CN109692683A - A kind of method and related device preparing iron acid zinc catalyst using single mold microwave - Google Patents
A kind of method and related device preparing iron acid zinc catalyst using single mold microwave Download PDFInfo
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- CN109692683A CN109692683A CN201811581428.4A CN201811581428A CN109692683A CN 109692683 A CN109692683 A CN 109692683A CN 201811581428 A CN201811581428 A CN 201811581428A CN 109692683 A CN109692683 A CN 109692683A
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- microwave
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- mold microwave
- zinc ferrite
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- 239000011701 zinc Substances 0.000 title claims abstract description 40
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000002253 acid Substances 0.000 title claims abstract description 33
- 239000003054 catalyst Substances 0.000 title claims abstract description 17
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 115
- 229910001308 Zinc ferrite Inorganic materials 0.000 claims abstract description 87
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 claims abstract description 84
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000002243 precursor Substances 0.000 claims abstract description 52
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000010453 quartz Substances 0.000 claims abstract description 37
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000007873 sieving Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 9
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 230000001698 pyrogenic effect Effects 0.000 claims abstract description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 92
- 239000007789 gas Substances 0.000 claims description 51
- 229910052757 nitrogen Inorganic materials 0.000 claims description 46
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical group [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 39
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 39
- 230000005284 excitation Effects 0.000 claims description 36
- 230000001105 regulatory effect Effects 0.000 claims description 32
- 230000005855 radiation Effects 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- 239000000523 sample Substances 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000498 cooling water Substances 0.000 claims description 14
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 14
- 239000012071 phase Substances 0.000 claims description 13
- 230000009977 dual effect Effects 0.000 claims description 11
- 230000003134 recirculating effect Effects 0.000 claims description 11
- 238000010992 reflux Methods 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 10
- 230000005540 biological transmission Effects 0.000 claims description 10
- 230000005672 electromagnetic field Effects 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000835 fiber Substances 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 4
- 239000000356 contaminant Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 230000011514 reflex Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- 239000012808 vapor phase Substances 0.000 claims description 3
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 claims 3
- 239000010881 fly ash Substances 0.000 claims 3
- 230000005611 electricity Effects 0.000 claims 1
- 239000003292 glue Substances 0.000 claims 1
- 229910001385 heavy metal Inorganic materials 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 72
- 238000001354 calcination Methods 0.000 abstract description 56
- 238000003980 solgel method Methods 0.000 abstract description 29
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 19
- 238000001179 sorption measurement Methods 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract 1
- 229940043267 rhodamine b Drugs 0.000 description 32
- 238000012512 characterization method Methods 0.000 description 16
- 239000013078 crystal Substances 0.000 description 15
- 238000002474 experimental method Methods 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- 238000000926 separation method Methods 0.000 description 12
- 238000004458 analytical method Methods 0.000 description 11
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 11
- 150000003751 zinc Chemical class 0.000 description 11
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000003009 desulfurizing effect Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013459 approach Methods 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
- 238000004364 calculation method Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000010189 synthetic method Methods 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/126—Microwaves
-
- 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
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Environmental & Geological Engineering (AREA)
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Abstract
The present invention relates to a kind of methods and related device that iron acid zinc catalyst is prepared using single mold microwave, are based on Zn (CH3COO)2·2H2O、Fe(NO3)3·6H2O, citric acid and dehydrated alcohol synthesize zinc ferrite precursor solution using sol-gel method；The zinc ferrite precursor solution of preparation is dried, the precursor after drying is ground, sieving separating；It is put into quartz tube reactor after the zinc ferrite precursor and Microwave Senstizer that sieving obtains are mixed according to the ratio uniform that mass ratio is 1:0~2:7, then is placed in single mold microwave reaction cavity；Fumed pyrogenic is carried out to the zinc ferrite precursor that sol-gel method synthesizes using single mold microwave.The present invention realizes rapid synthesis environment functional material using microwave irradiation technology, feature is that required calcinating consumption is low, the reaction time is shorter and attribute of the synthesis ferrous acid Zinc material with quick adsorption hardly degraded organic substance, the disadvantages of the method overcome traditional reaction time is longer, energy consumption is high, at high cost provides the new technology and method of a kind of zinc ferrite environment functional material synthesis.
Description
Technical field
The present invention relates to zinc ferrite material synthesis method technical fields more particularly to a kind of utilization single mold microwave to prepare ferrous acid
The method of zinc catalyst and corresponding single mold microwave reaction unit.
Background technique
Zinc ferrite (ZnFe2O4) it is a kind of catalyst with visible light catalysis activity, since forbidden gap energy is only 1.9eV,
It is also considered as a kind of ideal visible light catalyst.ZnFe2O4There are two big main bugbears in light-catalyzed reaction for powder: light
Raw electron-hole cannot efficiently separate and react after recycle, limit ZnFe2O4The practical application of photochemical catalyst.Mesh
Before, the main synthetic method of zinc ferrite has coprecipitation, sol-gal process, conventional hydrothermal method and microwave-hydrothermal method etc., above-mentioned conjunction
Reaction atmosphere is prepared for the ZnFe that finally synthesizes at what is used in method2O4Material property is vital.With the molten of classics
For glue-gel method, the adhesives such as citric acid by after being reacted with metallic ion coordination formed the netted colloform texture of space multistory,
And zinc ferrite crystal is ultimately formed by heat treatment processes such as calcinings.However, high-temperature burning process often leads to ferrous acid Zinc material
Duct collapses, and can also significantly reduce the specific surface area of material, reduces effecting reaction active site.How pyroreaction condition is realized
Preparing zinc ferrite crystal and retaining large specific surface area is current one of Research Challenges.Under inert gas shielding atmosphere, adopt
Being prepared in ideal zinc ferrite materials theory with microwave energy sol-gel method precursor is feasibility.
Currently, studying the micro-wave dielectric radiating system using multimode cavity body mostly to prepare ferrous acid Zinc material.Such as:
Patent ZL 2016109160397 discloses a kind of utilization multi-mode microwave radiation roasting crucible and multi-mode microwave fabricated in situ ferrous acid
The method of zinc desulfurizing agent.The desulfurizing agent precursor of synthesis is after grinding, kneading, extrusion, drying and moulding, then passes through microwave reflection
Etc. approach by radiation profiles in multi-mode microwave reactor cavity body, to the synthesis in the oxygen-containing atmosphere of 2~8% (v/v)
Desulfurizing agent precursor is reacted to prepare ferrous acid Zinc material.
There are energy fields to be unevenly distributed, energy density in preparation inorganic material reaction process for above-mentioned multimode cavity body
More low significant drawback cannot accurately monitor materials synthesis temperature, influence the performance of synthetic material.
Summary of the invention
The purpose of the invention is to overcome technical problem of the existing technology, a kind of utilization single mold microwave preparation is provided
The method and related device of iron acid zinc catalyst can generate standing wave etc. in reaction cavity and significantly improve reaction chamber by it
Intracorporal radiation energy field density, and the field of radiational energy is relatively uniform, can preferably solve multi-mode microwave synthetic inorganic material mistake
Defect existing for journey can synthesize the ferrous acid Zinc material with large specific surface area and stronger absorption property.
