to.The present invention utilizes ammonia, is made in calcination process For N doping Zinc vanadate is gone out, it is effectively improved the visible light utilization efficiency and photocatalytic activity of Zinc vanadate.
Invention content
The purpose of the present invention is preparing the Zinc vanadate photochemical catalyst with high visible light utilization efficiency and high catalytic activity, And its catalytic cycle stability is high, promotes the practical application of Zinc vanadate.
Purpose adopts the following technical scheme that realize the present invention:
Using ammonia as nitrogen source, the Zinc vanadate of N doping is prepared in calcination process.Under the action of N doping, vanadic acid is improved The visible light catalysis activity of zinc.
A kind of preparation of N doping Zinc vanadate photochemical catalyst, characterization step are as follows:
(1)It weighs a certain amount of zinc sulfate to be dissolved in 50mL ethyl alcohol, stir evenly;
(2)It weighs a certain amount of ammonium metavanadate to be dissolved in above-mentioned solution, magnetic agitation is uniform;
(3)By step(2)Solution carries out centrifuge washing, and drying is placed in tube furnace;
(4)It is calcined under ammonia atmosphere, obtains N doping Zinc vanadate photochemical catalyst.
Zinc sulfate quality is 0.69g, a concentration of 13.8g/L in step (1).
Ammonium metavanadate quality is 0.186 g, a concentration of 3.72g/L in step (2).
Calcination temperature is 350 DEG C in step (4), reaction time 2h.
Eccentric cleaning process in step (3) is first to be cleaned 4 times with ethyl alcohol, then clean 2 times with deionized water, centrifugation rate 10000rpm, time 6min.
The N doping Zinc vanadate photochemical catalyst is used for the visible light photocatalytic degradation of organic pollution in aqueous solution.
Target contaminant is rhodamine B.
The invention has the advantages that:
1. preparation method of the present invention prepares the preparation of N doping Zinc vanadate photochemical catalyst using calcination method, belong to new Photochemical catalyst;
2. the N doping Zinc vanadate photochemical catalyst in the present invention has good photocatalytic activity, catalytic activity is in Zinc vanadate On the basis of have and be obviously improved.It degrades under the irradiation of the artificial visible light sources of 90min rhdamine B, palliating degradation degree reaches 45%, it is 2 times of Zinc vanadate catalytic activity.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of N doping Zinc vanadate photochemical catalyst.
Fig. 2 is the photocatalytic degradation figure of N doping Zinc vanadate photochemical catalyst.
Specific implementation mode
A kind of preparation of N doping Zinc vanadate photochemical catalyst, characterization step are as follows:
(1)It weighs a certain amount of zinc sulfate to be dissolved in 50mL ethyl alcohol, stir evenly;
(2)It weighs a certain amount of ammonium metavanadate to be dissolved in above-mentioned solution, magnetic agitation is uniform;
(3)By step(2)Solution carries out centrifuge washing, and drying is placed in tube furnace;
(4)It is calcined under ammonia atmosphere, obtains N doping Zinc vanadate photochemical catalyst.
Zinc sulfate quality is 0.69g, a concentration of 13.8g/L in step (1).
Ammonium metavanadate quality is 0.186 g, a concentration of 3.72g/L in step (2).
Calcination temperature is 350 DEG C in step (4), reaction time 2h.
Eccentric cleaning process in step (3) is first to be cleaned 4 times with ethyl alcohol, then clean 2 times with deionized water, centrifugation rate 10000rpm, time 6min.
The N doping Zinc vanadate photochemical catalyst is used for the visible light photocatalytic degradation of organic pollution in aqueous solution.
Examples of implementation are enumerated below prepares N doping Zinc vanadate photochemical catalyst.
Case study on implementation 1
A kind of preparation of N doping Zinc vanadate photochemical catalyst.
0.69g zinc sulfate is weighed in 50mL ethyl alcohol, is stirred evenly;0.186g ammonium metavanadates are subsequently added into, magnetic force is continued Stirring;After the completion of reaction, centrifuge washing is first cleaned 4 times with ethyl alcohol, is being washed with water 2 times, centrifugal speed 8000rpm, and the time is 6min.60 DEG C of dryings in last baking oven.Obtained powder is placed in tube furnace, with 5 DEG C/min's under the protection of ammonia gas Heating rate is heated to 350 DEG C, keeps the temperature 2h, finally obtains N doping Zinc vanadate photochemical catalyst.
Case study on implementation 2
N doping Zinc vanadate photochemical catalyst rhodamine B degradation under visible light illumination.
Rhodamine B degradation experiment is carried out by N doping Zinc vanadate photochemical catalyst made from 1 method of case study on implementation.Rhodamine B The concentration of solution is 1 × 10-5mol L-1;Composite material powder 50mg is taken, is placed in the above-mentioned rhodamine B solutions of 100mL, dark It stirs 60 minutes in room, is then placed in solution in the visible light source that ultraviolet light is filtered, take 5mL rhodamine Bs within every 10 minutes Solution measures the characteristic peaks of rhodamine B in solution with ultraviolet-visible spectrophotometer.
The degradation curve of N doping Zinc vanadate photochemical catalyst Visible Light Induced Photocatalytic rhodamine B is obtained by case study on implementation 2, sees Fig. 2. The photochemical catalyst powder that as can be seen from Figure 2 prepared by case study on implementation 1 catalytic degradation after illumination 90min reaches 45%, shows more High photocatalytic activity.

