CN105771957A - Bismuth niobate porous microspheres with photocatalytic activity and ultrasonic atomizing preparation method thereof - Google Patents
Bismuth niobate porous microspheres with photocatalytic activity and ultrasonic atomizing preparation method thereof Download PDFInfo
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- CN105771957A CN105771957A CN201610165257.1A CN201610165257A CN105771957A CN 105771957 A CN105771957 A CN 105771957A CN 201610165257 A CN201610165257 A CN 201610165257A CN 105771957 A CN105771957 A CN 105771957A
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 53
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 25
- 239000004005 microsphere Substances 0.000 title abstract 4
- 239000002243 precursor Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 150000001621 bismuth Chemical class 0.000 claims abstract description 10
- 239000012159 carrier gas Substances 0.000 claims abstract description 10
- 150000002821 niobium Chemical class 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000011148 porous material Substances 0.000 claims description 30
- 150000003839 salts Chemical class 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000003595 mist Substances 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000000889 atomisation Methods 0.000 claims description 2
- ANERHPOLUMFRDC-UHFFFAOYSA-K bismuth citrate Chemical class [Bi+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O ANERHPOLUMFRDC-UHFFFAOYSA-K 0.000 claims description 2
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 27
- 239000000463 material Substances 0.000 description 11
- 238000006731 degradation reaction Methods 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000000356 contaminant Substances 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 239000011941 photocatalyst Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- KKMOSYLWYLMHAL-UHFFFAOYSA-N 2-bromo-6-nitroaniline Chemical compound NC1=C(Br)C=CC=C1[N+]([O-])=O KKMOSYLWYLMHAL-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- ZMQLNDRNRHUWBB-UHFFFAOYSA-N niobium;oxalic acid;hydrate Chemical compound O.[Nb].OC(=O)C(O)=O ZMQLNDRNRHUWBB-UHFFFAOYSA-N 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 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
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 1
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000005620 antiferroelectricity Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- PMVFCJGPQOWMTE-UHFFFAOYSA-N bismuth calcium Chemical compound [Ca].[Bi] PMVFCJGPQOWMTE-UHFFFAOYSA-N 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health 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
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 230000000280 vitalizing effect Effects 0.000 description 1
Classifications
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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
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
-
- B01J35/39—
-
- B01J35/40—
-
- B01J35/51—
-
- B01J35/60—
-
- 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
- B01J37/343—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 ultrasonic wave energy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/06—Polluted air
Abstract
The invention discloses bismuth niobate porous microspheres with photocatalytic activity and an ultrasonic atomizing preparation method thereof. The preparation method include the steps of firstly, mixing and dissolving bismuth salt and niobium salt, and acidifying with an appropriate amount of nitric acid solution to form a clear precursor solution; secondly, adding the clear precursor solution obtained the first step into the liquid containing cup of an ultrasonic atomizer for atomizing so as to allow the precursor solution of bismuth niobate to exist in a small fog drop form; thirdly, feeding the fog drops obtained in the second step into the heating reaction area of a tube furnace through carrier gas for reaction, absorbing the reaction products with cold water, and drying to obtain the bismuth niobate porous microspheres. The preparation method has the advantages that by the precise control of raw material use amount and ultrasonic atomizing conditions, the bismuth niobate porous microspheres with coarse and porous surfaces and with the average diameter being 1-3 micrometers are obtained; the preparation method is simple in process, easy to control, low in cost and easy to achieve large-scale production.
Description
Technical field
The present invention relates to the preparation of a kind of Inorganic Non-metallic Materials with photocatalytic activity, particularly relate to a kind of bismuth niobate multi-pore micron ball with photocatalytic activity and preparation method thereof.
