CN109529892A - A kind of nano strip MOA composite photo-catalyst preparation method - Google Patents
A kind of nano strip MOA composite photo-catalyst preparation method Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 136
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 27
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 27
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 235000015393 sodium molybdate Nutrition 0.000 claims description 18
- 239000011684 sodium molybdate Substances 0.000 claims description 18
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 17
- 230000035484 reaction time Effects 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000000428 dust Substances 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 7
- 230000002194 synthesizing effect Effects 0.000 claims description 7
- 229910001868 water Inorganic materials 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- YLWSLXWWQRXXMX-UHFFFAOYSA-N [Mo](=O)(=O)=O.[Na] Chemical compound [Mo](=O)(=O)=O.[Na] YLWSLXWWQRXXMX-UHFFFAOYSA-N 0.000 claims 1
- 239000012218 nanoagent Substances 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 abstract description 47
- 238000000034 method Methods 0.000 abstract description 16
- 230000015556 catabolic process Effects 0.000 abstract description 11
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 238000010521 absorption reaction Methods 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 230000008021 deposition Effects 0.000 abstract description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [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 14
- 229940043267 rhodamine b Drugs 0.000 description 14
- 239000000975 dye Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 206010013786 Dry skin Diseases 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000003708 ampul Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
- 229920003081 Povidone K 30 Polymers 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 239000001000 anthraquinone dye Substances 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000031709 bromination Effects 0.000 description 1
- 238000005893 bromination reaction Methods 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
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- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- -1 oxygen ion Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
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- 239000000758 substrate Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 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
- 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
-
- 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/132—Halogens; Compounds thereof with chromium, molybdenum, tungsten or polonium
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- 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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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention discloses a kind of nano strip MOA composite photo-catalyst preparation methods, first pass through microwave-hydro-thermal method and nano strip molybdenum trioxide (MoO is prepared3), then with nano strip molybdenum trioxide (MoO3) it is presoma, using silver nitrate and sodium bromide as raw material, using deionized water as solvent, using polyvinylpyrrolidone as surfactant, on nano strip molybdenum trioxide surface, deposition AgBr nano particle forms heterojunction structure, is synthesized by two-step process to obtain band-like MoO3/ AgBr (MOA) composite photo-catalyst.Step of the present invention is simple, strong operability, stable reaction is controllable, nano strip MOA composite photo-catalyst obtained has suitable band gap, there is good absorption to ultraviolet light, the visible light in sunlight, the energy of sunlight can be made full use of, photocatalysis performance is superior, stability is good, being capable of fast degradation rhdamine B.
Description
Technical field
The present invention relates to a kind of photochemical catalysts, more particularly, to a kind of nano strip MOA composite photo-catalyst preparation method.
Background technique
Since 21 century, the economic progress being skyrocketed through with social civilization, science, offer convenience to our life and
While comfortable, also to we bring it is many it is huge, be difficult to the contradiction coordinated, such as: the deterioration of ecological environment, the energy are withered
It exhausts, the pollution of water resource and shortage etc., these problems are all urgently to be resolved.In recent years, with printing and dyeing, weaving, petroleum
The fast development of industrial and commercial bank's industry, containing be largely difficult to degrade, waste water that organic dyestuff that COD value is high is discharged with these industries into
Enter into nature, seriously affect the living environment of the mankind and aquatile, wherein the waste water that dye industry generates has become
Main pollution source of water body.For pollutant mainly based on azo dyes and anthraquinone dye, feature is exactly good water solubility, biology drop
Solution rate is low, it is difficult to handle, therefore the processing of colored organism is always the difficult point in terms of ring protection in water, processing method is always
It is the emphasis of concern.
The method of processing organic wastewater mainly has at present: (1) physical method: including absorption method, membrane separation technique, extraction
Deng;(2) chemical method: including chemical oxidization method, electrochemical process and photochemical oxidation method etc.;(3) biodegradation method: including aerobic
Biological treatment, Anaerobic biotreatment method etc..In the above method, the advantages of photochemical method, is obvious: (1) energy utilized
From sunlight, chemical energy is converted light energy into;(2) other cocatalysts are not needed in the whole process, can make to contaminate
Material molecule is thoroughly degraded;(3) final product is H2O、CO2Deng other small-molecule substances, secondary dirt will not be caused to water and environment
Dye.
