CN109731617A - A kind of Fe3O4/ polypyrrole/polyaniline/TiO2The preparation method of/ZnO composite material - Google Patents
A kind of Fe3O4/ polypyrrole/polyaniline/TiO2The preparation method of/ZnO composite material Download PDFInfo
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- CN109731617A CN109731617A CN201811525253.5A CN201811525253A CN109731617A CN 109731617 A CN109731617 A CN 109731617A CN 201811525253 A CN201811525253 A CN 201811525253A CN 109731617 A CN109731617 A CN 109731617A
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- polypyrrole
- polyaniline
- tio
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 229920000128 polypyrrole Polymers 0.000 title claims abstract description 123
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 102
- 239000002131 composite material Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 121
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 42
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 32
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 19
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- WHMDKBIGKVEYHS-IYEMJOQQSA-L Zinc gluconate Chemical compound [Zn+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O WHMDKBIGKVEYHS-IYEMJOQQSA-L 0.000 claims abstract description 12
- 239000006185 dispersion Substances 0.000 claims abstract description 12
- 239000011670 zinc gluconate Substances 0.000 claims abstract description 12
- 235000011478 zinc gluconate Nutrition 0.000 claims abstract description 12
- 229960000306 zinc gluconate Drugs 0.000 claims abstract description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 11
- 150000003233 pyrroles Chemical class 0.000 claims abstract description 10
- 235000019441 ethanol Nutrition 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 6
- 235000011118 potassium hydroxide Nutrition 0.000 claims abstract description 6
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 claims abstract description 6
- 235000019252 potassium sulphite Nutrition 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 23
- 229910021641 deionized water Inorganic materials 0.000 claims description 23
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 229960004756 ethanol Drugs 0.000 claims description 7
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 206010011224 Cough Diseases 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000002525 ultrasonication Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 19
- 238000007146 photocatalysis Methods 0.000 abstract description 17
- 230000005415 magnetization Effects 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000007774 longterm Effects 0.000 abstract description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 84
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 55
- 239000011787 zinc oxide Substances 0.000 description 42
- 239000004408 titanium dioxide Substances 0.000 description 7
- 229940056319 ferrosoferric oxide Drugs 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920006389 polyphenyl polymer Polymers 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000004069 differentiation Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000003403 water pollutant Substances 0.000 description 2
- NAOLWIGVYRIGTP-UHFFFAOYSA-N 1,3,5-trihydroxyanthracene-9,10-dione Chemical compound C1=CC(O)=C2C(=O)C3=CC(O)=CC(O)=C3C(=O)C2=C1 NAOLWIGVYRIGTP-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention belongs to photocatalysis technology fields, and in particular to a kind of Fe3O4/ polypyrrole/polyaniline/TiO2The preparation method of/ZnO composite material;Fe is prepared with frerrous chloride, potassium sulfite, polyvinylpyrrolidone and potassium hydroxide isothermal reaction first3O4, pyrroles, ethyl alcohol and concentrated hydrochloric acid are then separately added into Fe3O4In dispersion liquid, Fe is obtained3O4/ polypyrrole, then aniline monomer, hydrochloric acid and ammonium persulfate are added to Fe3O4In/polypyrrole dispersion liquid, Fe is prepared3O4/ polypyrrole/polyaniline, by way of sol-gel, in Fe3O4/ polypyrrole/polyaniline surface coats TiO2, finally, by Fe3O4/ polypyrrole/polyaniline/TiO2/ ZnO is scattered in acetone, adds ammonium hydroxide, ultrasonic wave dispersion plus zinc gluconate reaction, Fe is prepared3O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material；Preparation method of the present invention is simple, and composite material possesses higher saturation magnetization and the magnetic rate of recovery, and the Fe being prepared3O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material possesses long-term, efficient photocatalysis performance and magnetic recyclability.
Description
Technical field
The invention belongs to photocatalysis technology fields, and in particular to a kind of Fe3O4/ polypyrrole/polyaniline/TiO2/ ZnO is multiple
The preparation method of condensation material.
