CN106345479A - Porous nanotube or nanofiber type ZnO/ZnFe2O4 composite photocatalyst and electrostatic spinning one-step preparation method thereof - Google Patents
Porous nanotube or nanofiber type ZnO/ZnFe2O4 composite photocatalyst and electrostatic spinning one-step preparation method thereof Download PDFInfo
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- CN106345479A CN106345479A CN201610602676.7A CN201610602676A CN106345479A CN 106345479 A CN106345479 A CN 106345479A CN 201610602676 A CN201610602676 A CN 201610602676A CN 106345479 A CN106345479 A CN 106345479A
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- 239000002131 composite material Substances 0.000 title claims abstract description 100
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 25
- 239000002121 nanofiber Substances 0.000 title claims abstract description 13
- 239000002071 nanotube Substances 0.000 title abstract description 9
- 229910001308 Zinc ferrite Inorganic materials 0.000 title abstract description 6
- NNGHIEIYUJKFQS-UHFFFAOYSA-L hydroxy(oxo)iron;zinc Chemical compound [Zn].O[Fe]=O.O[Fe]=O NNGHIEIYUJKFQS-UHFFFAOYSA-L 0.000 title abstract 5
- 238000009987 spinning Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000002243 precursor Substances 0.000 claims abstract description 28
- 150000003839 salts Chemical class 0.000 claims abstract description 28
- 239000012528 membrane Substances 0.000 claims abstract description 27
- 150000003751 zinc Chemical class 0.000 claims description 21
- 150000002505 iron Chemical class 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 7
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 239000004246 zinc acetate Substances 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 230000000593 degrading effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 45
- 229910052782 aluminium Inorganic materials 0.000 description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 14
- 239000011888 foil Substances 0.000 description 14
- 239000000835 fiber Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 230000005684 electric field Effects 0.000 description 7
- 230000005685 electric field effect Effects 0.000 description 7
- 238000003760 magnetic stirring Methods 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 6
- 229960004756 ethanol Drugs 0.000 description 5
- 239000002114 nanocomposite Substances 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 229910021392 nanocarbon Inorganic materials 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229940043267 rhodamine b Drugs 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000143432 Daldinia concentrica Species 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 150000001875 compounds Chemical group 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- SDGKUVSVPIIUCF-UHFFFAOYSA-N 2,6-dimethylpiperidine Chemical compound CC1CCCC(C)N1 SDGKUVSVPIIUCF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000231 atomic layer deposition Methods 0.000 description 1
- 230000000680 avirulence Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- LMDAGMAWWYVRJZ-UHFFFAOYSA-N ethanol;zinc Chemical compound [Zn].CCO LMDAGMAWWYVRJZ-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- -1 saccharide compound Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
-
- 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
- B01J37/342—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 electric, magnetic or electromagnetic fields, e.g. for magnetic separation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to the technical field of composite photocatalysts for organic pollutant degrading, and particularly relates to a porous nanotube or nanofiber type ZnO/ZnFe2O4 composite photocatalyst and an electrostatic spinning one-step preparation method thereof. The preparation method comprises the following steps: (1) preparation of a spinning precursor; (2) preparation of a Zn salt/Fe salt/PVP composite fibrous membrane by an electrostatic spinning method; (3) one-step preparation of the porous nanotube or nanofiber type ZnO/ZnFe2O4 composite photocatalyst. According to the method, after the electrostatic spinning step is completed, the composite photocatalyst with porous nanotube or nanofiber type ZnO/ZnFe2O4 is obtained by one step, so that the performance of the ZnO/ZnFe2O4 composite photocatalyst is further improved.
Description
Technical field
The invention belongs to organic pollutant degradation with composite photo-catalyst technical field and in particular to a kind of porous nanotube
Shape or nanometer fibrous zno/znfe2o4Composite photo-catalyst and its electrostatic spinning one one step preparation method.