A kind of most common photochemical catalyst is TiO2, with very high stability, nontoxic and abundant raw material is held
Be easy to get to, but its that there are energy bands is excessive, lead to that sunlight cannot be made full use of, in addition the recombination rate mistake of photo-generate electron-hole pairs
Height, the activity and catalysis reaction efficiency that will lead to catalyst reduce.TiO2The two defects limit its business and life
In extensive use.
Summary of the invention
Goal of the invention of the invention is to provide for that a kind of step is simple, and strong operability, stable reaction is controllable, using nothing
The nano strip MOA composite photo-catalyst preparation method that any environmentally harmful solvent is reacted, nano strip obtained
MOA composite photo-catalyst has suitable band gap, has good absorption, Ke Yichong to ultraviolet light, the visible light in sunlight
Divide the energy using sunlight, photocatalysis performance is superior, and stability is good, being capable of fast degradation rhodamine B (RhB) dyestuff.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of nano strip MOA composite photo-catalyst preparation method of the invention, comprising the following steps:
(1) synthesizing nano strip molybdenum trioxide
Sodium molybdate dissolution is obtained into sodium molybdate solution in deionized water, dust technology is being added by molybdic acid in sodium molybdate solution
Sodium solution pH, which is adjusted to being transferred in microwave reactor after 1.9~2.3, to be reacted, and is centrifuged after reaction, isolate difference
It is dry after deionized water, washes of absolute alcohol, obtain nano strip molybdenum trioxide.Crystal form of the reaction condition for molybdenum trioxide
There is large effect, the pattern that can change product influences performance, therefore, by the considered critical to reaction condition, through microwave-
The all more appropriate nano strip molybdenum trioxide (MoO of size, pattern is prepared in hydro-thermal method3), and time-consuming short, reaction condition
Simply, process is stably and controllable.
(2) synthesizing nano strip MOA composite photo-catalyst
In deionized water by the nano strip molybdenum trioxide ultrasonic disperse in step (1), be added polyvinylpyrrolidone,
Silver nitrate is gradually added dropwise excessive sodium bromide solution and is transferred in microwave reactor after being dissolved, being dispersed to be reacted, reaction
After be centrifuged, it is dry after isolate uses deionized water, washes of absolute alcohol respectively, obtain product MOA.With silver nitrate and bromination
Sodium is raw material, and deionized water is solvent, and polyvinylpyrrolidone is surfactant, is deposited on nano strip molybdenum trioxide surface
AgBr nano particle finally obtains nano strip MOA (MoO to form diverse structure3/ AgBr) composite photo-catalyst.
The nano strip MOA composite photo-catalyst that the present invention obtains can be applied to rhodamine B degradation dyestuff (RhB).The band
Shape MoO3/ AgBr (MOA) composite photo-catalyst catalytic degradation dyestuff is roughly divided into following a step: (1) radiation of visible light
Under, MoO3Electron hole pair is generated with AgBr;(2) due to MoO3Heterojunction structure with the matching of AgBr bandedge placement, formation can
So that light induced electron is quickly transferred to MoO from AgBr conduction band3On conduction band, hole is then by MoO3It is transferred in AgBr valence band,
It realizes the separation of photo-generate electron-hole pairs, reduces compound;(3) electronics can generate one of activity in transfer process with dissolved oxygen
Substance negative oxygen ion (O2 -), oxidation dye molecule, hole then can direct oxidation dye molecule generation CO2And H2The small molecules such as O
Product.
Preferably, sodium molybdate solution concentration is 0.1mmol/mL in step (1).
Preferably, dust technology concentration is 4mol/L in step (1).
Preferably, reaction temperature is 130~170 DEG C, reaction time 20min in step (1).
Preferably, isolate uses deionized water, washes of absolute alcohol three times respectively in step (1).
Preferably, drying temperature is 50 DEG C in step (1).
Preferably, in step (2), nano strip molybdenum trioxide, polyvinylpyrrolidone, silver nitrate molar ratio be 1:
1:1。
Preferably, react under dark condition and carry out in step (2), reaction temperature is 50~70 DEG C, and the reaction time is
2~4min.
Preferably, isolate uses deionized water, washes of absolute alcohol three times respectively in step (2).