Background technique
Along with industrial expansion, environmental pollution has become survival and development of mankind and needs the significant problem that solves, and its
Middle water pollution is even more the health of the directly threat mankind, therefore how the pollutant in efficient degradation water body just becomes whole world section
Scholar needs the project captured, and compared with traditional water pollutant processing technique, Photocatalitic Technique of Semiconductor has efficient, low
Carbon, environmental protection, low toxicity, it is low in cost the advantages that, especially developed in recent years it is a series of have visible light-responded photochemical catalyst
So that this technology is using having great application prospect in sunlight processing environment pollutant, this kind of material is also urged as light
Change the hot spot of research field.
Titanium dioxide is common photocatalytic degradation material, although having under visible light illumination condition to water pollutant
Higher Photocatalytic activity, but their Shortcomings in terms of post-processing and recycling and reusing, such as need high speed
Centrifugation, addition precipitating reagent etc., are unfavorable for practical application.
The features such as ferroso-ferric oxide is a kind of excellent soft magnetic materials, has non-toxic inexpensive, easily prepares, magnetic good, commonly uses
The carrier and photochemical catalyst of photocatalyst are compound to be recycled well, still, the introducing meeting of ferroso-ferric oxide
The photocatalysis performance of composite material is reduced, this is because the electronics of ferroso-ferric oxide is easier to migrate into titanium dioxide, from
And the separative efficiency of electronics and empty electronics pair is affected, it is reduced so as to cause the photocatalysis performance of composite material.
Summary of the invention
It is an object of the invention to: a kind of Fe is provided3O4/ polypyrrole/polyaniline/TiO2The preparation side of/ZnO composite material
Method, the present invention are improved the separative efficiency in light induced electron and hole by the synergistic effect between titanium dioxide, zinc oxide, passed through
To Fe3O4Polypyrrole modifying is carried out, and carries out polyaniline-coated, improves the magnetic recyclability of composite material, meanwhile, it reduces
Fe3O4The photocatalysis performance of titanium dioxide is influenced.
A kind of Fe3O4/ polypyrrole/polyaniline TiO2The preparation method of/ZnO composite material, includes the following steps:
S1、Fe3O4Preparation: by frerrous chloride, potassium sulfite, polyvinylpyrrolidone and potassium hydroxide according to mass ratio 1.5:
0.8:0.7:0.7 is dissolved in deionized water, and under helium protection, isothermal reaction, reaction temperature is 160-180 DEG C of reaction time
For 7-9h, Fe is prepared after separating, washing and drying3O4；
S2、Fe3O4The preparation of/polypyrrole: the Fe that step S1 is prepared3O4It is scattered in deionized water, Fe3O4Quality with
The solid-to-liquid ratio of deionized water volume is 1g:200mL, then by pyrroles and ethyl alcohol, concentrated hydrochloric acid is separately added into Fe3O4In dispersion liquid, wherein
Deionized water, pyrroles, ethyl alcohol, concentrated hydrochloric acid volume ratio are 100:0.1:10:3, uniform stirring 2h, the product deionized water of acquisition
It is rinsed with dehydrated alcohol, for 24 hours, Fe is prepared in vacuum drying3O4/ polypyrrole；
S3、Fe3O4The preparation of/polypyrrole/polyaniline: Fe is prepared in step S23O4/ polypyrrole is scattered in deionized water,
Fe3O4The solid-to-liquid ratio of/polypyrrole quality and deionized water volume is 1g:100mL, and aniline monomer is added, and salt is added in ultrasonic 10min
Acid and ammonium persulfate, wherein the volume ratio of aniline monomer and hydrochloric acid is 0.2-0.8:1, and hydrochloric acid volume is with ammonium persulfate liquid-solid ratio
1ml:1g, mechanic whirl-nett reaction for 24 hours, are separated, washed, dried, and Fe is prepared3O4/ polypyrrole/polyaniline；
