CN109317133A - A kind of microwave synthesis method of niobium pentaoxide/nano titania compound photochemical catalyst - Google Patents
A kind of microwave synthesis method of niobium pentaoxide/nano titania compound photochemical catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 42
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000001308 synthesis method Methods 0.000 title claims abstract description 5
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 title description 4
- -1 titania compound Chemical class 0.000 title description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012153 distilled water Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000002244 precipitate Substances 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000010189 synthetic method Methods 0.000 claims 8
- 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 claims 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 12
- 238000003786 synthesis reaction Methods 0.000 abstract description 12
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 238000006731 degradation reaction Methods 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000007146 photocatalysis Methods 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 235000021050 feed intake Nutrition 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 14
- 239000010955 niobium Substances 0.000 description 12
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 9
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 229910011006 Ti(SO4)2 Inorganic materials 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 5
- 239000006260 foam Substances 0.000 description 5
- 239000002114 nanocomposite Substances 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 description 5
- 235000011152 sodium sulphate Nutrition 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 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 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 229910000484 niobium oxide Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000005303 weighing 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J37/34—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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- 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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Abstract
The invention discloses a kind of Nb2O5/TiO2The microwave synthesis method of nano-complex photochemical catalyst, comprising the following steps: (1) disperse lauryl sodium sulfate in distilled water, Ti (SO is added4)2And it is uniformly dispersed to obtain mixed liquor A；(2) by Nb2O5, urea be added in mixed liquor A, be uniformly dispersed to obtain mixed liquid B；(3) mixed liquid B is heated to reaction under microwave, cooling obtains mixed liquor C after fully reacting；(4) supernatant liquor of mixed liquor C is discarded into reservation subnatant, then is centrifugated washing and is precipitated；(5) washing of precipitate is drying to obtain.Beneficial effects of the present invention: (1) being synthesized by the way of microwave heating, and aggregate velocity is fast, the time is short；(2) primary raw material used in is Ti (SO4)2, inexpensive, easy transport and storage；(3) photochemical catalyst synthesized by does not need to be heat-treated, and simplifies processing step；(4) directly feed intake synthesis, saves cost；(5) photocatalysis performance of the catalyst synthesized by is fabulous, and degradation rate is up to 95.50% in 50min.
Description
Technical field
The invention belongs to photochemical catalysts to synthesize field, and in particular to a kind of Nb2O5/TiO2Nano-complex photochemical catalyst
Microwave synthesis method.
Background technique
In recent years, niobium oxide and Nb5+The TiO of doping2Photocatalysis research, which is presented, enlivens trend, such as Nb2O5Light is urged
Change Oxidation of Alcohol, chitosan-Nb2O5Compound photocatalytic degradation of dye, mesoporous Nb2O5The preparation of photocatalysis Decomposition methanol aqueous solution
Hydrogen, Ti-Nb composite oxides decompose water under ultraviolet and visible optical radiation and decompose acetone etc. under visible light.With TiO2
It compares, niobium oxide has good compatibility to the organic matter in gas phase and water body environment, it is ensured that photochemical catalyst is multiple
To the adsorption capacity of organic matter under miscellaneous catalytic condition, promote the depth degradation of organic matter.
Nb at present2O5-TiO2What the synthesis of composite oxides used has coprecipitation, high temperature solid phase synthesis etc..Above-mentioned side
Have the disadvantage in that segregation problems existing for coprecipitation perplex always researcher in method；High temperature solid phase synthesis high energy consumption,
The problem of coarse grains, could not solve always.
Summary of the invention
In order to solve the above technical problems, synthesizing Nb using microwave the present invention provides a kind of2O5/TiO2Nano combined object light
The method of catalyst.This method reaction speed is fast, the nanometer that reaction condition is mild, efficiency is high, the time is short, at low cost, prepared
Complex catalyst catalytic performance is fabulous.
Innovation of the invention is: one, using the synthesis that directly feeds intake, all raw materials once put into reaction, simple fast
Cost is saved in victory；Two, using microwave synthesising reacting speed is fast, efficiency is high, the time is short, synthesis is only needed 20 minutes；Three, master used
Wanting raw material is Ti (SO4)2, cheap and easy to get, easily keeping is transported, and storage uses safe；Four, synthesized photochemical catalyst does not need heat
Processing directly uses；Five, the photocatalysis performance of synthesized photochemical catalyst is fabulous, is that simulation is dirty with 20mg/L methyl orange solution
Object is contaminated, in 20mg/L methyl orange solution, catalyst amount 1.8g/L, with the Photocatalytic Activity for Degradation of 400nm or more,
Degradation rate is up to 95.50% in 50min.