The purpose of the present invention is achieved through the following technical solutions:
The present invention provides a kind of method for preparing iron acid zinc catalyst using single mold microwave comprising:
Regulated power supply, microwave power regulating device, microwave excitation generating device, single mold microwave reaction unit and gas phase are collected
Device；
The regulated power supply provides stable power source for entire single mold microwave reaction unit；
The regulated power supply connects the microwave power regulating device；The microwave power regulating device is inputted by electric current
Control line and control voltage control line are connect with the microwave excitation generating device；The microwave excitation generating device and the list
Mould microwave reactor is connected by flange form；
The single mold microwave reaction unit includes adjusting terminal short circuit piston and single mold microwave reaction cavity；The single mode is micro-
Wave reaction unit is returned by adjusting the microwave pulse signal reflex that terminal short circuit piston generates the microwave excitation generating device
It goes, forms amplitude, frequency and electromagnetic field direction of vibration is all the same, transmission direction is opposite back wave, and occur with microwave excitation
The microwave pulse incident wave that device generates forms interference reaction in single mold microwave reaction cavity；By adjusting terminal short circuit
The position of piston generates single and high uniformity high power density energy field in monofilm microwave reaction cavity；
The gas phase collection device include nitrogen cylinder, mass flow controller, quartz reactor, quartz fibre filter cylinder frame,
Reflux condenser, resin cartridge, toluene absorbing liquid, sodium hydroxide absorbing liquid, gas dry pipe, gas sampling probe, Portable gas
Matter combined instrument；
Nitrogen in nitrogen cylinder enters quartz reactor after gas valve and mass flow controller with certain flow；Dress
There is the quartz reactor of flying dust sample layer to be placed in the reaction cavity of the single mold microwave reactor, flying dust sample is in the single mode
After microwave reactor carries out single mold microwave pyrolytic reaction, the vapor phase contaminants of generation can successively pass through quartz fibre filter with nitrogen
Tub, reflux condenser, resin cartridge, toluene absorbing liquid, sodium hydroxide absorbing liquid, gas dry pipe, gas sampling probe, finally
Into portable gas chromatograph-mass spectrometer.
It is highly preferred that the single mold microwave reactor further include:
Circulator and water load, dual directional coupler, three screw tuners and vertical waveguide microwave excitation cavity；
The circulator and water load, dual directional coupler, three screw tuners, vertical waveguide microwave excitation cavity each other it
Between pass through flange form connect；The single mold microwave reactor monitors the microwave energy of transmitted in both directions by dual directional coupler, and
The microwave radiation energy field in the monofilm microwave reaction cavity is adjusted by three screw tuners and terminal short circuit piston；It is described
Circulator and water load absorb the monofilm microwave reaction cavity and are transmitted back to the unabsorbed microwave come.
It is highly preferred that the single mold microwave reactor further include:
Infrared radiation thermometer and computer；
The two sides of monofilm microwave reaction cavity are arranged in the probe of the infrared radiation thermometer, and infrared radiation thermometer and computer connect
The temperature for connecing real-time monitoring sample changes with time.
It is highly preferred that the single mold microwave reaction unit further include:
Recirculating cooling water system I；
The recirculating cooling water system I is in parallel with the circulator and water load, mentions for the circulator and water load 4.1
For recirculated cooling water.
The present invention also provides a kind of methods for preparing iron acid zinc catalyst using single mold microwave comprising:
Step S101 is based on Zn (CH3COO)2·2H2O、Fe(NO3)3·6H2O, citric acid and dehydrated alcohol, utilization are molten
Glue-gel method synthesizes zinc ferrite precursor solution；
By Zn (CH3COO)2·2H2O and Fe (NO3)3·6H2O is dissolved in dehydrated alcohol according to the molar ratio of 1:2, stirring
Until solid is completely dissolved；It is added dropwise after citric acid is dissolved in dehydrated alcohol in above-mentioned solution, citric acid and again
The molar ratio of metal ion keeps 1.0:1.0~1.0:1.5；Obtain zinc ferrite precursor solution；
The zinc ferrite precursor solution of preparation is dried in step S102, grinds to the precursor after drying, crosses and sieves
From；
Step S103, the zinc ferrite precursor that sieving is obtained and Microwave Senstizer are 1:0~2:7 according to mass ratio
Ratio uniform mixing after be put into quartz tube reactor, then be placed in single mold microwave reaction cavity；Using single mold microwave to colloidal sol-
The zinc ferrite precursor of gel method synthesis carries out fumed pyrogenic.
It is highly preferred that being passed through inert gas always in the entire reaction process of microwave-heating, single mold microwave reaction cavity is kept
Interior temperature is at 300~600 DEG C.
It is highly preferred that Microwave Senstizer is silicon carbide in the step S103, partial size is 1.5~1.8mm.
It is highly preferred that the inert atmosphere is nitrogen atmosphere in the step S103.
It is highly preferred that the sieving separating of the zinc ferrite precursor uses the sieve of 100 mesh.
The present invention has the following technical effect that it can be seen from the technical solution of aforementioned present invention
(1) addition Microwave Senstizer reduces the microwave absorbing property of calcining layer, extends the heating-up time of calcining sample；
(2) the more uniform uniformity for advantageously ensuring that calcined materials of single mold microwave reaction cavity energy field；
(3) the ferrous acid Zinc material that microwave radiation energy field assigns preparation under nitrogen protection has the spies such as biggish specific surface area
Different functional attributes.
(4) zinc ferrite function is prepared under the conditions of 300~600 degree using single mold microwave radiotechnology the present invention provides a kind of
Can material method simultaneously for simultaneously adsorption-photocatalytic degradation RhB dyestuff, this method at that same temperature, have energy consumption compared with
The advantages that low, reaction time is short and easy Magnetic Isolation.
(5) present invention can prepare environment functional material for calcination method and provide a kind of new technology and new synthesis technology.