S4、Fe3O4/ polypyrrole/polyaniline/TiO2Preparation: butyl titanate, acetylacetone,2,4-pentanedione are gradually added to dehydrated alcohol
In, wherein butyl titanate, acetylacetone,2,4-pentanedione molar ratio be 1:1, uniform stirring, be made sol-gel solution, be added step S3
Fe is prepared3O4/ polypyrrole/polyaniline, sol-gel solution and Fe3O4/ polypyrrole/polyaniline mass ratio is 8:1, uniformly
Stirring carries out hydro-thermal reaction, and hydrothermal temperature is that 500-550 DEG C of the hydro-thermal reaction time is 1-2h, is centrifuged after cooling, and washing is simultaneously
It is dry, Fe is prepared3O4/ polypyrrole/polyaniline/TiO2；
S5、Fe3O4/ polypyrrole/polyaniline/TiO2The preparation of/ZnO composite material: the Fe that step S4 is prepared3O4/ poly- pyrrole
Cough up/polyaniline/TiO2Be scattered in acetone, ammonium hydroxide be added, ultrasonic wave decentralized processing obtains dispersion liquid, under agitation to
In 55-60 DEG C of dispersion liquid be added dropwise zinc gluconate acetone soln, continue at 55-60 DEG C stir 2-3h, separating, washing and
After drying, Fe is prepared3O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material；Fe3O4/ polypyrrole/polyaniline/TiO2、
Acetone, ammonium hydroxide, zinc gluconate acetone soln mass ratio be 1:350:5:280, the acetone soln of the zinc gluconate
Zinc gluconate mass percentage be 7-9%.
Beneficial effect
(1) Fe that the present invention will be prepared3O4It is surface modified with polypyrrole, then carries out polyaniline-coated, gather at this time
Aniline is easily coated on the Fe crossed by polypyrrole modifying3O4Surface passes through Fe3O4Surface modified, coat improve it is compound
The magnetic recyclability of material, meanwhile, reduce Fe3O4The photocatalysis performance of titanium dioxide is influenced, by changing aniline monomer
Additional amount changes the Fe crossed by polypyrrole modifying3O4The thickness of surface polyaniline-coated, so that the magnetism for improving composite material is returned
Receive performance and catalytic performance.
(2) present invention is in Fe3O4/ polypyrrole/polyaniline surface recombination titanium dioxide, zinc oxide, titanium dioxide, zinc oxide
Between synergistic effect be conducive to the separation in light induced electron and hole, while extended in the photohole service life, so that multiple
The photocatalytic activity of condensation material greatly improves.
(3) preparation method of the present invention is simple, the Fe being prepared3O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material is gathered around
There is higher saturation magnetization, the magnetic rate of recovery is higher, and possesses stronger photocatalytic degradation capability, and be prepared
Fe3O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material possesses long-term, efficient photocatalysis performance and magnetic recyclability.
Detailed description of the invention
Fig. 1 is the Fe that 1 step S1 of embodiment is prepared3O4TEM figure；
Fig. 2 is the Fe that 1 step S2 of embodiment is prepared3O4The TEM of/polypyrrole schemes；
A, b, c are respectively the Fe that scheme one, scheme two, scheme three are prepared in step S3 in embodiment 1 in Fig. 33O4/ poly- pyrrole
Cough up/polyaniline TEM figure；
B is the Fe that step S4 is prepared in Fig. 43O4/ polypyrrole/polyaniline/TiO2XRD spectrum, a be step S5 be prepared into
The Fe arrived3O4/ polypyrrole/polyaniline/TiO2The XRD spectrum of/ZnO composite material；
Fig. 5 is the Fe that 1 step S5 of embodiment is prepared3O4/ polypyrrole/polyaniline/TiO2The SEM of/ZnO composite material schemes；
Fig. 6 is the Fe that embodiment 1 is prepared3O4/ polypyrrole/polyaniline/TiO2The photocatalysis performance broken line of/ZnO composite material
Figure；
Fig. 7 is the Fe that embodiment 1 is prepared3O4/ polypyrrole/polyaniline/TiO2The hysteresis loop figure of/ZnO composite material；
Fig. 8 is the Fe that embodiment 1 is prepared3O4/ polypyrrole/polyaniline/TiO2The photocatalysis performance line chart of composite material；
1,2 be respectively Fe in Fig. 93O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material and Fe3O4/ polypyrrole/polyaniline/
TiO2Composite material magnetic rate of recovery line chart.