Technical solution provided by the invention is as follows:
A kind of Nb2O5/TiO2The microwave synthesis method of nano-complex photochemical catalyst, which is characterized in that including following step
It is rapid:
(1) it disperses lauryl sodium sulfate in distilled water, Ti (SO is added4)2And it is uniformly dispersed to obtain mixed liquor A；
(2) by Nb2O5, urea be added in mixed liquor A, be uniformly dispersed to obtain mixed liquid B；
(3) mixed liquid B is heated to reaction under microwave, cooling obtains mixed liquor C after fully reacting；
(4) supernatant liquor of mixed liquor C is discarded into reservation subnatant, then is centrifugated washing and is precipitated；
(5) washing of precipitate is drying to obtain.
Every 1g lauryl sodium sulfate is dissolved in 100ml distilled water in above-mentioned steps (1), and Ti (SO is added4)2Amount be
2.4g。
Dispersing method is ultrasonic disperse in above-mentioned steps (1).
Nb in above-mentioned steps (2)2O5With TiO2Molar ratio be 1~2:1, preferably 1.3~1.7:1
Using every 1g lauryl sodium sulfate as reference in above-mentioned steps (2), amount of urea 5.0g.
It is 650W that the power of microwave, which is the power of microwave, in above-mentioned steps (3), and service intermittent is that a job follows with 30s
Ring, work 12s, stops 18s；Heating time is 20min.
Cleaning solvent includes distilled water and acetone in above-mentioned steps (5).
Drying temperature is 60 DEG C in above-mentioned steps (5), drying time 8h.
Beneficial effects of the present invention:
(1) it is synthesized by the way of microwave heating, synthesising reacting speed is fast, efficiency is high, the time is short, and synthesis only needs 20
Minute；
(2) primary raw material used in is Ti (SO4)2, cheap and easy to get, easily keeping is transported, and storage uses safe；
(3) photochemical catalyst synthesized by does not need to be heat-treated, and directly uses, and simplifies processing step；
(4) using the synthesis that directly feeds intake, all raw materials disposably put into reaction, simple and fast, save cost；
(5) photocatalysis performance of the photochemical catalyst synthesized by is fabulous, using 20mg/L methyl orange solution as simulating pollution object,
In 20mg/L methyl orange solution, catalyst amount 1.8g/L, with the Photocatalytic Activity for Degradation of 400nm or more, the interior drop of 50min
Solution rate is up to 95.50%.
Detailed description of the invention
Fig. 1 is Nb2O5And Nb2O5/TiO2X-ray diffractogram；
Fig. 2 is Nb2O5/TiO2The field emission scanning electron microscope figure of nanocomposite samples；
Fig. 3 is Nb2O5/TiO2Visible absorption spectra figure of the nano-complex photochemical catalyst for methyl orange solution of degrading；
Fig. 4 is different feed ratios to Nb2O5/TiO2The curve that nanocomposite photocatalytic degradation influences；
Fig. 5 is different catalysts dosage to Nb2O5/TiO2The curve that nanocomposite photocatalytic degradation influences.
Specific embodiment
The present invention will be described combined with specific embodiments below, and the contents of the present invention are completely without being limited thereto.
Embodiment 1
Nb2O5/TiO2The synthesis of nano-complex photochemical catalyst
1.0g lauryl sodium sulfate (SDS) is weighed in 100mL distilled water and ultrasonic disperse is to being completely dissolved, is added
2.4g Ti(SO4)2Into above-mentioned solution, ultrasonic disperse dissolves, by Nb2O5: TiO2Molar ratio is that 1.5:1 is accurately weighed centainly
The Nb of amount2O5To in above-mentioned solution, 5.0g urea ultrasonic disperse is added, is transferred in round-bottomed flask.It installs reflux unit and connects
Condensed water, using 650W microwave intermittent-heating, with 30s for a working cycles, work 12s, stops 18s, microwave heating
20min, then cooled to room temperature, supernatant liquor is outwelled, take subnatant be transferred in centrifuge tube be centrifugated and with steaming
Distilled water is washed to non-foam, then by product dehydrate and is transferred in small beaker with acetone.Vacuum drying (60 DEG C) 8h obtains nanometer
Compound photochemical catalyst.
Embodiment 2
Nb2O5/TiO2The synthesis of nano-complex photochemical catalyst
1.0g lauryl sodium sulfate (SDS) is weighed in 100mL distilled water and ultrasonic disperse is to being completely dissolved, is added
2.4g Ti(SO4)2Into above-mentioned solution, ultrasonic disperse dissolves, by Nb2O5: TiO2Molar ratio accurately weighs a certain amount of for 1:1
Nb2O5To in above-mentioned solution, 5.0g urea ultrasonic disperse is added, is transferred in round-bottomed flask.It installs reflux unit and connects cold
Condensate, using 650W microwave intermittent-heating, with 30s for a working cycles, work 12s, stops 18s, microwave heating 20min,
Then cooled to room temperature outwells supernatant liquor, takes subnatant to be transferred to centrifuge separation in centrifuge tube and is washed with distillation
It washs to non-foam, then by product dehydrate and is transferred in small beaker with acetone.Vacuum drying (60 DEG C) 8h obtains nano-complex
Photochemical catalyst.