Background technology
Along with the raising of environmental consciousness, in recent years to environmental protection, save the aspect such as the energy and energy conversion and had and widely pay close attention to.Photochemical catalyst is applied to the numerous areas such as photolysis water hydrogen, the degraded of organic pollution, material automatically cleaning, the depollution of environment and medical and health as a kind of advanced new forms of energy.Compared with many types of catalyst, it is regarded as a kind of high-efficiency environment friendly and cost savings type catalyst.In field of environment pollution control, photocatalysis is that one can be realized the emerging technology that in environment, multiple poisonous and harmful substance is efficiently removed by living radical produced by solar energy vitalizing semiconductor, had broad application prospects.Titanium dioxide has been obtained for studying widely as first generation semiconductor light-catalyst, but can only irradiate at ultraviolet light because of its band gap length and just can be excited;And the electron hole produced easily is combined, causing quantum efficiency relatively low, greatly affect its photocatalytic activity, its application is subject to certain restrictions.Therefore, exploitation preparation process is easy, be catalyzed the high heterojunction photocatalyst of activity has important practical significance.
Many studies have shown that, bismuth based compound has preferable visible light catalysis activity, becomes the study hotspot of photocatalysis environmental area instantly.Prepare KNb at present3O18、Bi5Nb3O15、BiNbO4、Bi2MNbO7、Bi2WO6、BiVO4、Bi2MoO6Deng bismuth series photocatalyst.BiNbO4It is a kind of microwave-medium ceramics received much concern in recent years, there is the advantages such as high-k, low-loss, low-temperature coefficient.BiNbO4There is low form α-BiNbO4With high temperature modification β-
BiNbO4Two kinds of crystal structures.α- BiNbO4Belonging to orthorhombic system, Bi and Nb forms the octahedron of distortion with oxygen, and octahedra connected by four corners, total is considered as by by Bi3+Multilayer [the NbO that ion is separated4]3-One-element group is formed.β- BiNbO4Structural aberration degree bigger, there is anti-ferroelectricity and ferroelasticity.Low-temperature phase α-BiNbO4At 1020 DEG C can stable existence, when exceeding this temperature occur irreversible transition become three monoclinic phases.
Chinese patent CN101948310A is by transition metal element doped entrance bismuth calcium niobate ceramic material so that it is piezoelectric property improves a lot than the piezoelectric property of unadulterated bismuth niobate calcium pottery.Chinese patent CN103936418A uses solid phase method to prepare A position lithium, cerium (Li, Ce), bismuth niobate calcium (CBN) ceramic powder material of the different doping in B position tungsten (W), this ceramic material prepared at relatively low sintering temperature (～1100) DEG C, its crystal grain is dense, crystal grain uniform, improves the compactness of sintering activity and pottery so that sintering effect is more preferable, and piezoelectric property is greatly improved, and reduce its dielectric loss.The nanometer bismuth niobate photocatalyst prepared is supported on LSA900C type synthetic resin by Chinese patent CN102294271A, and the synthetic resin loaded nanometer bismuth niobate photocatalyst catalytic efficiency prepared is high, catalysis activity is big, load fastness is strong and service life is long.
The most relevant BiNbO4Material is few at the report of photocatalysis field.Conventional method many employings solid reaction process and coprecipitation prepare BiNbO4Material.But solid reaction process needs roasting at very high temperatures, consume energy higher, and the BiNbO that two kinds of methods obtain4Material all presents the pattern that sheet-like particle is mutually assembled, and the specific surface area causing gained sample is the least.Along with the increase of sintering temperature, sample is gradually changed to compact texture by open structure so that the specific surface area that sample is little continues to decline, and affects its photocatalysis performance.In order to better profit from the Photocatalytic Degradation Property of bismuth niobate, researcher develops the bismuth niobate material of diverse microcosmic structure, specific surface area and optical characteristics, but rarely has the bismuth niobate of report chondritic.The material obtained by conventional method still cannot overcome the reunion of bismuth niobate particle, causes light degradation ability to decline.
Summary of the invention
First purpose of the present invention is to provide that a kind of preparation technology is reasonable, controlled, quick, environmental protection and have the bismuth niobate multi-pore micron ball preparation method with photocatalytic activity of continuous prodution power.