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated；It should be understood that these embodiments are merely to illustrate the present invention
Rather than the claimed range of the limitation present invention；It will further be understood that read the content lectured of the present invention it
Afterwards, those skilled in the art can make various changes or modification to the present invention, and such equivalent forms are equally fallen within appended by the application
Claims limited range.
Embodiment 1
A kind of Fe3O4/ polypyrrole/polyaniline/TiO2The preparation method of/ZnO composite material, includes the following steps:
S1、Fe3O4Preparation: by frerrous chloride, potassium sulfite, polyvinylpyrrolidone and potassium hydroxide according to mass ratio 1.5:
0.8:0.7:0.7 is dissolved in deionized water, and under helium protection, isothermal reaction, reaction temperature is 170 DEG C of reaction time to be
Fe is prepared after 8h, separating, washing and drying3O4;
Fig. 1 is the Fe that the present embodiment is prepared3O4TEM figure, by the Fe being prepared3O4TEM figure it can be seen that preparation
Obtained Fe3O4In microballoon shape, size distribution is more uniform, and roundness is higher.
S2、Fe3O4The preparation of/polypyrrole: the Fe that step S1 is prepared3O4It is scattered in deionized water, Fe3O4Matter
The solid-to-liquid ratio of amount and deionized water volume is 1g:200mL, then by pyrroles and ethyl alcohol, concentrated hydrochloric acid is separately added into Fe3O4In dispersion liquid,
Wherein deionized water, pyrroles, ethyl alcohol, concentrated hydrochloric acid volume ratio be 100:0.1:10:3, uniform stirring 2h, the product of acquisition spend from
Sub- water and dehydrated alcohol rinse, and for 24 hours, Fe is prepared in vacuum drying3O4/ polypyrrole；
Fig. 2 is the Fe that the present embodiment is prepared3O4The TEM of/polypyrrole schemes, by the Fe being prepared3O4The TEM of/polypyrrole schemes
It can be seen that polypyrrole is uniformly coated on ferroso-ferric oxide surface, polypyrrole is uniformly coated on ferroso-ferric oxide surface
Reason is likely to pyrrole monomer and Fe3O4It is scattered in deionized water, due to the hydrophobicity of pyrrole monomer, and nitrogen and iron are easy
Coordination is formed, therefore, polypyrrole is uniformly coated on ferroso-ferric oxide surface.