Background technology
In recent years, because the fast development of modern industrialization is so that environment suffers serious polluting, including air pollution and
Water pollution, thus affecting orthobiosiss and the work of people, affects China's sustainable development view, therefore solves environmental pollution
Problem is extremely urgent, is also a challenging problem.The semi-conducting material of nanostructured is in photocatalytic degradation Organic substance
Aspect shows superior performance, can be with effectively solving problem of environmental pollution.Nanometer zno is one of common semiconductor material, tool
There are preferable photoelectric properties, photocatalysis performance and good chemical stability, the advantage such as avirulence.Further, since the forbidden band of zno
Wider width, by the ultraviolet excitation of the minor proportion in sunlight, and due to its quantum size effect, can only make the suction of light
The raw blue shift of transmitting-receiving, leads to the utilization rate to sunlight too low, greatly limit the practical application of zno, is unfavorable for that it is real in industry
Development in trampling.A kind of less znfe of energy gap of therefore necessary combination2o4Material is improving it to the sensitivity of light and right
The utilization rate of sunlight.
Nanometer znfe2o4It is a kind of more visible light catalyst of present research and magnetic material, its energy gap is less,
Sensitive to visible ray, nontoxic, chemical stability is good, and spectral response range is big, accordingly, it is capable to effectively utilize sunlight, however, its
Photocatalytic activity is not high, and the efficiency of Direct Resolution organic pollution is low.Zno and znfe2o4Being combined of bi-material, can be with advantage
Complementation, (400-800nm accounts for sunlight so as to expand visible region to effective absorption of light to play synergism
50%), improve the utilization rate to sunlight of composite, and composite is nontoxic, will not bring secondary pollution to environment.
Due to nanometer znfe2o4It is a kind of magnetic material, can give composite certain magnetic property, be easy to magnetic recovery and recycle.
Preparation zno/znfe at present2o4The method of composite photo-catalyst have sol-gal process, coprecipitation, hydrothermal synthesis method,
Method of electrostatic spinning etc..zno/znfe2o4The pattern of composite has nanoparticle, hollow ball, nanofiber etc..Wherein zno/
znfe2o4Nanoparticle typically adopts hydro-thermal method to prepare, and easily reunites, has a strong impact on its dispersibility, and then affects its performance.As
Cn 101759146b discloses zno/znfe2o4The synthetic method of composite Nano hollow ball, the first step is water-soluble with saccharide compound
Liquid, through Hydrothermal Synthesiss, prepares nano carbon microsphere as template；Carbon ball template is dispersed in containing zinc salt, iron salt and weak base second step
Alcoholic solution in, at a certain temperature react 4-20h, cooled, be centrifugally separating to obtain metal hydroxidess cladding Nano carbon balls；
3rd step, metal hydroxidess cladding Nano carbon balls is calcined 2-10h at 450-800 DEG C, obtains zno/znfe2o4Composite Nano
Hollow ball.Cn 102861586b discloses the zno/znfe of nucleocapsid structure2o4Composite photo-catalyst, the first step adopts divalent zinc
Salt, trivalent iron salt are dissolved in dehydrated alcohol, and naoh adjusts ph value, and then, under the conditions of 90-250 DEG C, Hydrothermal Synthesiss at least react
5h, cools down Magneto separate, and washing is dried to obtain znfe2o4, as core template, second step, by znfe2o4It is dispersed in as core template
In zinc salt ethanol solution, add alkali liquor, heating, cool down Magneto separate, washing is dried to obtain the zno/znfe of nucleocapsid structure2o4Compound
Photocatalyst.Cn103103634b discloses one kind and prepares znfe using coaxial electrostatic co-spun yarn method2o4Nano-particle-zno nanometer
The preparation method of fiber composite nano material, the ethanol solution that the first step is prepared containing zinc salt and high molecular polymer spins as kernel
Silk solution, it is molten as shell spinning that second step prepares the ethanol solution containing divalent zinc salt, trivalent iron salt and high molecular polymer
Liquid；Then kernel and shell spinning liquid are loaded coaxial electrostatic cospinning silk device, carry out common-battery spinning, obtain composite Nano fine
Dimension, the 3rd step carries out heating anneal to composite nano fiber, cooling, obtains znfe2o4Nano-particle-zno nanofiber is combined and receives
Rice material, wherein zno is nanofiber, znfe2o4Being attached to zno for nano-particle is on nanofiber surface.