Therefore, the invention has the following beneficial effects: first pass through microwave-hydro-thermal method nano strip molybdenum trioxide is prepared
(MoO3), then with nano strip molybdenum trioxide (MoO3) it is that presoma is with deionized water using silver nitrate and sodium bromide as raw material
Solvent, using polyvinylpyrrolidone as surfactant, on nano strip molybdenum trioxide surface, deposition AgBr nano particle is formed
Heterojunction structure is synthesized by two-step process to obtain band-like MoO3/ AgBr (MOA) composite photo-catalyst, step is simple, operability
By force, stable reaction is controllable, and nano strip MOA composite photo-catalyst obtained has suitable band gap, to ultraviolet in sunlight
Light, visible light have good absorption, can make full use of the energy of sunlight, and photocatalysis performance is superior, and stability is good, can
Fast degradation rhdamine B.
Detailed description of the invention
Fig. 1 is the nano strip molybdenum trioxide (MoO being prepared in embodiment 13) (a) and nano strip MOA (MoO3/
AgBr) the XRD spectrum of (b) composite photo-catalyst.
Fig. 2 is the nano strip molybdenum trioxide (MoO being prepared in embodiment 13) TEM figure.
Fig. 3 is the nano strip MOA (MoO being prepared in embodiment 13/ AgBr) composite photo-catalyst SEM figure.
Fig. 4 is the nano strip MOA (MoO being prepared in embodiment 13/ AgBr) composite photo-catalyst HR-TEM figure.
Fig. 5 is the nano strip MOA (MoO being prepared in embodiment 13/ AgBr) composite photo-catalyst EDS figure.
Fig. 6 is the nano strip molybdenum trioxide (MoO being prepared in embodiment 13), nano strip MOA (MoO3/AgBr)
The DRS figure (a) and nano strip molybdenum trioxide (MoO of composite photo-catalyst3) band gap calculation figure (b).
Fig. 7 is RhB degradation effect comparison diagram.
Fig. 8 is the nano strip MOA (MoO being prepared in embodiment 13/ AgBr) composite photo-catalyst visible light catalytic
Degradation RhB actual effect figure.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and detailed description.
Embodiment 1
(1) synthesizing nano strip molybdenum trioxide
It is 0.1mmol/mL sodium molybdate solution that 2mmol sodium molybdate, which is dissolved in 20mL deionized water, and obtains concentration, in molybdic acid
It is transferred in microwave reactor and reacts after 4mol/L dust technology is added and adjusts sodium molybdate solution pH to 2 in sodium solution,
Reaction temperature is 160 DEG C, and reaction time 20min is centrifuged after reaction, and isolate uses deionized water, dehydrated alcohol respectively
After cleaning three times, in 50 DEG C of dryings, nano strip molybdenum trioxide is obtained;
(2) MOA is synthesized
By the 1mmol nano strip molybdenum trioxide ultrasonic disperse in step (1) in 100mL deionized water, poly- second is added
Excessive sodium bromide solution is gradually added dropwise in alkene pyrrolidone (PVP-k30), silver nitrate after being dissolved, being dispersed to be transferred to microwave anti-
Answer device to be reacted under dark condition, nano strip molybdenum trioxide, polyvinylpyrrolidone, silver nitrate molar ratio be 1:1:
1, reaction temperature is 60 DEG C, and reaction time 3min is centrifuged after reaction, and isolate uses deionized water, dehydrated alcohol respectively
After cleaning three times, in 50 DEG C of dryings, the band-like MOA (MoO of product nano is obtained3/ AgBr) composite photo-catalyst.
Nano strip MOA (the MoO that the present embodiment obtains3/ AgBr) composite photo-catalyst XRD spectrum it is as shown in Figure 1.Figure
That (b) is represented in 1 is nano strip MOA (MoO3/ AgBr) composite photo-catalyst XRD spectrum, (a) indicate three oxygen of nano strip
Change molybdenum (MoO3) XRD spectrum, with figure (a) compare, figure (b) in obviously there are (111), (200), (220), (222) of AgBr
The characteristic peak of four crystal faces, it was demonstrated that pass through NaBr and AgNO3After reaction, AgBr is successfully supported on band-like-MoO3Surface, the two
It is formed with and is conducive to light-catalysed heterojunction structure.