S3、Fe3O4The preparation of/polypyrrole/polyaniline:
Scheme one: Fe is prepared in step S23O4/ polypyrrole is scattered in deionized water, Fe3O4/ polypyrrole quality and go from
The solid-to-liquid ratio of sub- water volume is 1g:100mL, and aniline monomer is added, and hydrochloric acid and ammonium persulfate is added, wherein aniline in ultrasonic 10min
The volume ratio of monomer and hydrochloric acid is 0.2:1, and hydrochloric acid volume and ammonium persulfate liquid-solid ratio are 1ml:1g, and mechanic whirl-nett reaction for 24 hours, passes through
Separation, washing, drying, are prepared Fe3O4/ polypyrrole/polyaniline；
Scheme two: Fe is prepared in step S23O4/ polypyrrole is scattered in deionized water, Fe3O4/ polypyrrole quality and go from
The solid-to-liquid ratio of sub- water volume is 1g:100mL, and aniline monomer is added, and hydrochloric acid and ammonium persulfate is added, wherein aniline in ultrasonic 10min
The volume ratio of monomer and hydrochloric acid is 0.5:1, and hydrochloric acid volume and ammonium persulfate liquid-solid ratio are 1ml:1g, and mechanic whirl-nett reaction for 24 hours, passes through
Separation, washing, drying, are prepared Fe3O4/ polypyrrole/polyaniline；
Scheme three: Fe is prepared in step S23O4/ polypyrrole is scattered in deionized water, Fe3O4/ polypyrrole quality and go from
The solid-to-liquid ratio of sub- water volume is 1g:100mL, and aniline monomer is added, and hydrochloric acid and ammonium persulfate is added, wherein aniline in ultrasonic 10min
The volume ratio of monomer and hydrochloric acid is 0.8:1, and hydrochloric acid volume and ammonium persulfate liquid-solid ratio are 1ml:1g, and mechanic whirl-nett reaction for 24 hours, passes through
Separation, washing, drying, are prepared Fe3O4/ polypyrrole/polyaniline；
Fig. 3 is the Fe that the present embodiment is prepared3O4/ polypyrrole/polyaniline TEM schemes, and a, b, c respectively correspond side in Fig. 3
The Fe that case one, scheme two, scheme three are prepared3O4/ polypyrrole/polyaniline TEM figure, by the Fe being prepared3O4/ poly- pyrrole
Cough up/TEM of polyaniline schemes it can be seen that polyaniline is all uniformly coated on Fe3O4/ polypyrrole surface, the polyphenyl not being scattered
The presence of amine.
S4、Fe3O4/ polypyrrole/polyaniline/TiO2Preparation: butyl titanate, acetylacetone,2,4-pentanedione are gradually added to anhydrous
In ethyl alcohol, wherein butyl titanate, acetylacetone,2,4-pentanedione molar ratio be 1:1, uniform stirring, be made sol-gel solution, be added step
Fe is prepared in rapid S3 scheme two3O4/ polypyrrole/polyaniline, sol-gel solution and Fe3O4/ polypyrrole/polyaniline mass ratio
For 8:1, uniform stirring carries out hydro-thermal reaction, and hydrothermal temperature is that 550 DEG C of the hydro-thermal reaction times are 1-2h, is centrifuged after cooling,
It washs and dries, Fe is prepared3O4/ polypyrrole/polyaniline/TiO2；
(b) is the Fe that the present embodiment is prepared in Fig. 43O4/ polypyrrole/polyaniline/TiO2XRD spectrum, by Fe3O4/ poly-
Pyrroles/polyaniline/TiO2XRD spectrum it can be seen that in Fig. 4 (b) remove Fe3O4Characteristic diffraction peak outside, 25.30 °,
There is tetragonal crystal system anatase TiO(101 at 48.06 °, 54.36 °, 62.58 °), (200), (105), (204) crystal face spy
Diffraction maximum is levied, shows that TiO2 is successfully coated on Fe3O4/ polypyrrole/polyaniline surface.
S5、Fe3O4/ polypyrrole/polyaniline/TiO2The preparation of/ZnO composite material: the Fe that step S4 is prepared3O4/
Polypyrrole/polyaniline/TiO2It is scattered in acetone, ammonium hydroxide is added, ultrasonic wave decentralized processing obtains dispersion liquid, in stirring condition
The acetone soln of zinc gluconate is added dropwise in the lower dispersion liquid to 55 DEG C, continues to stir 2h, separating, washing and drying at 55 DEG C
Afterwards, Fe is prepared3O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material；Fe3O4/ polypyrrole/polyaniline/TiO2, acetone,
Ammonium hydroxide, zinc gluconate acetone soln mass ratio be 1:350:5:280, the grape of the acetone soln of the zinc gluconate
The mass percentage of saccharic acid zinc is 8%.