A kind of znfe of cn103094558b2o4The preparation method of based nano composite material, the first step is by zinc salt, iron salt and organic complexing agent
It is mixed to get slurry in a solvent, then slurry carries out solidification at 40-200 DEG C and becomes xerogel；Second step is by xerogel o again2
At atmosphere and 350-850 DEG C, calcining cooling obtains znfe2o4Based nano composite material, described znfe2o4The nano combined material of base
Material is by the znfe with spinel structure2o4The offspring that nano-particle is reunited with metal oxide nanoparticles.As
(preparation of zinc ferrite nano composite structure and its photocatalysis characteristic research, Liu He, Changchun University of Science and Technology's master thesis) report
Road zno/znfe2o4The preparation method of nano-composite fiber, the first step adopts method of electrostatic spinning containing zinc salt, iron salt and will gather
The ethanol solution spinning of compound forms znfe2o4Precursor fibre film, be then passed through high-temperature calcination technique and obtain znfe2o4Receive
Rice fiber；Second step, with znfe2o4Nanofiber is base material, deposits zno thin film using technique for atomic layer deposition, then through moving back
Fiery process, to sample treatment, prepares one-dimensional core shell znfe2o/zno4Nano-composite fiber.
Therefore, it can be said that existing zno/znfe2o4Composite photo-catalyst synthetic method craft is complicated, specific surface area is low, and
Not with regard to preparing porous nanotube or nanometer fibrous zno/znfe2o4The report of composite photo-catalyst.And come on the whole
See, prepare zno/znfe at present2o4The complex process of composite, and the zno/znfe preparing2o4Pattern be hollow ball, core/
Shell compound particle, znfe2o4Nano-particle-zno nanofiber composite nano materials or core shell znfe2o4/ zno composite fibre.
Additionally, existing process is not reported prepares porous nanotube or nanometer fibrous zno/znfe using method of electrostatic spinning one step2o4Multiple
The method of closing light catalyst.
Content of the invention
For solving the deficiencies in the prior art, the invention provides a kind of porous nano tubulose or nanometer fibrous zno/
znfe2o4Composite photo-catalyst and its electrostatic spinning one one step preparation method.
A kind of porous nano tubulose or nanometer fibrous zno/znfe2o4The electrostatic spinning one step preparation of composite photo-catalyst
Method, comprises the following steps:
1) preparation of spinning presoma
Mol ratio is 1.0:(0～2.0) divalent zinc salt of (not comprising 0 and 2.0 two endpoint value) is molten with trivalent iron salt
In organic solvent, add Polyvinylpyrrolidone (pvp), the presoma that magnetic agitation obtains brownish red homogeneous transparent is molten
Liquid.
Step 1) in:
Divalent zinc salt is selected from any one in zinc acetate, zinc nitrate, zinc sulfate or zinc chloride；
Trivalent iron salt is selected from any one in iron chloride, ferric nitrate, iron acetate, iron sulfate or ferric acetyl acetonade；
Organic solvent is selected from ethanol, methanol or n, any one in n- dimethylformamide；
The molecular weight of pvp is more than 900000；
Divalent zinc salt and the gross mass of trivalent iron salt are 0.12～0.25g/ml with the mass volume ratio of organic solvent；
Divalent zinc salt and the gross mass of trivalent iron salt are 1.0～1.6 with the mass ratio of pvp；
In precursor solution, the concentration of divalent zinc salt is 0.042～0.10g/ml；
In precursor solution, the concentration of trivalent iron salt is 0.08～0.15g/ml.
2) method of electrostatic spinning preparation zn salt/fe salt/pvp composite cellulosic membrane
With step 1) obtain precursor solution and carry out electrostatic spinning for spinning liquid, obtain zn salt/fe salt/pvp composite fibre
Film.
Step 2) in:
Spinning voltage 10～20kv；
Accept distance 10～20cm；
Air humidity 25～50%.