Nano strip MOA (the MoO that the present embodiment obtains3/ AgBr) composite photo-catalyst TEM figure it is as shown in Figure 2.From figure
It can be clearly seen in 2, the nano strip molybdenum trioxide (MoO that embodiment 1 obtains3) in the banded structure of rule, and surface light
It is sliding, without the product of any other pattern.
Nano strip MOA (the MoO that the present embodiment obtains3/ AgBr) composite photo-catalyst SEM figure it is as shown in Figure 3.From
Fig. 3 can be clearly seen, in nano strip molybdenum trioxide (MoO3) surface adhere to granular AgBr.
Nano strip MOA (the MoO that the present embodiment obtains3/ AgBr) composite photo-catalyst HR-TEM figure it is as shown in Figure 4.
From fig. 4, it can be seen that nano strip molybdenum trioxide (MoO3) and the lattice fringe of AgBr it is interlaced, form heterojunction structure,
The separation and transfer of photogenerated charge can be effectively promoted, photocatalysis efficiency is improved, it is very identical with XRD spectrum result.
Nano strip MOA (the MoO that the present embodiment obtains3/ AgBr) composite photo-catalyst EDS figure it is as shown in Figure 5.From
Fig. 5 can be seen that the nano strip MOA (MoO that embodiment 1 obtains3/ AgBr) in composite photo-catalyst containing all elements (Ag,
Mo, O, Br).The source of C may be the conducting resinl of substrate in figure.
Nano strip molybdenum trioxide (the MoO that the present embodiment obtains3), nano strip MOA (MoO3/ AgBr) composite photocatalyst
The DRS figure (a) and nano strip molybdenum trioxide (MoO of agent3) band gap calculation figure (b) it is as shown in Figure 6.(a) figure can from Fig. 6
To find out, nano strip molybdenum trioxide (MoO3) there is absorption near 420nm, illustrate that it has certain absorption to visible light;From
Plate α-MoO known in the figure (b) of Fig. 63Band gap Eg=2.95eV forms MoO in loaded Ag Br3Absorption after/AgBr is obvious
Move back, ABSORPTION EDGE at 480nm, can responding to visible light, this illustrates MoO3The band gap of/AgBr is relatively narrow, and product pair can be improved
The absorption of visible light, to enhance its visible light catalytic ability.
Nano strip MOA (the MoO that the present embodiment obtains3/ AgBr) composite photocatalyst for degrading RhB effect picture such as Fig. 7
It is shown.From figure 7 it can be seen that the absorption peak of dyestuff is lower and lower with the increase of light application time, the degradation curve in 18min
Already close to level, illustrate nano strip MOA (MoO3/ AgBr) composite photo-catalyst to RhB have good photocatalytic degradation
Efficiency, in 18min i.e. close to degradable RhB dye solution.
To nano strip MOA (MoO obtained in embodiment 13/ AgBr) composite photo-catalyst progress photocatalysis performance survey
Examination, while with nano strip molybdenum trioxide (MoO obtained in embodiment 13) as a comparison case 1, it is received with obtained in embodiment 1
Band-like molybdenum trioxide (the MoO of rice3) and AgBr mixture (MoO3+ AgBr) as a comparison case 2, wherein MoO3+ AgBr by with
Lower step is made: according to step (1) synthesizing nano strip molybdenum trioxide (MoO in embodiment 13), for use;Take the poly- second of 0.6g
Alkene pyrrolidone and 1mmol AgNO3Wherein, after dissolution, dispersion 1h, excessive NaBr is added dropwise in dissolution simultaneously dropwise wherein
Solution reacts 5min in microwave reactor and obtains product, uses deionized water and washes of absolute alcohol 3 times, 50 DEG C of dryings respectively
12h obtains AgBr powder;By AgBr powder and nano strip molybdenum trioxide (MoO3) be uniformly mixed to get MoO3+AgBr。
The specific steps of photocatalysis performance test are as follows:
(1) 30mg sample is weighed, the RhB solution of 30mL is measured in quartz ampoule (concentration of RhB is 15mg/L), by sample
Product are added in quartz ampoule, quartz ampoule are transferred to photochemical reactor, and suspension is stirred 60min in the dark and is guaranteed in room
The lower pollutant of temperature and photochemical catalyst adsorb dissociation equilibrium;
(2) light source is opened, makes radiation of visible light suspension, every 3min, by sample take out it is a small amount of and with centrifuge from
The heart, revolving speed 20000r/min, time 1min, with the sample particle in suspended liquid.The supernatant liquor being centrifuged is taken, is made
Its absorbance is surveyed with ultraviolet-visible spectrophotometer, finally obtains degradation curve.