(a) is the Fe that the present embodiment is prepared in Fig. 43O4/ polypyrrole/polyaniline/TiO2The XRD of/ZnO composite material
Map, by Fe3O4/ polypyrrole/polyaniline/TiO2The XRD spectrum of/ZnO composite material is it can be seen that (a) removes Fe in Fig. 43O4
Characteristic diffraction peak outside, there is hexagonal crystal at 31.74 °, 34.32 °, 36.26 °, 47.38 °, 56.44 °, 62.82 °, 68.12 °
Be the ZnO(100 of wurtzite structure), (002), (101), (102), (110), (103), (112) crystal face characteristic diffraction peak, table
Bright zinc oxide is successfully coated on Fe3O4/ polypyrrole/polyaniline/TiO2Surface；Fig. 5 is the Fe that the present embodiment is prepared3O4/ poly-
Pyrroles/polyaniline/TiO2The SEM of/ZnO composite material schemes, as seen from Figure 5: the Fe being prepared3O4/ polypyrrole/polyphenyl
Amine/TiO2/ ZnO composite gauge shape is uniform, and in addition to becoming large-sized, apparent change in shape does not occur.
Embodiment 2
In order to investigate Fe3O4/ polypyrrole/polyaniline/TiO2The photocatalysis performance of/ZnO composite material takes 5mg embodiment 1 to prepare
Obtained Fe3O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material is added to 100ml, and concentration is the methyl orange solution of 1mg/L
In, preceding 1h is stirred under dark condition, and rear 1h carries out light-catalyzed reaction under the conditions of radiation of visible light, every 15min, takes out first
Base orange solution, measures methyl orange concentration at this time, and Fig. 6 is the Fe that the present embodiment is prepared3O4/ polypyrrole/polyaniline/TiO2/
The photocatalysis performance line chart of ZnO composite material, as seen from Figure 6: preceding 1h is stirred under dark condition, and methyl orange solution is dense
Degree gradually becomes smaller and the C/C in 60min0It is 0.71, this is because under dark condition, Fe3O4/ polypyrrole/polyaniline/TiO2/
ZnO composite material possesses stronger adsorption capacity, with the extension of time, absorption property is lower, so, methyl orange solution concentration
Reduction trend slows down；1h carries out light-catalyzed reaction under the conditions of radiation of visible light afterwards, and the decline of methyl orange solution concentration is obvious, and
C/C when 120min0It is 0.02, this is because Fe3O4/ polypyrrole/polyaniline/TiO2The structure of/ZnO composite material, to visible light
Utilization rate becomes larger, and possesses higher Photocatalytic Degradation Property.
Embodiment 3
In order to investigate Fe3O4/ polypyrrole/polyaniline/TiO2The magnetic recyclability of/ZnO composite material, to Fe3O4/ polypyrrole/poly-
Aniline/TiO2/ ZnO composite material carries out, in 25 DEG C of survey hysteresis loops as shown in fig. 7, as seen from Figure 7: its saturated magnetization
Intensity is 25.0emu/g, Fe3O4/ polypyrrole/polyaniline/TiO2The remanent magnetism and coercivity of/ZnO composite material are substantially zeroed, can
To be rapidly magnetized and demagnetize, it is ensured that after through externally-applied magnetic field magnetization recycling, Fe3O4/ polypyrrole/polyaniline/
TiO2The magnetism of/ZnO composite material itself rapidly disappears, it can be effectively prevented and reunites because band is magnetic, and influences
Its photocatalysis effect.