Detailed description of the invention
Fig. 1 is the structural diagram of the present invention；
Fig. 2 (a) prepares precursor for sol-gel method and prepares iron in 300~600 degree of calcinings of single mold microwave (nitrogen+SiC)
The warming process of sour Zinc material；
Fig. 2 (b) prepares precursor for sol-gel method and prepares iron in 300~600 degree of calcinings of single mold microwave (nitrogen+SiC)
The XRD result of sour Zinc material；
The ferrous acid Zinc material TEM photo that Fig. 3 (a) is temperature when being 300 degree of single mold microwave (nitrogen+SiC)；
The ferrous acid Zinc material TEM photo that Fig. 3 (b) is temperature when being 400 degree of single mold microwave (nitrogen+SiC)；
The ferrous acid Zinc material TEM photo that Fig. 3 (c) is temperature when being 500 degree of single mold microwave (nitrogen+SiC)；
The ferrous acid Zinc material TEM photo that Fig. 3 (d) is temperature when being 600 degree of single mold microwave (nitrogen+SiC)；
Fig. 4 (a) is that sol-gel method prepares ferrous acid Zinc material of the precursor by 300~600 degree of Muffle furnace calcining preparations
XRD；
Fig. 4 (b) is that sol-gel method prepares ferrous acid Zinc material of the precursor by 300~600 degree of atmosphere furnace calcining preparations
XRD；
Fig. 5 (a) prepares precursor for sol-gel method and prepares zinc ferrite in 300~600 degree of calcinings of single mold microwave (nitrogen)
(a) warming procedure chart of material；
Fig. 5 (b) prepares precursor for sol-gel method and prepares zinc ferrite in 300~600 degree of calcinings of single mold microwave (nitrogen)
The XRD result schematic diagram of material；
Fig. 6 (a) is that sol-gel method prepares precursor by 300~600 degree of single mold microwave (nitrogen+SiC) calcining preparations
Ferrous acid Zinc material adsorbs RhB removal efficiency；
Fig. 6 (b) prepares precursor for sol-gel method and prepares the suction of ferrous acid Zinc material by 300~600 degree of Muffle furnace calcinings
Attached RhB removal efficiency；
Fig. 6 (c) prepares precursor for sol-gel method and prepares the suction of ferrous acid Zinc material by 300~600 degree of atmosphere furnace calcinings
Attached RhB removal efficiency；
Fig. 7 (a) is body before Muffle furnace, 400 degree of firing sols of atmosphere furnace and single mold microwave (nitrogen+SiC)-gel method preparation
Body prepares zinc ferrite material light catalysis degradation RhB effect picture (illustration is Magnetic Isolation effect)；
Fig. 7 (b) is the zinc ferrite that single mold microwave (nitrogen+SiC) 400 degree of firing sol-gel methods prepare precursor preparation
Photocatalysis recycles effect；
Fig. 8 be sol-gel method prepare precursor (citric acid and metal ion initial proportion are respectively 1:1,1:1.2 and
The removal efficiency of zinc ferrite material light catalysis degradation MB 1:1.5) is prepared by 600 degree of single mold microwave (nitrogen+SiC) calcinings；
Fig. 9 (a) is that sol-gel method prepares precursor (citric acid and metal ion initial proportion be respectively 1:1) respectively
The absorption of ferrous acid Zinc material is prepared by 600 degree of single mold microwave (nitrogen+SiC), single mold microwave (air+SiC) and Muffle furnace calcinings
The removal efficiency of RhB；
Fig. 9 (b) is that sol-gel method prepares precursor (citric acid and metal ion initial proportion be respectively 1:1.2) point
Not Jing Guo 600 degree of single mold microwave (nitrogen+SiC), single mold microwave (air+SiC) and Muffle furnace calcinings prepare the suction of ferrous acid Zinc material
The removal efficiency of attached RhB；
Figure 10 is the flow chart of the embodiment of the present invention two.
In attached drawing:
Regulated power supply 1, microwave power regulating device 2, microwave excitation generating device 3, single mold microwave reaction unit 4 and gas phase
Collection device 5；
Timer 2 .1, temperature sensor 2.2, anode current display 2.3, filament pre-heating device 2.4, power governor
2.5, power supply indicator 2.6, power switch 2.7, microwave indicator light 2.8, microwave switch 2.9；
Low pressure indicator light 3.1, microwave indicator light 3.2, high input voltage port 3.3, control signal mouth 3.4, electric current input
Control line 3.5 and control voltage control line 3.6；
Circulator and water load 4.1, recirculating cooling water system I 4.2, dual directional coupler 4.3, three screw tuners 4.4,
Vertical waveguide microwave excitation cavity 4.5, monofilm microwave reaction cavity 4.6, terminal short circuit piston 4.7, infrared radiation thermometer 4.8 and calculating
Machine 4.9；
Nitrogen cylinder 5.1, gas valve 5.2, mass flow controller 5.3, quartz reactor 5.4, quartz fibre filter cylinder frame
5.5, reflux condenser 5.6, recirculating cooling water system II 5.7, resin cartridge 5.8, toluene absorbing liquid 5.9, sodium hydroxide absorbing liquid
5.10, gas dry pipe 5.11, gas sampling probe 5.12, portable gas chromatograph-mass spectrometer 5.13.
Specific embodiment
In order to make those skilled in the art more fully understand the technical solution of the application, below with reference to attached drawing to this hair
It is bright to be described in further details.
Embodiment one:
The present invention provides a kind of single mold microwave reaction unit, and structure is as shown in Figure 1, comprising: regulated power supply 1, microwave function
Rate regulating device 2, microwave excitation generating device 3, single mold microwave reaction unit 4 and gas phase collection device 5；
Regulated power supply 1 provides stable electric power for entire single mold microwave reaction unit；Regulated power supply 1 connects microwave power tune
Regulating device 2；Microwave power regulating device 2 passes through electric current input control line and control voltage control line and microwave excitation generating device
3 connections, microwave excitation generating device 3 are connect with single mold microwave reactor 4 by flange form, and gas phase collection device 5 and single mode are micro-
The reaction cavity of wave reactor 4 is connected.
The function and its structure of all parts are specific as follows:
Regulated power supply 1:
Regulated power supply 1 is connected with microwave power regulating device 2, provides stable electric power for microwave power regulating device 2
Source.
Microwave power regulating device 2:
Anode current is micro- and wave radiation power for adjusting for microwave power regulating device 2, mentions for microwave excitation generating device 3
For stable electric current and power, and time timing is provided and monitors the temperature of monofilm microwave reaction cavity.
The microwave power regulating device 2 includes timer 2 .1, temperature sensor 2.2, anode current display 2.3, filament
Preheater 2.4, power governor 2.5, power supply indicator 2.6, power switch 2.7, microwave indicator light 2.8, microwave switch 2.9.
Timer 2 .1 is that entire microwave power regulating device 2 provides time timing；Temperature sensor 2.2 is used to monitor list
The temperature of film microwave reaction cavity；Filament pre-heating device 2.4 is used to stablize heater current.Regulation power adjuster 2.5 can change
Anode current；Anode current is presented to the user by anode current display 2.3；It can change by the power governor 2.5
Microwave irradiation power (0~1kW) realizes the influence that different radiant powers react sample temperature-rise period and single mold microwave；Power supply
Indicator light 2.6 is connected with power switch 2.7, and microwave indicator light 2.8 is connected with microwave switch 2.9, anode current display 2.3 with
Power governor 2.5 is connected.
Microwave excitation generating device 3:
Microwave excitation generating device 3 is connected with microwave power regulating device 2, is adjusted according to microwave power regulating device 2
Electric current and power afterwards generate corresponding microwave pulse signal.