The RhB solution of any component will be not added with as blank group.
Finally obtained degradation effect is as shown in Figure 8.
As can be seen from Figure 8: (1) nano strip MOA (MoO3/ AgBr) composite photo-catalyst be not nano strip three aoxidize
Molybdenum (MoO3) and AgBr simple combination;(2) blank group the result shows that influence of the visible light to RhB is very small, can ignore
Disregard;(3) nano strip MOA (MoO3/ AgBr) composite photo-catalyst photocatalysis efficiency compared to MoO3And MoO3+ AgBr, all
It is greatly improved, 93% can reach to the degradation of RhB in 18 min.
Embodiment 2
(1) synthesizing nano strip molybdenum trioxide
It is 0.1mmol/mL sodium molybdate solution that 2mmol sodium molybdate, which is dissolved in 20mL deionized water, and obtains concentration, in molybdic acid
It is transferred in microwave reactor and carries out instead after 4mol/L dust technology is added and adjusts sodium molybdate solution pH to 1.9 in sodium solution
It answers, reaction temperature is 130 DEG C, and reaction time 20min is centrifuged after reaction, and isolate uses deionized water, anhydrous second respectively
After alcohol cleaning three times, in 50 DEG C of dryings, nano strip molybdenum trioxide is obtained;
(2) MOA is synthesized
By the 1mmol nano strip molybdenum trioxide ultrasonic disperse in step (1) in 100mL deionized water, poly- second is added
Excessive sodium bromide solution is gradually added dropwise in alkene pyrrolidone (PVP K30), silver nitrate after being dissolved, being dispersed to be transferred to microwave anti-
Answer device to be reacted under dark condition, nano strip molybdenum trioxide, polyvinylpyrrolidone, silver nitrate molar ratio be 1:1:
1, reaction temperature is 60 DEG C, and reaction time 3min is centrifuged after reaction, and isolate uses deionized water, dehydrated alcohol respectively
After cleaning three times, in 50 DEG C of dryings, the band-like MOA (MoO of product nano is obtained3/ AgBr) composite photo-catalyst.
Embodiment 3
(1) synthesizing nano strip molybdenum trioxide
It is 0.1mmol/mL sodium molybdate solution that 2mmol sodium molybdate, which is dissolved in 20mL deionized water, and obtains concentration, in molybdic acid
It is transferred in microwave reactor and carries out instead after 4mol/L dust technology is added and adjusts sodium molybdate solution pH to 2.3 in sodium solution
It answers, reaction temperature is 170 DEG C, and reaction time 20min is centrifuged after reaction, and isolate uses deionized water, anhydrous second respectively
After alcohol cleaning three times, in 50 DEG C of dryings, nano strip molybdenum trioxide is obtained;
(2) MOA is synthesized
By the 1mmol nano strip molybdenum trioxide ultrasonic disperse in step (1) in 100mL deionized water, poly- second is added
Excessive sodium bromide solution is gradually added dropwise in alkene pyrrolidone (PVP K30), silver nitrate after being dissolved, being dispersed to be transferred to microwave anti-
Answer device to be reacted under dark condition, nano strip molybdenum trioxide, polyvinylpyrrolidone, silver nitrate molar ratio be 1:1:
1, reaction temperature is 60 DEG C, and reaction time 3min is centrifuged after reaction, and isolate uses deionized water, dehydrated alcohol respectively
After cleaning three times, in 50 DEG C of dryings, the band-like MOA (MoO of product nano is obtained3/ AgBr) composite photo-catalyst.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (9)
1. a kind of nano strip MOA composite photo-catalyst preparation method, which comprises the following steps: (1) synthesize nanometer
Band-like molybdenum trioxide
Sodium molybdate dissolution is obtained into sodium molybdate solution in deionized water, it is in addition dust technology that sodium molybdate is molten in sodium molybdate solution
Liquid pH, which is adjusted to being transferred in microwave reactor after 1.9~2.3, to be reacted, and is centrifuged after reaction, isolate is spent respectively
It is dry after ionized water, washes of absolute alcohol, obtain nano strip molybdenum trioxide;(2) synthesizing nano strip MOA composite photo-catalyst
In deionized water by the nano strip molybdenum trioxide ultrasonic disperse in step (1), polyvinylpyrrolidone, nitric acid is added
Silver is gradually added dropwise excessive sodium bromide solution and is transferred in microwave reactor after being dissolved, being dispersed to be reacted, and reaction terminates
After be centrifuged, it is dry after isolate uses deionized water, washes of absolute alcohol respectively, obtain the band-like MOA composite photocatalyst of product nano
Agent.