Comparative example 1
The present embodiment provides a kind of Fe3O4/ polypyrrole/polyaniline/TiO2The preparation method of composite material, compared with Example 1,
Fe in step S4 in the present embodiment and embodiment 13O4/ polypyrrole/polyaniline/TiO2Preparation process it is identical, difference
It is in the present embodiment is not in Fe3O4/ polypyrrole/polyaniline/TiO2Surface coat ZnO, Fe3O4/ polypyrrole/polyphenyl
Amine/TiO2For final composite material；
In order to investigate the Fe that the present embodiment is prepared3O4/ polypyrrole/polyaniline/TiO2The photocatalysis performance of composite material, takes
The Fe that 5mg embodiment 1 is prepared3O4/ polypyrrole/polyaniline/TiO2Composite material is added to 100ml, and concentration is 1mg/L's
In methyl orange solution, preceding 1h is stirred under dark condition, and rear 1h carries out light-catalyzed reaction under the conditions of radiation of visible light, every
15min takes out methyl orange solution, measures methyl orange concentration at this time, and Fig. 8 is the Fe that the present embodiment is prepared3O4/ polypyrrole/poly-
Aniline/TiO2The photocatalysis performance line chart of composite material, as seen from Figure 8: rear 1h is carried out under the conditions of radiation of visible light
Light-catalyzed reaction, with the extension of light application time, compared to Fe3O4/ polypyrrole/polyaniline/TiO2This implementation of/ZnO composite material
The Fe that example is prepared3O4/ polypyrrole/polyaniline/TiO2The photocatalysis performance line chart of composite material gradually tends towards stability,
C/C when 120min0It is 0.34, show that its Photocatalytic Degradation Property is lower.
Comparative example 2
Respectively to Fe3O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material and Fe3O4/ polypyrrole/polyaniline/TiO2Composite wood
Material carries out the test of magnetic recyclability, and 1,2 be respectively Fe in Fig. 93O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material and Fe3O4/
Polypyrrole/polyaniline/TiO2Composite material magnetic recycles line chart, as seen from Figure 9: when cycle-index is 6 times, Fe3O4/ poly-
Pyrroles/polyaniline/TiO2/ ZnO composite material and Fe3O4/ polypyrrole/polyaniline/TiO2The composite material rate of recovery is respectively
94.2%, 84.4%, and Fe3O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material is compared to Fe3O4/ polypyrrole/polyaniline/
TiO2Composite material is with the increase of cycle-index, and the decline of magnetic recovery rate is slow, this is because Fe3O4/ polypyrrole/polyaniline/
TiO2Its volume of/ZnO composite material is larger and the relatively high magnetism that is easier of saturation magnetization settles, in Fe3O4/ polypyrrole/
Polyaniline/TiO2Surface coats layer of ZnO, prevents composite material in use, due to there is the case where oxidation, damage,
Reduce the magnetic recyclability and photocatalysis performance of composite material.
The above, only of the invention illustrates embodiment, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, under the premise of not departing from the method for the present invention, that makes several changes
It also should be regarded as protection scope of the present invention into supplement；All those skilled in the art, do not depart from spirit of that invention and
In the case where range, using the equivalent variations of a little change, modification and differentiation that disclosed above technology contents are made, it is
Equivalent embodiment of the invention；Meanwhile any equivalent variations that all substantial technologicals according to the present invention do above-described embodiment
Change, modification and differentiation, still fall within protection scope of the present invention.