Microwave excitation generating device 3 is connected with microwave power regulating device 2, which refers to including low pressure
Show lamp 3.1, microwave indicator light 3.2, high input voltage port 3.3, control signal mouth 3.4, electric current input control line 3.5 and control
Voltage control line 3.6.
Electric current input control line 3.5 is connected with high input voltage port 3.3, controls voltage control line 3.6 and control signal
Mouth 3.4 is connected.The control signal of control signal mouth 3.4 connects the voltage of the outlet line of the high input voltage port 3.3；It is low
Pressure indicator light 3.1 and microwave indicator light 3.2 are connected in parallel on respectively on the outlet line of high input voltage port 3.3.
Pass through electric current input control line 3.5 and control between above-mentioned microwave excitation generating device 3 and microwave power regulating device 2
Voltage control line 3.6 processed connects.
Single mold microwave reaction unit 4:
Single mold microwave reaction unit 4 is connect by flange form with microwave excitation generating device 3, will by adjusting terminal piston
The microwave pulse signal reflex that microwave excitation generating device 3 generates is gone back to form amplitude, frequency and electromagnetic field direction of vibration homogeneous
Back wave same, transmission direction is opposite, and it is micro- in single mode with the microwave pulse incident wave of the generation of microwave excitation generating device 3
Interference reaction is formed in wave reaction cavity；By adjusting the position of terminal piston, generated in monofilm microwave reaction cavity single
And the high power density energy field of high uniformity, promote the material in the intracorporal quartz reactor of monofilm microwave reaction chamber to be filled
Divide reaction, and monitors the microwave energy of transmitted in both directions in experiment, the extra microwave energy returned to monofilm microwave reaction cavity reflections
Amount is absorbed.
Single mold microwave reaction unit 4 is connect by flange with microwave excitation generating device 3, the single mold microwave reaction unit 4
Including circulator and water load 4.1, recirculating cooling water system I 4.2, dual directional coupler 4.3, three screw tuners 4.4, vertical
Waveguide microwave excitation cavity 4.5, monofilm microwave reaction cavity 4.6, terminal short circuit piston 4.7, infrared radiation thermometer 4.8 and computer
4.9。
After opening microwave power source and setting 2.3 numerical value of anode current display, generated through microwave excitation generating device 3
Microwave pulse radiation signal forms incidence wave, successively micro- by dual directional coupler 4.3, three screw tuners 4.4, vertical waveguide
Wave excitation chamber 4.5 enters monofilm microwave reaction cavity 4.6, reflects and is formed in the metal surface of terminal short circuit piston 4.7
Back wave, back wave and incidence wave being capable of further occurrence interference phenomenon；It, can by adjusting the position of terminal short circuit piston 4.7
So that amplitude, frequency and electromagnetic field direction of vibration is all the same, transmission direction is opposite back wave and incidence wave are anti-in monofilm microwave
It answers and forms standing wave in cavity 4.6, to guarantee that microwave radiation electromagnetic field density is maximum in monofilm microwave reaction cavity 4.6.
Connection relationship between each component of single mold microwave reaction unit 4 is as follows:
Above-mentioned circulator and water load 4.1, dual directional coupler 4.3, three screw tuners 4.4, vertical waveguide microwave swash
Chamber 4.5, monofilm microwave reaction cavity 4.6, terminal short circuit piston 4.7 are encouraged, is connected, can be freely torn open by flange form each other
It unloads.
Above-mentioned circulator and water load 4.1, which absorb, not to be absorbed and reflected microwave by monofilm microwave reaction cavity 4.6,
It avoids magnetron temperature excessively high and aging is accelerated.By adjusting circulator and water load 4.1, microwave reflection can be reduced to micro-
The influence of wave magnetron.Recirculating cooling water system I 4.2 is in parallel with above-mentioned circulator and water load 4.1, is circulator and water load
4.1 provide recirculated cooling water.
Dual directional coupler 4.3 is used to monitor the microwave energy of transmitted in both directions in experiment；Three screw tuners 4.4 are according to double
The microwave energy size that directional coupler 4.3 monitors adjusts back wave to adjust reflected current and then realize；
Vertical waveguide microwave excitation cavity 4.5 for changing microwave transmission direction so that incidence wave and back wave, vertically into
Enter in monofilm microwave reaction cavity 4.6；
Monofilm microwave reaction cavity 4.6 is for placing quartz reactor and absorbing single mold microwave, due to incidence wave and reflection
Wave can vertically into its reaction cavity, so its reaction cavity can do it is smaller.
It is short by terminal after the microwave pulse radiation signal that microwave excitation generating device 3 generates reaches terminal short circuit piston 4.7
The metal surface of road piston 4.7 reflects back, and forms amplitude, frequency and electromagnetic field direction of vibration is all the same, transmission direction is opposite
Back wave, and with microwave excitation generating device 3 generate microwave pulse incident wave in single mold microwave reaction cavity 4.6
Form interference reaction；By adjust terminal piston 4.7 position, can make amplitude, frequency and electromagnetic field direction of vibration it is all the same,
The opposite back wave of transmission direction and incidence wave form standing wave in monofilm microwave reaction cavity 4.6, to guarantee monofilm microwave
Microwave radiation electromagnetic field density is maximum in reaction cavity 4.6.
The two sides of monofilm microwave reaction cavity 4.6, infrared radiation thermometer 4.8 and meter is arranged in the probe of infrared radiation thermometer 4.8
The temperature that calculation machine 4.9 connects real-time monitoring sample changes with time.
It is produced since above-mentioned single mold microwave reaction unit 4 is formed by terminal short circuit piston 4.7 with microwave excitation generating device 3
Raw microwave incidence wave has same-amplitude, frequency and the opposite back wave of electromagnetic field direction of vibration, transmission direction, and passes through tune
The position of terminal short circuit piston 4.7 is saved to adjust back wave and incidence wave and form interference in single mold microwave reaction cavity 4.6
Reaction, microwave transmission direction is adjusted by vertical waveguide microwave excitation cavity 4.5, is adjusted and is reflected by three screw tuners 4.4
The size of wave makes amplitude, frequency and electromagnetic field direction of vibration is all the same, transmission direction is opposite back wave and incidence wave in monofilm
Standing wave is formed in microwave reaction cavity 4.6, generates single and high uniformity high power density energy field, and since monofilm is micro-
The cavity of wave reaction cavity 4.6 is smaller, therefore the microwave radiation energy density in single mold microwave reaction cavity 4.6 is micro- with respect to multimode
Wave is larger.This, which is just determined, penetrates readily through solid mineral material and forms medium temperature reaction atmosphere in the single mold microwave short time, in list
(400~600 DEG C) of mould microwave medium temperature reactions, reaction process have many advantages, such as that low energy consumption, microwave radiation field is uniform.
And the back wave and incidence wave of above-mentioned single mold microwave reaction unit 4 can be adjusted by corresponding device,
Its controllability is high, heating uniformity is good.