3) porous nano tubulose or nanometer fibrous zno/znfe2o4One step preparation of composite photo-catalyst
By step 2) zn salt/fe salt/high molecular polymer composite cellulosic membrane of obtaining calcined, and obtains porous nanotube
Shape or nanometer fibrous zno/znfe2o4Composite photo-catalyst.
Step 3) in:
Heating rate is 0.5～5 DEG C/min；
Calcining heat is 500～600 DEG C；
Calcination time 2～4h.
Further:
When divalent zinc salt concentration be more than or equal to 0.042 and less than or equal to 0.075g/ml, trivalent iron salt concentration be more than etc.
In 0.08 and less than or equal to 0.12g/ml when, obtain porous nano tubulose zno/znfe2o4Composite photo-catalyst；
When divalent zinc salt concentration be more than 0.075 and less than or equal to 0.10g/ml, trivalent iron salt concentration be more than 0.12 and
During less than or equal to 0.15g/ml, obtain nanometer fibrous zno/znfe2o4Composite photo-catalyst.
There is marginal value in the concentration of divalent zinc salt and trivalent iron salt, below marginal value, obtain porous nano tubulose zno/
znfe2o4Composite photo-catalyst, in the case of more than marginal value, obtains nanometer fibrous zno/znfe2o4Composite photocatalyst
Agent.
Present invention also offers the porous nano tubulose being prepared according to said method or nanometer fibrous zno/
znfe2o4Composite photo-catalyst.
By porous nano tubulose provided by the present invention or nanometer fibrous zno/znfe2o4Composite photo-catalyst quiet
Electrospun one one step preparation method, can be after electrostatic spinning step, and a step obtains with porous nano tubulose or nanometer fibrous
zno/znfe2o4Composite photo-catalyst, further improve zno/znfe2o4The performance of composite photo-catalyst.
Brief description
Fig. 1 is porous nano tubulose zno/znfe provided by the present invention2o4Composite photo-catalyst scanning electron microscope (SEM) photograph.
Fig. 2 is porous nano tubulose zno/znfe provided by the present invention2o4The scanning electron microscope of composite photo-catalyst cross section
Figure.
Fig. 3 is nanometer fibrous zno/znfe provided by the present invention2o4The scanning electron microscope (SEM) photograph of composite photo-catalyst.
Fig. 4 is nanometer fibrous zno/znfe provided by the present invention2o4The scanning electron microscope of composite photo-catalyst cross section
Figure.
Fig. 5 is porous nano tubulose zno/znfe provided by the present invention2o4The transmission electron microscope photo of composite photo-catalyst.
Fig. 6 is porous nano tubulose zno/znfe provided by the present invention2o4Composite photo-catalyst High-Resolution Map.
Fig. 7 is porous nano tubulose zno/znfe provided by the present invention2o4The xrd spectrogram of composite photo-catalyst.
Specific embodiment
Hereinafter the principle and feature of the present invention is described, illustrated embodiment is served only for explaining the present invention, is not intended to
Limit the scope of the present invention.
In embodiment, the catalytic performance test method of photocatalyst is as follows:
Weigh the photocatalyst of 50mg this patent preparation, be dispersed in the rhodamine b aqueous solution that 50ml concentration is 10mg/l,
Magnetic agitation 30min reaches adsorption-desorption balance to suspension in the dark, irradiates Imitating sunlight catalytic in 500w xenon source
Degraded rhodamine b solution, in certain time interval, samples, centrifugation removes photocatalyst and utilizes ultraviolet-uisible spectrophotometer
The residual concentration of rhodamine b in test solution, after reaction 150min, stops experiment.
Embodiment 1
Porous nano tubulose zno/znfe2o4The preparation of composite photo-catalyst 1: by the nitre of the zinc acetate of 0.33g and 0.61g
Sour ferrum (mol ratio 1:1) is added to 6ml n, in n- dimethylformamide, is placed on magnetic stirring apparatuss quick stirring so as to molten
0.9g pvp is finally added to above-mentioned solution by solution, quickly stirs 4h, forms the transparent precursor solution of uniform brownish red.