Claims (8)
1. a kind of Fe3O4/ polypyrrole/polyaniline TiO2The preparation method of/ZnO composite material, which is characterized in that including walking as follows
It is rapid:
S1、Fe3O4Preparation: frerrous chloride, potassium sulfite, polyvinylpyrrolidone and potassium hydroxide are dissolved in deionized water
In, helium protection under, isothermal reaction, reaction temperature be 7-9h, separating, washing and drying in 160-180 DEG C of reaction time
After Fe is prepared3O4；
S2、Fe3O4The preparation of/polypyrrole: the Fe that step S1 is prepared3O4It is scattered in deionized water, Fe3O4Quality with
The solid-to-liquid ratio of deionized water volume is 1g:200mL, then pyrroles, ethyl alcohol and concentrated hydrochloric acid are separately added into Fe3O4In dispersion liquid, uniformly
2h is stirred, the product deionized water and dehydrated alcohol of acquisition are rinsed, and for 24 hours, Fe is prepared in vacuum drying3O4/ polypyrrole；
S3、Fe3O4The preparation of/polypyrrole/polyaniline: Fe is prepared in step S23O4/ polypyrrole is scattered in deionized water,
Fe3O4The solid-to-liquid ratio of/polypyrrole quality and deionized water volume is 1g:100mL, and aniline monomer is added, and salt is added in ultrasonic 10min
Acid and ammonium persulfate, mechanic whirl-nett reaction for 24 hours, are separated, washed, dried, and Fe is prepared3O4/ polypyrrole/polyaniline；
S4、Fe3O4/ polypyrrole/polyaniline/TiO2Preparation: butyl titanate, acetylacetone,2,4-pentanedione are gradually added to dehydrated alcohol
In, sol-gel solution is made in uniform stirring, step S3 is added, Fe is prepared3O4/ polypyrrole/polyaniline, sol-gel
Solution and Fe3O4/ polypyrrole/polyaniline mass ratio is 8:1, and uniform stirring carries out hydro-thermal reaction, is centrifuged after cooling, washs and do
It is dry, Fe is prepared3O4/ polypyrrole/polyaniline/TiO2；
S5、Fe3O4/ polypyrrole/polyaniline/TiO2The preparation of/ZnO composite material: the Fe that step S4 is prepared3O4/ poly- pyrrole
Cough up/polyaniline/TiO2It is scattered in acetone, ammonium hydroxide is added, ultrasonication obtains dispersion liquid, under agitation to 55-60
DEG C dispersion liquid in the acetone soln of zinc gluconate is added dropwise, continue to stir 2-3h, separating, washing and drying at 55-60 DEG C
Afterwards, Fe is prepared3O4/ polypyrrole/polyaniline/TiO2/ ZnO composite material.
2. a kind of Fe according to claim 13O4/ polypyrrole/polyaniline TiO2The preparation method of/ZnO composite material,
It is characterized in that, frerrous chloride, potassium sulfite, polyvinylpyrrolidone and potassium hydroxide is dissolved in deionized water in step S1
In, frerrous chloride, potassium sulfite, polyvinylpyrrolidone and potassium hydroxide quality ratio are 1.5:0.8:0.7:0.7.
3. a kind of Fe according to claim 13O4/ polypyrrole/polyaniline TiO2The preparation method of/ZnO composite material,
It is characterized in that, deionized water, pyrroles, ethyl alcohol, concentrated hydrochloric acid volume ratio are 100:0.1:10:3 in step S2.
4. a kind of Fe according to claim 13O4/ polypyrrole/polyaniline TiO2The preparation method of/ZnO composite material,
It is characterized in that, the volume ratio of aniline monomer and hydrochloric acid is 0.2-0.8:1 in step S3, and hydrochloric acid volume is with ammonium persulfate liquid-solid ratio
1ml:1g。
5. a kind of Fe according to claim 13O4/ polypyrrole/polyaniline TiO2The preparation method of/ZnO composite material,
Be characterized in that, butyl titanate in step S4, acetylacetone,2,4-pentanedione molar ratio be 1:1.
6. a kind of Fe according to claim 13O4/ polypyrrole/polyaniline TiO2The preparation method of/ZnO composite material,
It is characterized in that, hydrothermal temperature is 500-550 DEG C in step S4, the hydro-thermal reaction time 1-2h.
7. a kind of Fe according to claim 13O4/ polypyrrole/polyaniline TiO2The preparation method of/ZnO composite material,
Be characterized in that, acetone in step S5, ammonium hydroxide, zinc gluconate the mass ratio of acetone soln be 1:350:5:280.
8. a kind of Fe according to claim 13O4/ polypyrrole/polyaniline TiO2The preparation method of/ZnO composite material,
It is characterized in that, the mass percentage of the zinc gluconate of the acetone soln of zinc gluconate is 7-9% in step S5.
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| CN113289593A (en) * | 2021-06-11 | 2021-08-24 | 清华大学深圳国际研究生院 | Preparation method and application of polyaniline and polypyrrole loaded magnetically modified biochar |
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