2. a kind of nano strip MOA composite photo-catalyst preparation method according to claim 1, which is characterized in that step
(1) in, sodium molybdate solution concentration is 0.1mmol/mL.
3. a kind of nano strip MOA composite photo-catalyst preparation method according to claim 1, which is characterized in that step
(1) in, dust technology concentration is 4mol/L.
4. a kind of nano strip MOA composite photo-catalyst preparation method according to claim 1, which is characterized in that step
(1) in, reaction temperature is 130~170 DEG C, reaction time 20min.
5. a kind of nano strip MOA composite photo-catalyst preparation method according to claim 1, which is characterized in that step
(1) in, isolate uses deionized water, washes of absolute alcohol three times respectively.
6. a kind of nano strip MOA composite photo-catalyst preparation method according to claim 1, which is characterized in that step
(1) in, drying temperature is 50 DEG C.
7. a kind of nano strip MOA composite photo-catalyst preparation method according to claim 1, which is characterized in that step
(2) in, nano strip molybdenum trioxide, polyvinylpyrrolidone, silver nitrate molar ratio be 1:1:1.
8. a kind of nano strip MOA composite photo-catalyst preparation method according to claim 1, which is characterized in that step
(2) it in, reacts under dark condition and carries out, reaction temperature is 50~70 DEG C, and the reaction time is 2~4min.
9. a kind of nano strip MOA composite photo-catalyst preparation method according to claim 1, which is characterized in that step
(2) in, isolate uses deionized water, washes of absolute alcohol three times respectively.
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CN115041182A (en) * | 2022-07-12 | 2022-09-13 | 重庆大学 | Magnetic ternary composite photocatalyst In-MoO 3 /SrFe 12 O 19 Preparation method of (1) |
CN115364848A (en) * | 2022-07-12 | 2022-11-22 | 重庆大学 | Strip-shaped composite photocatalyst In-MoO 3 Preparation method of (1) |
CN116046726A (en) * | 2023-01-28 | 2023-05-02 | 云南民族大学 | Silver nanoparticle modified molybdenum trioxide nanocomposite, preparation method and application thereof |
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CN111617781A (en) * | 2020-07-10 | 2020-09-04 | 福州大学 | Z-shaped composite photocatalyst of molybdenum bronze hydride coated with zinc indium sulfide and preparation method and application thereof |
CN111617781B (en) * | 2020-07-10 | 2022-11-15 | 福州大学 | Z-shaped composite photocatalyst of molybdenum bronze hydride coated with zinc indium sulfide and preparation method and application thereof |
CN115041182A (en) * | 2022-07-12 | 2022-09-13 | 重庆大学 | Magnetic ternary composite photocatalyst In-MoO 3 /SrFe 12 O 19 Preparation method of (1) |
CN115364848A (en) * | 2022-07-12 | 2022-11-22 | 重庆大学 | Strip-shaped composite photocatalyst In-MoO 3 Preparation method of (1) |
CN115364848B (en) * | 2022-07-12 | 2023-06-09 | 重庆大学 | Stripe-shaped composite photocatalyst In-MoO 3 Is prepared by the preparation method of (2) |
CN115041182B (en) * | 2022-07-12 | 2023-06-09 | 重庆大学 | Magnetic ternary composite photocatalyst In-MoO 3 /SrFe 12 O 19 Is prepared by the preparation method of (2) |
CN116046726A (en) * | 2023-01-28 | 2023-05-02 | 云南民族大学 | Silver nanoparticle modified molybdenum trioxide nanocomposite, preparation method and application thereof |
CN116046726B (en) * | 2023-01-28 | 2023-12-08 | 云南民族大学 | Preparation method of silver nanoparticle modified molybdenum trioxide nanocomposite |
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