The precursor solution preparing is moved in spinning syringe, connects high voltage power supply, receptor aluminum foil plate connects
Negative pole, wherein syringe needle internal diameter about 1mm, set spinning voltage 12kv, accept apart from 14cm, wherein air humidity controls in 25-
50%.Turn on the power, precursor solution stretches ejection in the presence of high voltage electric field, form a taper at shower nozzle
Taylor bores, and under high voltage electric field effect, solution continues to move to the aluminum foil plate with low potential, is finally formed on receiver board
The fibrous membrane of yellow, thus obtained zn salt/fe salt/pvp composite cellulosic membrane using method of electrostatic spinning one step.
Composite cellulosic membrane is put in temperature programming Muffle furnace, heating rate is set as 1 DEG C/min, 500 DEG C of calcining 3.5h,
Obtain porous nano tubulose zno/znfe2o4Composite photo-catalyst, its photocatalytic degradation efficiency is 82%.
Embodiment 2
Porous nano tubulose zno/znfe2o4The preparation of composite photo-catalyst 2: by the acetyl of the zinc acetate of 0.44g and 0.7g
Acetone ferrum (mol ratio 1:1) is added to 6ml n, in n- dimethylformamide, be placed on magnetic stirring apparatuss quick stirring so as to
0.9g Polyvinylpyrrolidone is finally added to above-mentioned solution by dissolving, quickly stirs 4h, forms the transparent forerunner of uniform brownish red
Liquid solution.
The precursor solution preparing is moved in spinning syringe, connects high voltage power supply, receptor aluminum foil plate connects
Negative pole, wherein syringe needle internal diameter about 1mm, set spinning voltage 12kv, accept apart from 14cm, wherein air humidity controls in 25-
50%.Turn on the power, precursor solution stretches ejection in the presence of high voltage electric field, form a taper at shower nozzle
Taylor bores, and under high voltage electric field effect, solution continues to move to the aluminum foil plate with low potential, is finally formed on receiver board
The fibrous membrane of yellow, thus obtained zn salt/fe salt/pvp composite cellulosic membrane using method of electrostatic spinning one step.
Composite cellulosic membrane is put in temperature programming Muffle furnace, heating rate is set as 1 DEG C/min, 550 DEG C of calcining 3h, obtains
To porous nano tubulose zno/znfe2o4Composite photo-catalyst, its degradation efficiency is 97%.
Embodiment 3
Porous nano tubulose zno/znfe2o4The preparation of composite photo-catalyst 3: by the second of the zinc acetate of 0.42g and 0.50g
Acyl acetone ferrum (mol ratio 1:0.74) is added in 6ml ethanol, is placed on magnetic stirring apparatuss quick stirring so as to dissolve,
Afterwards 0.95g pvp is added to above-mentioned solution, quickly stirs 4h, form the transparent precursor solution of uniform brownish red.
The precursor solution preparing is moved in spinning syringe, connects high voltage power supply, receptor aluminum foil plate connects
Negative pole, wherein syringe needle internal diameter about 1mm, set spinning voltage 11kv, accept apart from 17cm, wherein air humidity controls in 25-
50%.Turn on the power, precursor solution stretches ejection in the presence of high voltage electric field, form a taper at shower nozzle
Taylor bores, and under high voltage electric field effect, solution continues to move to the aluminum foil plate with low potential, is finally formed on receiver board
The fibrous membrane of yellow, thus obtained zn salt/fe salt/pvp composite cellulosic membrane using method of electrostatic spinning one step.
Composite cellulosic membrane is put in temperature programming Muffle furnace, heating rate is set as 2 DEG C/min, 500 DEG C of calcining 3h, obtains
To porous nano tubulose zno/znfe2o4Composite photo-catalyst, its degradation efficiency is 73%.