Gas phase collection device 5:
Gas phase collection device 5 is acquiring vapor phase contaminants sample after single mold microwave pyrolytic reaction；And qualitative analysis gas
Volatile organic matter in sample；To in the quartz reactor 5.4 after low temperature pyrogenation in the development of single mold microwave reaction unit 4
After sample sieving separating Microwave Senstizer, available calcined solid mineral material sample under sieve.
Gas phase collection device 5 includes nitrogen cylinder 5.1, gas valve 5.2, mass flow controller 5.3, quartz reactor
5.4, quartz fibre filter cylinder frame 5.5, reflux condenser 5.6, recirculating cooling water system II 5.7, resin cartridge 5.8, toluene absorbing liquid
5.9, sodium hydroxide absorbing liquid 5.10, gas dry pipe 5.11, gas sampling probe 5.12, portable gas chromatograph-mass spectrometer 5.13.
Connection relationship between the function and these components of each component of gas phase collection device 5 is as follows:
Nitrogen cylinder 5.1 is filled with nitrogen；Nitrogen cylinder 5.1 passes through the input terminal of gas valve 5.2 and mass flow controller 5.3
It is connected.The output end of mass flow controller 5.3 protrudes into quartz reactor 5.4；It is anti-that quartz reactor 5.4 is placed in monofilm microwave
It answers in cavity 4.6；One end of quartz fibre filter cylinder frame 5.5 is protruded into quartz reactor 5.4, the other end and reflux condenser 5.6
It is connected；The output end of reflux condenser 5.6 is connected with resin cartridge 5.8, toluene absorbing liquid 5.9, sodium hydroxide absorbing liquid in turn
5.10, gas dry pipe 5.11, gas sampling probe 5.12 and portable gas chromatograph-mass spectrometer 5.13；Recirculating cooling water system II
5.7 is in parallel with reflux condenser 5.6, to reduce gas temperature.
Nitrogen in nitrogen cylinder 5.1 enters stone after gas valve 5.2 and mass flow controller 5.3 with certain flow
English reactor 5.4；Quartz reactor 5.4 is placed in monofilm microwave reaction cavity 4.6, the gas phase after single mold microwave pyrolytic reaction
Pollutant successively passes through quartz fibre filter cylinder frame 5.5, reflux condenser 5.6, resin cartridge 5.8, toluene absorbing liquid with nitrogen
5.9, after sodium hydroxide absorbing liquid 5.10, gas dry pipe 5.11, gas sampling probe 5.12, into portable gas chromatograph-mass spectrometer
5.13；Wherein, quartz fibre filter cylinder frame 5.5 is for capturing particulate matter, reflux condenser 5.6 and recirculating cooling water system II 5.7
For reducing gas temperature, for resin cartridge 5.8 for adsorbing gas phase organic matter, toluene absorbing liquid 5.9 is unadsorbed for absorbing
Organic matter, sodium hydroxide absorbing liquid 5.10 are used to remove the water of gas for absorbing gaseous acid pollution, gas dry pipe 5.11
Point, gas sampling probe 5.12 is for acquiring gaseous sample, and portable gas chromatograph-mass spectrometer 5.13 is in qualitative analysis gas
Volatile organic matter.
Embodiment two:
The present invention provides a kind of method for preparing iron acid zinc catalyst using single mold microwave, implementing procedure such as Figure 10 institutes
Show, specifically includes the following steps:
Step S101, sol-gel method synthesize zinc ferrite precursor
By Zn (CH3COO)2·2H2O and Fe (NO3)3·6H2O is dissolved in dehydrated alcohol according to the molar ratio of 1:2, uses magnetic
Power stirring is stirred repeatedly until solid is completely dissolved；
Citric acid (concentration 10mM) is added dropwise after being also dissolved in dehydrated alcohol in above-mentioned solution, citric acid and again
The molar ratio of metal ion keeps 1.0:1.0~1.0:1.5.
The zinc ferrite precursor of preparation is dried in step S102, grinds to the precursor after drying, sieving separating.
Above-mentioned zinc ferrite precursor is put in an oven, is first saved 10 hours at 80 degree, and final 150 degree save 2 hours.Sieving
Separation uses the sieve of 100 mesh.
Step S103 carries out fumed pyrogenic to the zinc ferrite precursor that sol-gel method synthesizes using single mold microwave.
It is put after above-mentioned zinc ferrite precursor and Microwave Senstizer are mixed according to the ratio uniform that mass ratio is 1:0~2:7
Enter quartz tube reactor, then is placed in single mold microwave reaction cavity；Be passed through before microwave-heating inert gas drive for a period of time it is residual
The air stayed, and single mold microwave radiant power source is opened, it keeps entire reaction process to be passed through inert gas always, keeps single mode micro-
The intracorporal temperature of wave reaction chamber carries out microwave-heating calcination reaction at 300~600 DEG C, to the intracorporal mixture of chamber.Microwave-heating
Time be 38 seconds~526 seconds.
In step S103, Microwave Senstizer is silicon carbide, and partial size is 1.5~1.8mm, body before Microwave Senstizer and zinc ferrite
The mass ratio of body is 1:0~2:7；
In step S103, the output power of single mold microwave device is 345~494W, and single mold microwave frequency is 2.45GHz；
In step S103, inert atmosphere is nitrogen atmosphere, and nitrogen (about 30 minutes) for a period of time are first passed through before microwave-heating,
Entire reaction process is passed through always nitrogen.
Beneficial effects of the present invention are verified through the following experiment:
Experiment 1
The molar ratio for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method is set to
1:1.5 is fully ground after mixing well with silicon carbide by 7:2 after being sieved and is transferred to quartz reactor, then is placed in single mold microwave
In the cavity of device (device is shown in that Fig. 1, single mold microwave output power are 410~494w), and continuously it is passed through under nitrogen atmosphere and carries out
Calcining, after calcining in 389 seconds maximum temperature up to 300 DEG C (temperature-rise period is shown in Fig. 2 (a)), stop single mold microwave radiation and after
It is continuous to be passed through nitrogen, until material layer cools to room temperature.Finally 100 mesh will be crossed by calcined material layer and silicon carbide blend
Sieve pore separation；Phenetic analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 2 (b), and TEM result is shown in Fig. 3 (a)；
ZnFe2O4:JCPDF 22-1012；ZnO:JCPDF36-1451).Take again calcining surplus material layer 0.1g absorption initial concentration be
Rhodamine b (RhB) solution 100mL of 4.96mg/L, after 16 minutes quick adsorptions react, the removal rate of RhB is 75.48%
(being detailed in Fig. 6 (a))；Under identical calcination temperature, the zinc ferrite of 300 DEG C of calcination reactions of Muffle furnace and tube furnace preparation, XRD analysis card
It is bright have zinc ferrite crystal generate (XRD characterization result is shown in Fig. 4 (a) and Fig. 4 (b)；ZnFe2O4:JCPDF 22-1012)；RhB is contaminated
Expect that adsorption reaction removal rate is respectively 7.91% (being detailed in Fig. 6 (b)) and 4.66% (being detailed in Fig. 6 (c)).