Embodiment 3
Nb2O5/TiO2The synthesis of nano-complex photochemical catalyst
1.0g lauryl sodium sulfate (SDS) is weighed in 100mL distilled water and ultrasonic disperse is to being completely dissolved, is added
2.4g Ti(SO4)2Into above-mentioned solution, ultrasonic disperse dissolves, by Nb2O5: TiO2Molar ratio is that 1.3:1 is accurately weighed centainly
The Nb of amount2O5To in above-mentioned solution, 5.0g urea ultrasonic disperse is added, is transferred in round-bottomed flask.It installs reflux unit and connects
Condensed water, using 650W microwave intermittent-heating, with 30s for a working cycles, work 12s, stops 18s, microwave heating
20min, then cooled to room temperature, supernatant liquor is outwelled, take subnatant be transferred in centrifuge tube be centrifugated and with steaming
Distilled water is washed to non-foam, then by product dehydrate and is transferred in small beaker with acetone.Vacuum drying (60 DEG C) 8h obtains nanometer
Compound photochemical catalyst.
Embodiment 4
Nb2O5/TiO2The synthesis of nano-complex photochemical catalyst
1.0g lauryl sodium sulfate (SDS) is weighed in 100mL distilled water and ultrasonic disperse is to being completely dissolved, is added
2.4g Ti(SO4)2Into above-mentioned solution, ultrasonic disperse dissolves, by Nb2O5: TiO2Molar ratio is that 1.7:1 is accurately weighed centainly
The Nb of amount2O5To in above-mentioned solution, 5.0g urea ultrasonic disperse is added, is transferred in round-bottomed flask.It installs reflux unit and connects
Condensed water, using 650W microwave intermittent-heating, with 30s for a working cycles, work 12s, stops 18s, microwave heating
20min, then cooled to room temperature, supernatant liquor is outwelled, take subnatant be transferred in centrifuge tube be centrifugated and with steaming
Distilled water is washed to non-foam, then by product dehydrate and is transferred in small beaker with acetone.Vacuum drying (60 DEG C) 8h obtains nanometer
Compound photochemical catalyst.
Embodiment 5
Nb2O5/TiO2The synthesis of nano-complex photochemical catalyst
1.0g lauryl sodium sulfate (SDS) is weighed in 100mL distilled water and ultrasonic disperse is to being completely dissolved, is added
2.4g Ti(SO4)2Into above-mentioned solution, ultrasonic disperse dissolves, by Nb2O5: TiO2Molar ratio accurately weighs a certain amount of for 2:1
Nb2O5To in above-mentioned solution, 5.0g urea ultrasonic disperse is added, is transferred in round-bottomed flask.It installs reflux unit and connects cold
Condensate, using 650W microwave intermittent-heating, with 30s for a working cycles, work 12s, stops 18s, microwave heating 20min,
Then cooled to room temperature outwells supernatant liquor, takes subnatant to be transferred to centrifuge separation in centrifuge tube and is washed with distillation
It washs to non-foam, then by product dehydrate and is transferred in small beaker with acetone.Vacuum drying (60 DEG C) 8h obtains nano-complex
Photochemical catalyst.
Embodiment 6
The form and morphology characterization of nano-complex photochemical catalyst prepared by embodiment 1
(1) XRD analysis: it will be seen from figure 1 that in Nb2O5/TiO2Only there is Nb in nano-complex spectrogram2O5Spy
Diffraction maximum is levied, does not find TiO substantially2Characteristic peak, it may be possible to due to TiO2Micro-and nano-particles are highly dispersed in Nb2O5In lattice
Caused by portion.And Nb2O5/TiO2The characteristic diffraction peak of nano-complex is than pure Nb2O5Characteristic diffraction peak want weak, illustrate TiO2Partly lead
Bluk recombination is modified to reduce Nb to a certain extent2O5The degree of order.
(2) SEM is characterized: figure it is seen that the Nb of preparation2O5/TiO2The piece of layered laminate is shown in nano-complex
Shape structure.
Application Example 1
Nb2O5/TiO2Photocatalysis performance test
Test method: accurately weighing a certain amount of sample in 20mg/L methyl orange solution, ultrasonic disperse, and it is flat to be protected from light absorption
Weigh 30min.0.25mL H is added2O2As initiator, visible light light of the xenon lamp of 350W as Photocatalytic Degradation On Methyl Orange Solution
Source (optical filter filters 400nm light below), sample liquid level to xenon source outlet height are about that 14cm carries out photocatalytic degradation,
Every the absorbance of 10~20min, 6~8mL of centrifuging and taking supernatant liquor measurement of ultraviolet-visible spectrophotometer methyl orange solution,
Until sample solution absorbance no longer declines.