Claims (5)

1. a kind of preparation of N doping Zinc vanadate photochemical catalyst, feature include the following steps:
(1)It weighs a certain amount of zinc sulfate to be dissolved in 50mL ethyl alcohol, stir evenly;
(2)It weighs a certain amount of ammonium metavanadate to be dissolved in above-mentioned solution, magnetic agitation is uniform;
(3)By step(2)Solution carries out centrifuge washing, and drying is placed in tube furnace;
(4)It is calcined under ammonia atmosphere, obtains N doping Zinc vanadate photochemical catalyst.
2. according to a kind of preparation of N doping Zinc vanadate photochemical catalyst of claim 1, it is characterised in that step(1)Middle zinc sulfate matter Amount is 0.69g, a concentration of 13.8g/L.
3. according to a kind of preparation of N doping Zinc vanadate photochemical catalyst of claim 1, it is characterised in that step(2)Middle ammonium metavanadate Quality be 0.186 g, a concentration of 3.72g/L.
4. according to a kind of preparation of N doping Zinc vanadate photochemical catalyst of claim 1, it is characterised in that step(4)Middle calcination temperature It is 350 DEG C, reaction time 2h, and is carried out under the protection of ammonia.
5. according to a kind of preparation of N doping Zinc vanadate photochemical catalyst of claim 1, it is characterised in that step(4)Calcination process In, complete N doping using ammonia.
CN201711484368.XA 2017-12-29 2017-12-29 A kind of preparation of N doping Zinc vanadate photochemical catalyst Pending CN108479829A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114335578A (en) * 2022-01-06 2022-04-12 齐鲁工业大学 Zinc vanadate electrocatalytic material and preparation method and application thereof
CN114534715A (en) * 2022-02-28 2022-05-27 商河县谱安检测技术中心 Formaldehyde purifying agent

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114335578A (en) * 2022-01-06 2022-04-12 齐鲁工业大学 Zinc vanadate electrocatalytic material and preparation method and application thereof
CN114335578B (en) * 2022-01-06 2023-07-25 齐鲁工业大学 Zinc vanadate electrocatalytic material and preparation method and application thereof
CN114534715A (en) * 2022-02-28 2022-05-27 商河县谱安检测技术中心 Formaldehyde purifying agent
CN114534715B (en) * 2022-02-28 2022-11-25 浙江会众环境工程有限公司 Formaldehyde purifying agent

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Application publication date: 20180904