Second object of the present invention is to provide a kind of by being precisely controlled the consumption of raw material and supersonic spraying condition, it is thus achieved that rough surface porous, the bismuth niobate multi-pore micron ball system with photocatalytic activity of average diameter 1-3um.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that:
The ultrasonic atomizatio preparation method of a kind of bismuth niobate multi-pore micron ball with photocatalytic activity, it is characterised in that comprise the following steps:
Step1: the preparation of the precursor solution of bismuth niobate salt: bismuth salt is mixed with niobium salt and is dissolved in deionized water, the bismuth salt wherein added and the mol ratio of niobium salt are 1:1～1:5, it is acidified to PH=1～3, room temperature 18 DEG C to 25 DEG C stirring 1～3 h with salpeter solution, forms precursor solution；
Step2: the atomization of the precursor solution of bismuth niobate salt: the precursor solution of the bismuth niobate salt obtained by Step1 is added in the liquid holding cup of ultrasonic atomizer carry out making mist, after ultrasonic atomizatio, make the precursor solution of bismuth niobate presented in little droplet, wherein ultrasonic frequency 1.7MHz ± 10%, condensation rate is 0.1～1L/h；
Step3: the production of bismuth niobate micron ball and collection: using air as carrier gas, the precursor solution droplet obtained by Step2 adds thermal reaction area 600～1000 DEG C by what tube furnace was sent in carrier gas, reacting, obtain product and absorbed by cooling down water, wherein flow rate of carrier gas is 10～70L/min.
Specifically, in described Step1, bismuth salt is five nitric hydrate bismuth or bismuth citrates, and the mol ratio of bismuth salt and niobium salt is 1:1～1:5.
Specifically, in Step1, with salpeter solution, precursor solution is acidified to PH=1～3.
Specifically, in Step2, the condensation rate of ultrasonic atomizatio is 0.1～1L/h.
Specifically, in Step3, the heating reaction zone temperature of tube furnace is 600～1000 DEG C, and atmospheric carrier air flow velocity is 10～70L/min.
Specifically, in Step3, the bismuth niobate multi-pore micron ball obtained is directly to be collected by water.
The invention have benefit that:
(1) by being precisely controlled the consumption of raw material and ultrasonic atomizatio method condition, it is thus achieved that rough surface porous, the bismuth niobate multi-pore micron ball of average diameter 1-3um；
(2) supersonic spraying preparation technology of the present invention is simple, it is easy to control, with low cost, it is easy to large-scale production, and bismuth niobate micron ball is obvious to the degradation effect of gaseous contaminant, has broad prospect of application in terms of air contaminant treatment.
Accompanying drawing explanation
Fig. 1 is the degradation rate-light application time curve of the photocatalytic degradation removal NO of the bismuth niobate micron ball of the embodiment of the present invention 1 to embodiment 3 preparation；
Fig. 2 is SEM (SEM) photo of the bismuth niobate multi-pore micron ball of the embodiment of the present invention 2 preparation.
Detailed description of the invention
The present invention will be further described below in conjunction with the accompanying drawings.
Embodiment
1
Step1: mix in the deionized water being dissolved in 50 mL by 2.0mmol bismuth citrate with the oxalic acid hydrate niobium of 10.0mmol, be acidified to PH=3 with appropriate salpeter solution, is stirred at room temperature 1h, forms precursor solution；
Step2: Step1 gained precursor solution is transferred to carry out making mist in the liquid holding cup of ultrasonic atomizer, after ultrasonic atomizatio, make the precursor solution of bismuth niobate presented in little droplet；
Step3: sending in the constant tube furnace of heating-up temperature with carrier gas stream for the precursor solution droplet that Step2 is obtained by 70L/min air, the droplet of precursor solution reacts through adding thermal reaction area (temperature is 1000 DEG C), product is absorbed by water and obtains.