Experiment 2
The molar ratio for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method is set to
1:1.5 is fully ground after mixing well with silicon carbide by 7:2 after being sieved and is transferred to quartz reactor, then is placed in single mold microwave
In the cavity of device (device is shown in that Fig. 1, single mold microwave output power are 410~494w), and continuously it is passed through under nitrogen atmosphere and carries out
Calcining, after calcining in 470 seconds maximum temperature up to 400 DEG C (temperature-rise period is shown in Fig. 2 (a)), stop single mold microwave radiation and after
It is continuous to be passed through nitrogen, until material layer cools to room temperature.Finally 100 mesh will be crossed by calcined material layer and silicon carbide blend
Sieve pore separation；Phenetic analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 2 (b), and TEM result is shown in Fig. 3 (b)；
ZnFe2O4:JCPDF 22-1012；ZnO:JCPDF36-1451).Take again calcining surplus material layer 0.1g absorption initial concentration be
Rhodamine b (RhB) solution 100mL of 4.96mg/L, after 16 minutes, the removal rate of RhB is 90.7% (being detailed in Fig. 6 (a))；
Under identical calcination temperature, the zinc ferrite of 400 DEG C of calcination reactions of Muffle furnace and tube furnace preparation, XRD analysis proof has zinc ferrite brilliant
(XRD characterization result is shown in Fig. 4 (a) and Fig. 4 (b) for body generation；ZnFe2O4:JCPDF 22-1012)；The reaction of RhB Dye Adsorption is gone
Except rate is respectively 5.95% (being detailed in Fig. 6 (b)) and 5.93% (being detailed in Fig. 6 (c)).
Experiment 3
The molar ratio for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method is set to
1:1.5 is fully ground after mixing well with silicon carbide by 7:2 after being sieved and is transferred to quartz reactor, then is placed in single mold microwave
In the cavity of device (device is shown in that Fig. 1, single mold microwave output power are 410~494w), and continuously it is passed through under nitrogen atmosphere and carries out
Calcining, after calcining in 486 seconds maximum temperature up to 500 DEG C (temperature-rise period is shown in Fig. 2 (a)), stop single mold microwave radiation and after
It is continuous to be passed through nitrogen, until material layer cools to room temperature.Finally 100 mesh will be crossed by calcined material layer and silicon carbide blend
Sieve pore separation；Material analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 2 (b), and TEM result is shown in Fig. 3 (c)；
ZnFe2O4:JCPDF 22-1012；ZnO:JCPDF36-1451).Take again calcining surplus material layer 0.1g absorption initial concentration be
Rhodamine b (RhB) solution 100mL of 4.96mg/L, after 16 minutes, the removal rate of RhB is 87.3% (being detailed in Fig. 5 (a))；
Under identical calcination temperature, the zinc ferrite of 500 DEG C of calcination reactions of Muffle furnace and tube furnace preparation, XRD analysis proof has zinc ferrite brilliant
(XRD characterization result is shown in Fig. 4 (a) and Fig. 4 (b) for body generation；ZnFe2O4:JCPDF 22-1012)；The reaction of RhB Dye Adsorption is gone
Except rate is respectively 4% (being detailed in Fig. 6 (b)) and 3.68% (being detailed in Fig. 6 (c)).
Experiment 4
The molar ratio for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method is set to
1:1.5 is fully ground after mixing well with silicon carbide by 7:2 after being sieved and is transferred to quartz reactor, then is placed in single mold microwave
In the cavity of device (device is shown in that Fig. 1, single mold microwave output power are 410~494w), and continuously it is passed through under nitrogen atmosphere and carries out
Calcining, after calcining in 526 seconds maximum temperature up to 600 DEG C (temperature-rise period is shown in Fig. 2 (a)), stop single mold microwave radiation and after
It is continuous to be passed through nitrogen, until material layer cools to room temperature.Finally 100 mesh will be crossed by calcined material layer and silicon carbide blend
Sieve pore separation；Material analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 2 (b), and TEM result is shown in Fig. 3 (d)；
ZnFe2O4:JCPDF 22-1012；ZnO:JCPDF36-1451).Take again calcining surplus material layer 0.1g absorption initial concentration be
Rhodamine b (RhB) solution 100mL of 4.96mg/L, after 16 minutes, the removal rate of RhB is 67.8% (being detailed in Fig. 6 (a))；
Under identical calcination temperature, the zinc ferrite of 600 DEG C of calcination reactions of Muffle furnace and tube furnace preparation, XRD analysis proof has zinc ferrite brilliant
(XRD characterization result is shown in Fig. 4 (a) and Fig. 4 (b) for body generation；ZnFe2O4:JCPDF 22-1012)；The reaction of RhB Dye Adsorption is gone
Except rate is respectively 4.65% (being detailed in Fig. 6 (b)) and 3.5% (being detailed in Fig. 6 (c)).
Experiment 5
The molar ratio for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method is set to
1:1.5 (is added without silicon carbide) and is transferred to quartz reactor, then is placed in the cavity of single mold microwave device after being fully ground sieving
(device is shown in that Fig. 1, single mold microwave output power are 410~494w), and be continuously passed through under nitrogen atmosphere and calcined, by 38 seconds
Maximum temperature stops single mold microwave and radiates and continue to be passed through nitrogen up to 300 DEG C (temperature-rise period is shown in Fig. 5 (a)) after calcining, until
Material layer cools to room temperature.Hole separation will be finally sieved with 100 mesh sieve by calcined material layer and silicon carbide blend；XRD points
Analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 5 (b)；ZnFe2O4:JCPDF 22-1012).Take calcining remaining again
Material layer 0.1g adsorbs methylenum careuleum (MB) solution 100mL that initial concentration is 10.0mg/L, after adsorption reaction in 30 minutes, MB
Removal rate be 4.49%；After the reaction was continued 2hr, the final removal rate of MB is 25.7%.
Experiment 6
The molar ratio for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method is set to
1:1.5 (is added without silicon carbide) and is transferred to quartz reactor, then is placed in the cavity of single mold microwave device after being fully ground sieving
(device is shown in that Fig. 1, single mold microwave output power are 410~494w), and be continuously passed through under nitrogen atmosphere and calcined, by 46 seconds
Maximum temperature stops single mold microwave and radiates and continue to be passed through nitrogen up to 400 DEG C (temperature-rise period is shown in Fig. 5 (a)) after calcining, until
Material layer cools to room temperature.Hole separation will be finally sieved with 100 mesh sieve by calcined material layer and silicon carbide blend；XRD points
Analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 5 (b)；ZnFe2O4:JCPDF 22-1012；ZnO:JCPDF 36-
1451).Methylenum careuleum (MB) solution 100mL that calcining surplus material layer 0.1g absorption initial concentration is 10.0mg/L is taken again, is passed through
After adsorption reaction in 30 minutes, the removal rate of MB is 3.65%；After the reaction was continued 2hr, the final removal rate of MB is 22.6%.