Degradation rate calculates: Dt=(A0-At)/A0 × 100%
In formula: methyl orange originates absorbance when A0 is without photocatalytic degradation；
At is the absorbance after methyl orange degradation t min.
Fig. 3 is Nb2O5/TiO2Nano-complex photochemical catalyst dosage is 1.8g/L degradation 50mL 20mg/L methyl orange solution
Visible absorption spectra figure.As can be seen from the figure after 50min radiation of visible light, the absorbance of solution no longer declines, drop
Solution rate has reached 95.50%, illustrates Nb prepared by embodiment 12O5/TiO2Nano-complex is good photochemical catalyst.
Fig. 4 is different feed ratios to Nb2O5/TiO2The curve that nanocomposite photocatalytic degradation influences, respectively using real
It applies catalyst prepared by a 1-5 and carries out catalytic degradation.We are available from figure works as Nb2O5: TiO2Molar ratio is
1.5:1 when photocatalysis effect it is best.Feed ratio is excessive or too small little on its final photocatalytic activity influence, but when catalysis
Between but differ greatly.When practical feed ratio is lower than optimum charging ratio, with the increase of feed ratio, Nb2O5Participate in capture and release
The ability in light induced electron and hole enhances to influence in the service life in light induced electron and hole, to enhance TiO2Photocatalytic activity.Work as reality
When border feed ratio is higher than optimum charging ratio, since the concentration of ion is excessive there is a possibility that in TiO2Inside reaches saturation and generates new
Phase reduces TiO2Effective surface area, to reduce photocatalysis efficiency.
Fig. 5 shows different catalysts dosage to Nb2O5/TiO2The curve that nanocomposite photocatalytic degradation influences, is adopted
It is catalyst prepared by embodiment 1.As can be seen from the figure the dosage of catalyst to final degradation rate height almost
Do not influence, it is main to influence catalysis time length.Wherein when catalyst amount is about 1.8g/L, photocatalytic degradation compared with
The high and used time is most short.In a certain range, when catalyst amount is less, with its photocatalysis of the increase of catalyst amount
Activity gradually rises.When catalyst reaches certain dosage, catalyst is since gravity is easy to be deposited on bottom, instead
It is unfavorable for the progress of light-catalyzed reaction.
The foregoing is only a preferred embodiment of the present invention, but the scope of protection of the invention be not limited thereto,
Any modification that anyone skilled in the art is made in the technical scope disclosed by the present invention, equivalent replacement and
Improve etc., it should be included within the protection scope of invention.
Claims (9)
1. a kind of Nb2O5/TiO2The microwave synthesis method of nano-complex photochemical catalyst, which comprises the following steps:
(1) it disperses lauryl sodium sulfate in distilled water, Ti (SO is added4)2And it is uniformly dispersed to obtain mixed liquor A；
(2) by Nb2O5, urea be added in mixed liquor A, be uniformly dispersed to obtain mixed liquid B；
(3) mixed liquid B is heated to reaction under microwave, cooling obtains mixed liquor C after fully reacting；
(4) supernatant liquor of mixed liquor C is discarded into reservation subnatant, then is centrifugated washing and is precipitated；
(5) washing of precipitate is drying to obtain.
2. synthetic method according to claim 1, it is characterised in that: every 1g lauryl sodium sulfate in the step (1)
It is dissolved in 100ml distilled water, Ti (SO is added4)2Amount be 2.4g.
3. synthetic method according to claim 1 or 2, it is characterised in that: dispersing method is ultrasound point in the step (1)
It dissipates.
4. synthetic method according to claim 1, it is characterised in that: Nb in the step (2)2O5With TiO2Molar ratio
For 1~2:1.
5. synthetic method according to claim 4, it is characterised in that: Nb in the step (2)2O5With TiO2Molar ratio
For 1.3~1.7:1.
6. synthetic method according to claim 1, it is characterised in that: with every 1g dodecyl sulphate in the step (2)
Sodium is reference, amount of urea 5.0g.
7. synthetic method according to claim 1, it is characterised in that: the power of microwave is 650W in the step (3),
Formula of having a rest work is with 30s for a working cycles, and work 12s, stops 18s；Heating time is 20min.
8. synthetic method according to claim 1, it is characterised in that: cleaning solvent includes distilled water in the step (5)
And acetone.
9. synthetic method according to claim 1, it is characterised in that: drying temperature is 60 DEG C in the step (5), dry
Time is 8h.
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