Products therefrom is BiNbO after testing4。
Embodiment
2
Step1: mix in the deionized water being dissolved in 50 mL by 2.0mmol bismuth citrate with the oxalic acid hydrate niobium of 2.0mmol, be acidified to PH=1 with appropriate salpeter solution, is stirred at room temperature 30min, forms precursor solution；
Step2: Step1 gained precursor solution is transferred to carry out making mist in the liquid holding cup of ultrasonic atomizer, after ultrasonic atomizatio, make the precursor solution of bismuth niobate presented in little droplet；
Step3: sending in the constant tube furnace of heating-up temperature with carrier gas stream for the precursor solution droplet that Step2 is obtained by 10L/min air, the droplet of precursor solution reacts through adding thermal reaction area (temperature is 900 DEG C), product is absorbed by water and obtains.
Products therefrom is BiNbO after testing4。
To the product BiNbO obtained4Carry out SEM test.Test result is as shown in Figure 1.
From figure 2 it can be seen that obtained BiNbO4Powder is chondritic, rough surface porous, in the range of average diameter 1-3um, illustrates that this preparation method can be successfully obtained bismuth niobate multi-pore micron ball.
Embodiment
3
Step1: mix in the deionized water being dissolved in 50 mL by 2.0mmol bismuth citrate with the oxalic acid hydrate niobium of 6.0mmol, be acidified to PH=2 with appropriate salpeter solution, is stirred at room temperature 3h, forms precursor solution；
Step2: Step1 gained precursor solution is transferred to carry out making mist in the liquid holding cup of ultrasonic atomizer, after ultrasonic atomizatio, make the precursor solution of bismuth niobate presented in little droplet；
Step3: sending in the constant tube furnace of heating-up temperature with carrier gas stream for the precursor solution droplet that Step2 is obtained by 50L/min air, the droplet of precursor solution reacts through adding thermal reaction area (temperature is 800 DEG C), product is absorbed by water and obtains.
Products therefrom is BiNbO after testing4。
It follows that we pass through correlation test to BiNbO4The photocatalytic activity of multi-pore micron ball is evaluated.
Simulated solar irradiation is utilized to irradiate BiNbO4Multi-pore micron ball, characterize for the speed of NO in its degraded air, it is passed through the continuous air flow that NO concentration is 400ppb in the reactor and carries out photocatalytic degradation test, using the xenon lamp of 300 W as simulated solar irradiation radiation source, the culture dish comprising 0.1 g catalyst fines sample is placed in the continuous air flow reactor with quartz glass window, after being passed through Dilution air continuously, concentration is the NO air-flow of 400 ppb, opens xenon lamp and test after gas absorption balances.
The catalytic performance of photochemical catalyst is evaluated by NO concentration in air-flow after the monitoring degraded of NOx dynamic monitor.
Fig. 1 is the BiNbO of embodiment 1,2,3 preparation4Degradation rate-light application time the curve of multi-pore micron ball photocatalytic degradation NO.
As can be seen from Figure 1:
(1) BiNbO prepared by embodiment 14Multi-pore micron ball shows good degradation property to NO, and simulated solar irradiation irradiates 10 minutes NO clearances up to 35%；
(2) BiNbO prepared by embodiment 24Multi-pore micron ball shows good degradation property to NO, and simulated solar irradiation irradiates 10 minutes NO clearances up to 47%；
(3) BiNbO prepared by embodiment 34Multi-pore micron ball shows good degradation property to NO, and simulated solar irradiation irradiates 10 minutes NO clearances up to 39%.
As can be seen here, the BiNbO that the method for the present invention is prepared is used4Multi-pore micron ball shows good degradation property to NO, and simulated solar irradiation irradiates 10 minutes NO clearances and may be up to 47%.
Due to the BiNbO using the method for the present invention to prepare4Multi-pore micron ball has bigger specific surface area, and pollutant is had good absorption and transmittability, so it can be used in the preparation of air cleaning support materials, it is used for removing gaseous contaminant present in air, in terms of environmental improvement, has broad prospect of application.
The preparation of the present invention main exploratory development bismuth niobate multi-pore micron ball and under simulated solar irradiation photocatalytic degradation to NOx.Having bismuth niobate multi-pore micron ball that the supersonic spraying of continuous prodution power quickly prepares by improving material specific surface area by utilization, so that the avtive spot removing pollutant increases, and this preparation technology is the most controlled, can be effective to industrialization and produce.