Experiment 7
The molar ratio for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method is set to
1:1.5 (is added without silicon carbide) and is transferred to quartz reactor, then is placed in the cavity of single mold microwave device after being fully ground sieving
(device is shown in that Fig. 1, single mold microwave output power are 410~494w), and be continuously passed through under nitrogen atmosphere and calcined, by 47 seconds
Maximum temperature stops single mold microwave and radiates and continue to be passed through nitrogen up to 500 DEG C (temperature-rise period is shown in Fig. 5 (a)) after calcining, until
Material layer cools to room temperature.Hole separation will be finally sieved with 100 mesh sieve by calcined material layer and silicon carbide blend；XRD points
Analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 5 (b)；ZnFe2O4:JCPDF 22-1012).Take calcining remaining again
Material layer 0.1g adsorbs methylenum careuleum (MB) solution 100mL that initial concentration is 10.0mg/L, and after absorption in 30 minutes, MB's is gone
Except rate is 0.43%；After the reaction was continued 2hr, the final removal rate of MB is 23%.
Experiment 8
The molar ratio for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method is set to
1:1.5 (is added without silicon carbide) and is transferred to quartz reactor, then is placed in the cavity of single mold microwave device after being fully ground sieving
(device is shown in that Fig. 1, single mold microwave output power are 410~494w), and be continuously passed through under nitrogen atmosphere and calcined, by 48 seconds
Maximum temperature stops single mold microwave and radiates and continue to be passed through nitrogen up to 600 DEG C (temperature-rise period is shown in Fig. 5 (a)) after calcining, until
Material layer cools to room temperature.Hole separation will be finally sieved with 100 mesh sieve by calcined material layer and silicon carbide blend；XRD points
Analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 5 (b)；ZnFe2O4:JCPDF 22-1012).Take calcining remaining again
Material layer 0.1g adsorbs methylenum careuleum (MB) solution 100mL that initial concentration is 10.0mg/L, after adsorption reaction in 30 minutes, MB
Removal rate be 2.2%；After the reaction was continued 2hr, the final removal rate of MB is 25.8%.
Experiment 9
The molar ratio for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method is set to
1:1.5 is fully ground after mixing well with silicon carbide by 7:2 after being sieved and is transferred to quartz reactor, then is placed in single mold microwave
In the cavity of device (device is shown in that Fig. 1, single mold microwave output power are 410~494w), and continuously it is passed through under nitrogen atmosphere and carries out
Calcining, after calcining in 470 seconds maximum temperature up to 400 DEG C (temperature-rise period is shown in Fig. 2 (a)), stop single mold microwave radiation and after
It is continuous to be passed through nitrogen, until material layer cools to room temperature.Finally 100 mesh will be crossed by calcined material layer and silicon carbide blend
Sieve pore separation；Phenetic analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 2 (b), and TEM result is shown in Fig. 3 (b)；
ZnFe2O4:JCPDF 22-1012；ZnO:JCPDF36-1451).Take again calcining surplus material layer 0.1g absorption initial concentration be
Rhodamine b (RhB) solution 100mL of 4.96mg/L, after 180 minutes visible light (λ > 420nm) catalytic degradations, RhB's is gone
Except rate be 85% (being detailed in Fig. 7 (a)), recycle secondly show be more than 73.1% degradation rate；Under identical calcination temperature,
The zinc ferrite of 400 DEG C of calcination reactions of Muffle furnace and tube furnace preparation, XRD analysis proof have zinc ferrite crystal to generate (XRD characterization knot
Fruit sees Fig. 4 (a) and Fig. 4 (b)；ZnFe2O4:JCPDF 22-1012)；15% respectively may be about to RhB Dye Adsorption reaction removal rate
(being detailed in Fig. 7 (a)) and 13% (being detailed in Fig. 7 (a)).
Experiment 10
By the molar ratio difference for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method
It is set to 1:1.0,1:1.2 and 1:1.5, is fully ground after being mixed well with silicon carbide by 7:2 after being sieved and is transferred to quartz reaction
Device, then (device is shown in that Fig. 1, single mold microwave output power are 410~494w) is placed in the cavity of single mold microwave device, and is continuously led to
Enter and calcined under nitrogen atmosphere, maximum temperature stops single mold microwave and radiate and continue up to 600 DEG C after calcining in 470 seconds
It is passed through nitrogen, until material layer cools to room temperature.It will finally be sieved with 100 mesh sieve by calcined material layer and silicon carbide blend
Hole separation；Phenetic analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 2 (b), ZnFe2O4:JCPDF 22-1012；
ZnO:JCPDF 36-1451).Take the methylenum careuleum (MB) that calcining surplus material layer 0.1g absorption initial concentration is 10mg/L respectively again
Solution 100mL, after absorption in 30 minutes, MB removal rate is respectively 32.7%, 40.5% and 45.2%；It again 360 minutes can
After light-exposed (λ > 420nm) catalytic degradation, MB removal rate distinguishes 86.1%, 94.5% and 95.5% (being detailed in Fig. 8).
Experiment 11
The molar ratio for the zinc ferrite precursor that citric acid coordination molysite and zinc salt are formed in above-mentioned sol-gel method is set to
1:1.0 and 1:1.2 is fully ground after mixing well with silicon carbide by 7:2 after being sieved and is transferred to quartz reactor, then is placed in list
In the cavity of mould microwave device (device is shown in that Fig. 1, single mold microwave output power are 410~494w), and continuously it is passed through nitrogen atmosphere
Under calcined, maximum temperature stops single mold microwave spoke up to 600 DEG C (temperature-rise period is shown in Fig. 2 (a)) after calcining in 526 seconds
It penetrates and continues to be passed through nitrogen, until material layer cools to room temperature.Calcined material layer and silicon carbide blend will finally be passed through
Sieve with 100 mesh sieve hole separation；Material analysis proof has zinc ferrite crystal to generate, and (XRD characterization result is shown in Fig. 2 (b)；ZnFe2O4:JCPDF
22-1012；ZnO:JCPDF 36-1451).The Luo Dan that calcining surplus material layer 0.1g absorption initial concentration is 4.96mg/L is taken again
Bright b (RhB) solution 100mL, after 16 minutes, the ZnFe of microwave nitrogen preparation2O4(N2, 1:1) removal RhB efficiency be
53% (being detailed in Fig. 9 (a)), and microwave air ZnFe2O4The ZnFe of (Air, 1:1) and Muffle furnace preparation2O4Remove the efficiency of RhB
Respectively 33.7% and 4.3%；Under identical calcination temperature, the ZnFe of microwave nitrogen preparation2O4(N2, 1:2) removal RhB efficiency
For 49.3% (being detailed in Fig. 9 (b)), and microwave air ZnFe2O4The ZnFe of (Air, 1:2) and Muffle furnace preparation2O4Remove RhB's
Efficiency is respectively 23.3% and 2.9% (being detailed in Fig. 9 (b)).
