CN108273534A - A kind of wolframic acid antimony is modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst - Google Patents
A kind of wolframic acid antimony is modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst Download PDFInfo
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- CN108273534A CN108273534A CN201711479425.5A CN201711479425A CN108273534A CN 108273534 A CN108273534 A CN 108273534A CN 201711479425 A CN201711479425 A CN 201711479425A CN 108273534 A CN108273534 A CN 108273534A
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 84
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 42
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 42
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 239000002253 acid Substances 0.000 title claims abstract description 32
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 32
- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 5
- 229940012189 methyl orange Drugs 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical group [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 241000258920 Chilopoda Species 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 241000270322 Lepidosauria Species 0.000 description 1
- 241000239226 Scorpiones Species 0.000 description 1
- 241000271897 Viperidae Species 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000016768 molybdenum Nutrition 0.000 description 1
- 239000000178 monomer 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
- 239000010865 sewage Substances 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- 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
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- 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
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- 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
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- 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
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- 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
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- 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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- Hydrology & Water Resources (AREA)
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Abstract
The preparation method for being modified three nitrogen of class graphene carbon, four composite photo-catalyst the invention discloses a kind of wolframic acid antimony and its application in photocatalytic pollutant degradation, belong to material preparation and light-catalysed technical field.The characteristics of catalyst, has：Shape characteristic with 2 dimensions, by the g C of the particle modified 2 dimension structure of wolframic acid antimony3N4It is combined.During preparing photochemical catalyst, using calcination method and hydro-thermal method simple for process, synthesizes wolframic acid antimony and be modified three nitrogen of class graphene carbon, four composite photo-catalyst.Under the action of wolframic acid antimony, wolframic acid antimony is modified three nitrogen of class graphene carbon, four composite photo-catalyst and shows good photocatalysis performance, promotes novel semi-conductor g C3N4The research of photochemical catalyst.
Description
Technical field
The invention belongs to materials synthesis and photocatalysis technology field, relates generally to a kind of wolframic acid antimony and be modified class graphene carbon three
The preparation of four composite photo-catalyst of nitrogen and photocatalytic activity research.
Background technology
With industrialized development, the problem of environmental pollution, becomes increasingly severe.How problem of environmental pollution is solved, at
The hot spot in investigation of materials field.
TiO was found for the first time from 19722Since photocatalytic activity, photocatalysis technology just receives people and widely closes
Note.The advantages that photocatalysis technology is by its energy conservation and environmental protection, non-secondary pollution provides an extraordinary solution for the processing of sewage
Certainly approach.Conductor photocatalysis material, which can utilize in inexhaustible, nexhaustible solar energy processing air or in water, to be had
Malicious harmful substance improves environment, achievees the purpose that utilization of resources ecology.Currently, a variety of different semiconductor light photochemical catalysts
Material is widely studied, such as zinc oxide, g-C3N4Deng.But three nitrogen four of class graphene carbon is extensive by its material source, synthesizes work
One of the thermoelectric material that the advantages that skill is simple, and the five poisonous creatures: scorpion, viper, centipede, house lizard, toad are pollution-free is studied as photocatalysis.
But there is also some defects for three nitrogen of class graphene carbon, four catalyst, for example, it obtains light induced electron-with high
Hole-recombination rate, this seriously inhibits its further development and applications.In this background, class graphene carbon how is improved
The photocatalysis efficiency of three nitrogen four, at the research emphasis of three nitrogen of class graphene carbon, four photochemical catalyst.Up to now, there are many sides
Method is used, such as:Pattern control, semiconductors coupling etc..But the photocatalysis efficiency of three nitrogen four of class graphene carbon, stability with
And Reusability in practical applications is still difficult to meet the needs of practical application.
In recent years, compound using other materials and the progress of three nitrogen of class graphene carbon, four catalyst, prepare composite photo-catalyst
Research make some progress, irradiation following table of obtained three nitrogen of class graphene carbon, four base composite photocatalyst in sunlight
Reveal good photocatalytic activity.The present invention carried out with three nitrogen four of class graphene carbon using wolframic acid antimony it is compound, formed wolframic acid antimony change
Three nitrogen of property class graphene carbon, four composite photo-catalyst, is effectively improved the visible light catalysis activity of three nitrogen four of class graphene carbon.
Invention content
The purpose of the present invention is prepare three nitrogen of class graphene carbon with high visible light utilization efficiency and high catalytic activity
Four base composite photocatalysts, and its catalytic cycle stability is high, promotes the practical application of three nitrogen four of class graphene carbon.