Embodiment 4
Porous nano tubulose zno/znfe2o4The preparation of composite photo-catalyst 4: by the chlorine of the zinc chloride of 0.37g and 0.66g
Change ferrum (mol ratio 1:1.5) and be added to 6ml n, in n- dimethylformamide, be placed on magnetic stirring apparatuss quick stirring so as to
1.0g pvp is finally added to above-mentioned solution by dissolving, quickly stirs 4h, forms the transparent precursor solution of uniform brownish red.
The precursor solution preparing is moved in spinning syringe, connects high voltage power supply, receptor aluminum foil plate connects
Negative pole, wherein syringe needle internal diameter about 1mm, set spinning voltage 13kv, accept apart from 16cm, wherein air humidity controls in 25-
50%.Turn on the power, precursor solution stretches ejection in the presence of high voltage electric field, form a taper at shower nozzle
Taylor bores, and under high voltage electric field effect, solution continues to move to the aluminum foil plate with low potential, is finally formed on receiver board
The fibrous membrane of yellow, thus obtained zn salt/fe salt/pvp composite cellulosic membrane using method of electrostatic spinning one step.
Composite cellulosic membrane is put in temperature programming Muffle furnace, heating rate is set as 1.5 DEG C/min, 550 DEG C of calcining 3h,
Obtain porous nano tubulose zno/znfe2o4Composite photo-catalyst, its photocatalytic degradation efficiency is 83%.
Embodiment 5
Nanometer fibrous zno/znfe2o4The preparation of composite photo-catalyst 1: by the acetyl of the zinc acetate of 0.55g and 0.88g
Acetone ferrum (mol ratio 1:1) is added to 6ml n, in n- dimethylformamide, be placed on magnetic stirring apparatuss quick stirring so as to
1.0g pvp is finally added to above-mentioned solution by dissolving, quickly stirs 4h, forms the transparent precursor solution of uniform brownish red.
The precursor solution preparing is moved in spinning syringe, connects high voltage power supply, receptor aluminum foil plate connects
Negative pole, wherein syringe needle internal diameter about 1mm, set spinning voltage 11kv, accept apart from 15cm, wherein air humidity controls in 25-
50%.Turn on the power, precursor solution stretches ejection in the presence of high voltage electric field, form a taper at shower nozzle
Taylor bores, and under high voltage electric field effect, solution continues to move to the aluminum foil plate with low potential, is finally formed on receiver board
The fibrous membrane of yellow, thus obtained zn salt/fe salt/pvp composite cellulosic membrane using method of electrostatic spinning one step.
Composite cellulosic membrane is put in temperature programming Muffle furnace, heating rate is set as 1 DEG C/min, 550 DEG C of calcining 3h, obtains
To nanometer fibrous zno/znfe2o4Composite photo-catalyst, its photocatalytic degradation efficiency is 90%.
Embodiment 6
Nanometer fibrous zno/znfe2o4The preparation of composite photo-catalyst 2: by the acetyl of the zinc nitrate of 0.49g and 0.87g
Acetone ferrum (mol ratio 1:1.5) is added in 6ml methanol, is placed on magnetic stirring apparatuss quick stirring so as to dissolving, finally will
0.9g Polyvinylpyrrolidone is added to above-mentioned solution, quickly stirs 4h, forms the transparent precursor solution of uniform brownish red.
The precursor solution preparing is moved in spinning syringe, connects high voltage power supply, receptor aluminum foil plate connects
Negative pole, wherein syringe needle internal diameter about 1mm, set spinning voltage 13kv, accept apart from 17cm, wherein air humidity controls in 25-
50%.Turn on the power, precursor solution stretches ejection in the presence of high voltage electric field, form a taper at shower nozzle
Taylor bores, and under high voltage electric field effect, solution continues to move to the aluminum foil plate with low potential, is finally formed on receiver board
The fibrous membrane of yellow, thus obtained zn salt/fe salt/pvp composite cellulosic membrane using method of electrostatic spinning one step.
Composite cellulosic membrane is put in temperature programming Muffle furnace, heating rate is set as 3 DEG C/min, 550 DEG C of calcining 3h, obtains
To nanometer fibrous zno/znfe2o4Composite photo-catalyst, its photocatalytic degradation efficiency is 79%.