Although the present invention has been described by way of example and in terms of the preferred embodiments, embodiment does not limit the present invention.This hair is not being departed from
In bright spirit and scope, any equivalent change or retouch done also belongs to the protection scope of the present invention.Therefore the present invention
Protection scope should be based on the content defined in the claims of this application.
Claims (9)
1. a kind of single mold microwave reaction unit, which is characterized in that the single mold microwave reaction unit includes:
Regulated power supply (1), microwave power regulating device (2), microwave excitation generating device (3), single mold microwave reaction unit (4) and
Gas phase collection device (5)；
The regulated power supply (1) provides stable power source for entire single mold microwave reaction unit；
The regulated power supply (1) connects the microwave power regulating device (2)；The microwave power regulating device (2) passes through electricity
Stream input control line and control voltage control line are connect with the microwave excitation generating device (3)；The microwave excitation fills
It sets (3) and is connect with the single mold microwave reactor (4) by flange form；
The single mold microwave reaction unit (4) includes adjusting terminal short circuit piston (4.7) and single mold microwave reaction cavity (4.6)；
The single mold microwave reaction unit (4) is generated the microwave excitation generating device (3) by adjusting terminal short circuit piston (4.7)
Microwave pulse signal reflex go back, form amplitude, frequency and electromagnetic field direction of vibration is all the same, transmission direction is opposite reflection
Wave, and the microwave pulse incident wave generated with microwave excitation generating device (3) is in single mold microwave reaction cavity (4.6) interior shape
It is reacted at interference；Position by adjusting terminal short circuit piston (4.7) generate in the monofilm microwave reaction cavity (4.6) it is single and
The high power density energy field of high uniformity；
The gas phase collection device (5) includes nitrogen cylinder (5.1), mass flow controller (5.3), quartz reactor (5.4), stone
English fiber filter cylinder frame (5.5), reflux condenser (5.6), resin cartridge (5.8), toluene absorbing liquid (5.9), sodium hydroxide absorbing liquid
(5.10), gas dry pipe (5.11), gas sampling probe (5.12), portable gas chromatograph-mass spectrometer (5.13)；
Nitrogen in nitrogen cylinder (5.1) enters stone after gas valve (5.2) and mass flow controller (5.3) with certain flow
English reactor (5.4)；Quartz reactor (5.4) equipped with flying dust sample layer is placed in the reaction of the single mold microwave reactor (4)
In cavity, flying dust sample is after the single mold microwave reactor (4) carries out single mold microwave pyrolytic reaction, the vapor phase contaminants of generation
Quartz fibre filter cylinder frame (5.5), reflux condenser (5.6), resin cartridge (5.8), toluene absorbing liquid can successively be passed through with nitrogen
(5.9), sodium hydroxide absorbing liquid (5.10), gas dry pipe (5.11), gas sampling probe (5.12), eventually enter into portable
Gas chromatograph-mass spectrometer (5.13).
2. a kind of single mold microwave reaction unit for removing incineration of refuse flyash dioxin according to claim 1, feature
It is, the single mold microwave reactor (4) further include:
Circulator and water load (4.1), dual directional coupler (4.3), three screw tuners (4.4) and vertical waveguide microwave excitation
Chamber (4.5)；
The circulator and water load (4.1), dual directional coupler (4.3), three screw tuners (4.4), vertical waveguide microwave
Excitation cavity (4.5) is connected by flange form each other；The single mold microwave reactor (4) passes through dual directional coupler (4.3)
The microwave energy of transmitted in both directions is monitored, and adjusts the monofilm by three screw tuners (4.4) and terminal short circuit piston (4.7)
Microwave radiation energy field in microwave reaction cavity (4.6)；It is anti-that the circulator and water load (4.1) absorb the monofilm microwave
Cavity (4.6) is answered to be transmitted back to the unabsorbed microwave come.
3. a kind of single mold microwave reaction unit for removing incineration of refuse flyash dioxin according to claim 1, feature
It is, the single mold microwave reactor (4) further include:
Infrared radiation thermometer (4.8) and computer (4.9)；
The probe of the infrared radiation thermometer (4.8) is arranged in the two sides of monofilm microwave reaction cavity (4.6), infrared radiation thermometer
(4.8) temperature for connecting real-time monitoring sample with computer (4.9) changes with time.
4. a kind of single mold microwave reaction unit for removing incineration of refuse flyash dioxin according to claim 2, feature
It is, the single mold microwave reaction unit further include:
Recirculating cooling water system I (4.2)；
The recirculating cooling water system I (4.2) is in parallel with the circulator and water load (4.1), is that the circulator and water are negative
It carries 4.1 and recirculated cooling water is provided.
5. a kind of method for preparing iron acid zinc catalyst using single mold microwave, which is characterized in that described to be prepared using single mold microwave
The method of iron acid zinc catalyst includes:
Step S101 is based on Zn (CH3COO)2·2H2O、Fe(NO3)3·6H2O, citric acid and dehydrated alcohol, it is solidifying using colloidal sol-
Glue method synthesizes zinc ferrite precursor solution；
By Zn (CH3COO)2·2H2O and Fe (NO3)3·6H2O is dissolved in dehydrated alcohol according to the molar ratio of 1:2, stirring until
Solid is completely dissolved；It is added dropwise after citric acid is dissolved in dehydrated alcohol in above-mentioned solution, citric acid and heavy metal
The molar ratio of ion keeps 1:1~1:1.5；Obtain zinc ferrite precursor solution；
The zinc ferrite precursor solution of preparation is dried in step S102, grinds to the precursor after drying, sieving separating；
The ratio that step S103, the zinc ferrite precursor that sieving is obtained and Microwave Senstizer are 1:0~2:7 according to mass ratio
Example is put into quartz tube reactor after evenly mixing, then is placed in single mold microwave reaction cavity；Using single mold microwave to sol-gel
The zinc ferrite precursor of method synthesis carries out fumed pyrogenic.
6. a kind of method for preparing iron acid zinc catalyst using single mold microwave according to claim 5, which is characterized in that
It is passed through inert gas always in the entire reaction process of microwave-heating, keeps the intracorporal temperature of single mold microwave reaction chamber 300
~600 DEG C.
7. a kind of method for preparing iron acid zinc catalyst using single mold microwave according to claim 5, which is characterized in that institute
It states in step S103, Microwave Senstizer is silicon carbide, and partial size is 1.5~1.8mm.
8. a kind of method for preparing iron acid zinc catalyst using single mold microwave according to claim 5, which is characterized in that institute
It states in step S103, the inert atmosphere is nitrogen atmosphere.
9. a kind of method for preparing iron acid zinc catalyst using single mold microwave according to claim 5, which is characterized in that
The sieving separating of the zinc ferrite precursor uses the sieve of 100 mesh.
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| CN109663557A (en) * | 2018-12-24 | 2019-04-23 | 环境保护部华南环境科学研究所 | Remove the single mold microwave reaction unit and method of incineration of refuse flyash dioxin |
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