Purpose adopts the following technical scheme that realize the present invention：
Three nitrogen four of class graphene carbon is prepared by calcination method, hydro-thermal reaction is then utilized, on three nitrogen of class graphene carbon, four surface
Wolframic acid antimony nano-particle is loaded, wolframic acid antimony is finally prepared and is modified three nitrogen of class graphene carbon, four composite photo-catalyst.In wolframic acid antimony
Under the action of, improve the visible light catalysis activity of three nitrogen four of class graphene carbon.
A kind of wolframic acid antimony is modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst, and characterization step is as follows：
（1）Appropriate dicyanodiamine is added in crucible, is heated in high temperature process furnances, g-C3N4 is made；
（2）2g g-C3N4 are taken to be dissolved in 40mL ethylene glycol solutions；
（3）To step（2）Appropriate SbCl is added in solution3, stir evenly；
（4）A certain amount of Na is added into (3) solution2WO6, stir evenly；
（5）20 mL water are added to (4) solution, stir evenly；
（6）The solution being stirred is transferred in autoclave and is reacted；
（7）By the sample centrifuge washing that the reaction was complete, is ground after dry and obtain composite photo-catalyst.
SbCl in step (3)3Quality be 0.9125g.
Na in step (4)2WO6Quality is 0.066g.
Reaction temperature is 180 DEG C in step (6), reaction time 20h.
Eccentric cleaning process in step (5) is first to be cleaned 4 times with ethyl alcohol, then clean 2 times with deionized water, centrifugation rate
8000rpm, time 6min.
A kind of wolframic acid antimony is modified three nitrogen of class graphene carbon, four composite photo-catalyst for organic pollution in aqueous solution
Visible light photocatalytic degradation.
Target contaminant is methyl orange solution.
The invention has the advantages that：
1. prepared by the present invention is that wolframic acid antimony is modified three nitrogen of class graphene carbon, four composite photo-catalyst, belong to new compound system；
2. the wolframic acid antimony in the present invention, which is modified three nitrogen of class graphene carbon, four composite photo-catalyst, has good photocatalytic activity,
Catalytic activity is in g-C3N4Have on the basis of monomer and is obviously improved.Decline by the irradiation of the artificial visible light sources of 90min retired
Base orange dyestuff, degradation reach 90%, and catalytic activity more light-catalysed than three four/silver oxide of nitrogen of class graphene carbon is 1.5 times high.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph that wolframic acid antimony is modified three nitrogen of class graphene carbon, four composite photo-catalyst.
Fig. 2 is the photocatalytic degradation figure that wolframic acid antimony is modified three nitrogen of class graphene carbon, four composite photo-catalyst.
Specific implementation mode
A kind of wolframic acid antimony is modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst, and characterization step is as follows：
（1）Appropriate dicyanodiamine is added in crucible, is heated in high temperature process furnances, g-C3N4 is made；
（2）2gg-C3N4 is taken to be dissolved in 40mL ethylene glycol solutions；
（3）To step（2）Appropriate SbCl is added in solution3, stir evenly；
（4）A certain amount of Na is added into (3) solution2WO6, stir evenly；
（5）20mL water is added to (4) solution, stirs evenly；
（6）The solution being stirred is transferred in autoclave and is reacted；
（7）By the sample centrifuge washing that the reaction was complete, is ground after dry and obtain composite photo-catalyst.
SbCl in step (3)3Quality be 0.9125g.
Na in step (4)2WO6Quality is 0.066g.
Reaction temperature is 180 DEG C in step (6), reaction time 20h.
Eccentric cleaning process in step (5) is first to be cleaned 4 times with ethyl alcohol, then clean 2 times with deionized water, centrifugation rate
8000rpm, time 6min.
A kind of wolframic acid antimony is modified three nitrogen of class graphene carbon, four composite photo-catalyst for organic pollution in aqueous solution
Visible light photocatalytic degradation.
Specific examples of the implementation prepares wolframic acid antimony and is modified three nitrogen of class graphene carbon, four composite photo-catalyst below.