Embodiment 7
Nanometer fibrous zno/znfe2o4The preparation of composite photo-catalyst 3: by the sulphuric acid of the zinc sulfate of 0.48g and 0.89g
Ferrum (mol ratio 1:1) is added to 6ml n, in n- dimethylformamide, is placed on magnetic stirring apparatuss quick stirring so as to molten
0.9g Polyvinylpyrrolidone is finally added to above-mentioned solution by solution, quickly stirs 3.5h, before the uniform brownish red of formation is transparent
Drive liquid solution.
The precursor solution preparing is moved in spinning syringe, connects high voltage power supply, receptor aluminum foil plate connects
Negative pole, wherein syringe needle internal diameter about 1mm, set spinning voltage 13.5kv, accept apart from 16cm, wherein air humidity controls in 25-
50%.Turn on the power, precursor solution stretches ejection in the presence of high voltage electric field, form a taper at shower nozzle
Taylor bores, and under high voltage electric field effect, solution continues to move to the aluminum foil plate with low potential, is finally formed on receiver board
The fibrous membrane of yellow, thus obtained zn salt/fe salt/pvp composite cellulosic membrane using method of electrostatic spinning one step.
Composite cellulosic membrane is put in temperature programming Muffle furnace, heating rate is set as 2.5 DEG C/min, 560 DEG C of calcining 3h,
Obtain nanometer fibrous zno/znfe2o4Composite photo-catalyst, its photocatalytic degradation efficiency is 81%.
Effect example
Fig. 1 is porous nano tubulose zno/znfe2o4Composite photo-catalyst scanning electron microscopic picture, as can be seen from the figure spins
Silk fiber film macromolecule after high-temperature calcination decomposes completely, the preferable tubular structure of the pattern being made up of inorganic nano-particle,
zno/znfe2o4Composite photo-catalyst is nano tube structure, its average diameter about 200nm, and has much nano level on tube wall
Aperture, porous nano tubular construction makes zno/znfe2o4Composite photo-catalyst has larger specific surface area, is greatly improved it
Photocatalytic activity.
Fig. 2 is porous nano tubulose zno/znfe2o4Composite photo-catalyst cross-sectional scans electron microscope, can from figure
Go out zno/znfe2o4There is preferable tubular structure, pipe mean inside diameter about 100nm, tube wall is made up of countless nanoscale small particles
, and much nano level apertures are had on tube wall.
Fig. 3 is nanometer fibrous zno/znfe2o4The scanning electron microscope (SEM) photograph of composite photo-catalyst, as can be seen from the figure zno/
znfe2o4There are good nanofibrous structures, average fibre diameter about 185m, fiber surface can be clearly seen about 30nm's
Small particles, fiber surface is coarse and atresia.
Fig. 4 is nanometer fibrous zno/znfe2o4The scanning electron microscope (SEM) photograph of composite photo-catalyst cross section, can be clear from figure
Chu finds out zno/znfe2o4Composite photo-catalyst is solid fibers shape structure, and fiber surface is made up of countless nanometer small particles.
Fig. 5 is porous nano tubulose zno/znfe2o4The transmission electron microscope photo of composite photo-catalyst, as can be seen from the figure
zno/znfe2o4Composite photo-catalyst has typical porous nano tubular construction, pipe average diameter about 200nm, and tube wall has substantially
Loose structure.
Fig. 6 is porous nano tubulose zno/znfe2o4Composite photo-catalyst high-resolution picture, as can be seen from the figure typical case
Zno and znfe2o4Hetero-junctions, illustrates to be successfully prepared porous nano tubulose zno/znfe using electrostatic spinning one-step method2o4Multiple
Closing light catalyst.