Bismuth niobate multi-pore micron ball material prepared by the present invention, due to the microstructure that it is special, adds the specific surface area of material so that it is has good pollutant absorption and transmittability, thus improves photocatalytic activity.Bismuth niobate micron ball is obvious to the degradation effect of gaseous contaminant, and simulated solar irradiation irradiates 10 minutes NO clearances and may be up to 48%, has broad prospect of application in terms of air contaminant treatment.This research has far reaching significance to the practical of photocatalysis technology.
The present invention be should be understood that; embodiment described above; the purpose of the present invention, technical scheme and beneficial effect have been carried out further details of explanation; these are only embodiments of the invention; it is not intended to limit the present invention; the technical scheme that the mode of all employing equivalents or equivalent transformation is obtained, all falls within protection scope of the present invention.
Claims (7)
1. the ultrasonic atomizatio preparation method of a bismuth niobate multi-pore micron ball with photocatalytic activity, it is characterised in that comprise the following steps:
Step1: the preparation of the precursor solution of bismuth niobate salt: bismuth salt is mixed with niobium salt and is dissolved in deionized water, the bismuth salt wherein added and the mol ratio of niobium salt are 1:1～1:5, it is acidified to PH=1～3, room temperature 18 DEG C to 25 DEG C stirring 1～3 h with salpeter solution, forms precursor solution；
Step2: the atomization of the precursor solution of bismuth niobate salt: the precursor solution of the bismuth niobate salt obtained by Step1 is added in the liquid holding cup of ultrasonic atomizer carry out making mist, after ultrasonic atomizatio, make the precursor solution of bismuth niobate presented in little droplet, wherein ultrasonic frequency 1.7MHz ± 10%, condensation rate is 0.1～1L/h；
Step3: the production of bismuth niobate micron ball and collection: using air as carrier gas, the precursor solution droplet obtained by Step2 adds thermal reaction area 600～1000 DEG C by what tube furnace was sent in carrier gas, reacting, obtain product and absorbed by cooling down water, wherein flow rate of carrier gas is 10～70L/min.
The ultrasonic atomizatio preparation method of the bismuth niobate multi-pore micron ball with photocatalytic activity the most according to claim 1, it is characterised in that in described Step1, bismuth salt is five nitric hydrate bismuth or bismuth citrates, and the mol ratio of bismuth salt and niobium salt is 1:1～1:5.
The ultrasonic atomizatio preparation method of the bismuth niobate multi-pore micron ball with photocatalytic activity the most according to claim 1, it is characterised in that in Step1, is acidified to PH=1～3 with salpeter solution by precursor solution.
The ultrasonic atomizatio preparation method of the bismuth niobate multi-pore micron ball with photocatalytic activity the most according to claim 1, it is characterised in that in Step2, the condensation rate of ultrasonic atomizatio is 0.1～1L/h.
The ultrasonic atomizatio preparation method of the bismuth niobate multi-pore micron ball with photocatalytic activity the most according to claim 1, it is characterised in that in Step3, the heating reaction zone temperature of tube furnace is 600～1000 DEG C, and atmospheric carrier air flow velocity is 10～70L/min.
The ultrasonic atomizatio preparation method of the bismuth niobate multi-pore micron ball with photocatalytic activity the most according to claim 1, it is characterised in that in Step3, the bismuth niobate multi-pore micron ball obtained is directly to be collected by water.
7. a bismuth niobate multi-pore micron ball with photocatalytic activity, it is characterized in that, the described bismuth niobate multi-pore micron ball with photocatalytic activity uses the ultrasonic atomizatio preparation method of arbitrary described bismuth niobate multi-pore micron ball with photocatalytic activity in claim 1 to 6 to be prepared from.
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| CN115069248A (en) * | 2022-07-12 | 2022-09-20 | 西南交通大学 | Silver niobate nano material and preparation method and application thereof |
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Application publication date: 20160720 |