Case study on implementation 1
Wolframic acid antimony is modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst
A certain amount of dicyanodiamine powder is weighed with crucible, is put into high temperature process furnances, is heated with the heating rate of 5 DEG C/min
To 550 DEG C, 4h is kept the temperature, g-C is finally obtained3N4Yellow powder.Take 2g g-C3N4, it is dissolved in 40mL ethylene glycol solutions, stirring is equal
It is even；Weigh 0.9125g SbCl3In solution, stir evenly；It is subsequently added into 0.066g Na2WO6Powder continues magnetic agitation；,
It is added in 20 mL deionized waters to above-mentioned solution, magnetic agitation；Then solution is poured into reaction kettle, is heated, heating temperature is
180 DEG C, time 20h.After the completion of reaction, centrifuge washing is first cleaned 4 times with ethyl alcohol, is being washed with water 2 times, and centrifugal speed is
8000rpm, time 6min.60 DEG C of dryings in last baking oven, it is multiple that grinding obtains wolframic acid antimony modification class three nitrogen four of graphene carbon
Closing light catalyst.
Case study on implementation 2
Wolframic acid antimony is modified four composite photo-catalyst of class graphene carbon three nitrogen and degrades under visible light illumination methyl orange
It is modified three nitrogen of class graphene carbon, four composite photo-catalyst by two selenizing molybdenums made from 1 method of case study on implementation and carries out degradation methyl
Orange experiment.The concentration of methyl orange solution is 1 × 10-5mol L-1；Composite material powder 50mg is taken, the above-mentioned methyl oranges of 100mL are placed in
It in solution, stirs 60 minutes in darkroom, is then placed in solution in the visible light source that ultraviolet light is filtered, take within every 10 minutes
5mL methyl orange solutions measure the characteristic peaks of methyl orange in solution with ultraviolet-visible spectrophotometer.
Wolframic acid antimony, which is obtained, by case study on implementation 2 is modified three nitrogen of class graphene carbon, four composite photo-catalyst Visible Light Induced Photocatalytic methyl orange
Degradation curve, see Fig. 2.The composite material powder that as can be seen from Figure 2 prepared by case study on implementation 1 is catalyzed drop after illumination 90min
Solution reaches 90% or more, shows high catalytic activity.
Claims (5)
1. a kind of wolframic acid antimony is modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst, feature includes the following steps：
（1）Appropriate dicyanodiamine is added in crucible, is heated in high temperature process furnances, g-C is made3N4；
（2）Take 2g g-C3N4It is dissolved in 40mL ethylene glycol solutions；
（3）To step（2）Appropriate SbCl is added in solution3, stir evenly；
（4）A certain amount of Na is added into (3) solution2WO6, stir evenly；
（5）20mL water is added to (4) solution, stirs evenly；
（6）The solution being stirred is transferred in autoclave and is reacted；
（7）By the sample centrifuge washing that the reaction was complete, is ground after dry and obtain composite photo-catalyst.
2. being modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst according to a kind of wolframic acid antimony of claim 1, feature exists
In SbCl3Quality be 0.9125g.
3. being modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst according to a kind of wolframic acid antimony of claim 1, feature exists
In Na2WO6Quality be 0.066g.
4. being modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst according to a kind of wolframic acid antimony of claim 1, feature exists
In preparation reaction temperature be 180 DEG C, reaction time 20h.
5. being modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst according to a kind of wolframic acid antimony of claim 1, feature exists
In composite catalyst pattern be two g-C3N4Piece loads wolframic acid antimony nano-particle.
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| CN201711479425.5A CN108273534A (en) | 2017-12-29 | 2017-12-29 | A kind of wolframic acid antimony is modified the preparation of three nitrogen of class graphene carbon, four composite photo-catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114100658A (en) * | 2021-11-23 | 2022-03-01 | 湖南农业大学 | Carbon nitride/tungsten trioxide/sulfur-doped antimony oxychloride double-Z-shaped composite photocatalyst and preparation method and application thereof |
| CN115722248A (en) * | 2022-11-17 | 2023-03-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Tungsten disulfide-graphite phase carbon nitride composite photocatalyst and preparation method and application thereof |
-
2017
- 2017-12-29 CN CN201711479425.5A patent/CN108273534A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114100658A (en) * | 2021-11-23 | 2022-03-01 | 湖南农业大学 | Carbon nitride/tungsten trioxide/sulfur-doped antimony oxychloride double-Z-shaped composite photocatalyst and preparation method and application thereof |
| CN114100658B (en) * | 2021-11-23 | 2023-09-12 | 湖南农业大学 | Carbon nitride/tungsten trioxide/sulfur doped antimony oxychloride double-Z-type composite photocatalyst, and preparation method and application thereof |
| CN115722248A (en) * | 2022-11-17 | 2023-03-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Tungsten disulfide-graphite phase carbon nitride composite photocatalyst and preparation method and application thereof |
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Application publication date: 20180713 |