Fig. 7 is porous nano tubulose zno and znfe2o4The xrd spectrogram of composite photo-catalyst, as we can see from the figure
2theta occurs in that znfe at 29.93,35.30,42.90,53.17,56.69,62.25 and 73.50 °2o4Characteristic diffraction peak,
31.58,34.30,36.08,47.58,62.40,66.98,68.08 and 68.84 ° occur in that zno characteristic diffraction peak, do not observe
To the peak of other oxides, the zno/znfe of this explanation present invention preparation2o4Only have zno and znfe in composite photo-catalyst2o4Two
Plant crystal.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvement made etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of porous nano tubulose or nanometer fibrous zno/znfe2o4The electrostatic spinning one step preparation side of composite photo-catalyst
Method is it is characterised in that comprise the following steps:
1) preparation of spinning presoma
Mol ratio is 1.0:(0～2.0) divalent zinc salt and trivalent iron salt be dissolved in organic solvent, add pvp, magnetic force stirs
Mix the precursor solution obtaining brownish red homogeneous transparent；
2) method of electrostatic spinning preparation zn salt/fe salt/pvp composite cellulosic membrane
With step 1) obtain precursor solution and carry out electrostatic spinning for spinning liquid, obtain zn salt/fe salt/pvp composite cellulosic membrane；
3) porous nano tubulose or nanometer fibrous zno/znfe2o4One step preparation of composite photo-catalyst
By step 2) zn salt/fe salt/pvp composite cellulosic membrane of obtaining calcined, and obtains porous nano tubulose or nanofiber
Shape zno/znfe2o4Composite photo-catalyst.
2. porous nano tubulose according to claim 1 or nanometer fibrous zno/znfe2o4The electrostatic of composite photo-catalyst
Spinning one one step preparation method is it is characterised in that step 1) in:
Divalent zinc salt is selected from any one in zinc acetate, zinc nitrate, zinc sulfate or zinc chloride；
Trivalent iron salt is selected from any one in iron chloride, iron acetate, iron sulfate, ferric nitrate or ferric acetyl acetonade；
Organic solvent is selected from ethanol, methanol or n, any one in n- dimethylformamide；
The molecular weight of pvp is more than 900000；
Divalent zinc salt and the gross mass of trivalent iron salt are 0.12～0.25g/ml with the mass volume ratio of organic solvent；
Divalent zinc salt and the gross mass of trivalent iron salt are 1.0～1.6 with the mass ratio of pvp；
In precursor solution, the concentration of divalent zinc salt is 0.042～0.10g/ml；
In precursor solution, the concentration of trivalent iron salt is 0.08～0.15g/ml.
3. porous nano tubulose according to claim 1 or nanometer fibrous zno/znfe2o4The electrostatic of composite photo-catalyst
Spinning one one step preparation method is it is characterised in that step 2) in, the technical parameter of electrostatic spinning is as follows:
Spinning voltage 10～20kv；
Accept distance 10～20cm；
Air humidity 25～50%.
4. porous nano tubulose according to claim 1 or nanometer fibrous zno/znfe2o4The electrostatic of composite photo-catalyst
Spinning one one step preparation method is it is characterised in that step 3) in, the technical parameter of calcining is as follows:
Heating rate is 0.5～5 DEG C/min；
Calcining heat is 500～600 DEG C；
Calcination time 2～4h.
5. porous nano tubulose according to claim 1 or nanometer fibrous zno/znfe2o4The electrostatic of composite photo-catalyst
Spinning one one step preparation method it is characterised in that: when divalent zinc salt concentration be more than or equal to 0.042 and less than or equal to 0.075g/ml,
When the concentration of trivalent iron salt is more than or equal to 0.08 and is less than or equal to 0.12g/ml, obtain porous nano tubulose zno/znfe2o4Compound
Photocatalyst.
6. porous nano tubulose according to claim 1 or nanometer fibrous zno/znfe2o4The electrostatic of composite photo-catalyst
Spinning one one step preparation method it is characterised in that: when divalent zinc salt concentration be more than 0.075 and be less than or equal to 0.10g/ml, trivalent
When the concentration of iron salt is more than 0.12 and is less than or equal to 0.15g/ml, obtain nanometer fibrous zno/znfe2o4Composite photo-catalyst.
7. a kind of porous nano tubulose being prepared according to the arbitrary described preparation method of claim 1 to 6 or nanofiber
Shape zno/znfe2o4Composite photo-catalyst.
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