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 PDFInfo
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- 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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- Prior art keywords
- photochemical catalyst
- zinc vanadate
- preparation
- doping
- doping zinc
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000011701 zinc Substances 0.000 title claims abstract description 42
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 42
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 7
- 229960001763 zinc sulfate Drugs 0.000 claims description 7
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 7
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 15
- 238000007146 photocatalysis Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000000356 contaminant Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 10
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 8
- 229940043267 rhodamine b Drugs 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- 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
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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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
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711484368.XA CN108479829A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation of N doping Zinc vanadate photochemical catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711484368.XA CN108479829A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation of N doping Zinc vanadate photochemical catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108479829A true CN108479829A (en) | 2018-09-04 |
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|---|---|---|---|
| CN201711484368.XA Pending CN108479829A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation of N doping Zinc vanadate photochemical catalyst |
Country Status (1)
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| CN (1) | CN108479829A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114335578A (en) * | 2022-01-06 | 2022-04-12 | 齐鲁工业大学 | A kind of 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 |
-
2017
- 2017-12-29 CN CN201711484368.XA patent/CN108479829A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114335578A (en) * | 2022-01-06 | 2022-04-12 | 齐鲁工业大学 | A kind of zinc vanadate electrocatalytic material and preparation method and application thereof |
| CN114335578B (en) * | 2022-01-06 | 2023-07-25 | 齐鲁工业大学 | A zinc vanadate electrocatalytic material and its preparation method and application |
| 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 |