CN111974460A - Preparation method of nano Fe-based compound loaded conductive polymer - Google Patents
Preparation method of nano Fe-based compound loaded conductive polymer Download PDFInfo
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- CN111974460A CN111974460A CN202010638179.9A CN202010638179A CN111974460A CN 111974460 A CN111974460 A CN 111974460A CN 202010638179 A CN202010638179 A CN 202010638179A CN 111974460 A CN111974460 A CN 111974460A
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- 229920001940 conductive polymer Polymers 0.000 title claims abstract description 33
- 150000001875 compounds Chemical class 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000178 monomer Substances 0.000 claims abstract description 13
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000001699 photocatalysis Effects 0.000 claims abstract description 11
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001447 ferric ion Inorganic materials 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 239000004065 semiconductor Substances 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 5
- 150000002500 ions Chemical class 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 15
- 229920000128 polypyrrole Polymers 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000002322 conducting polymer Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 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
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229920000767 polyaniline Polymers 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- -1 potassium ferricyanide Chemical compound 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 2
- 235000019797 dipotassium phosphate Nutrition 0.000 claims description 2
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 2
- 235000019800 disodium phosphate Nutrition 0.000 claims description 2
- 229960002413 ferric citrate Drugs 0.000 claims description 2
- 150000004677 hydrates Chemical class 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
- YHGPYBQVSJBGHH-UHFFFAOYSA-H iron(3+);trisulfate;pentahydrate Chemical compound O.O.O.O.O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O YHGPYBQVSJBGHH-UHFFFAOYSA-H 0.000 claims description 2
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- SHXXPRJOPFJRHA-UHFFFAOYSA-K iron(iii) fluoride Chemical compound F[Fe](F)F SHXXPRJOPFJRHA-UHFFFAOYSA-K 0.000 claims description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 235000011008 sodium phosphates Nutrition 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 229930192474 thiophene Natural products 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 239000011669 selenium Substances 0.000 claims 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims 2
- RVIXKDRPFPUUOO-UHFFFAOYSA-N dimethylselenide Chemical compound C[Se]C RVIXKDRPFPUUOO-UHFFFAOYSA-N 0.000 claims 2
- 229910052711 selenium Inorganic materials 0.000 claims 2
- 229940091258 selenium supplement Drugs 0.000 claims 2
- 229910052717 sulfur Inorganic materials 0.000 claims 2
- 239000011593 sulfur Substances 0.000 claims 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims 1
- 239000003570 air Substances 0.000 claims 1
- 229910052786 argon Inorganic materials 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 238000006731 degradation reaction Methods 0.000 claims 1
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 claims 1
- 239000003344 environmental pollutant Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 229910052734 helium Inorganic materials 0.000 claims 1
- 239000001307 helium Substances 0.000 claims 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000002114 nanocomposite Substances 0.000 claims 1
- 150000004767 nitrides Chemical class 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 125000001741 organic sulfur group Chemical group 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 231100000719 pollutant Toxicity 0.000 claims 1
- 229920000123 polythiophene Polymers 0.000 claims 1
- 150000003346 selenoethers Chemical class 0.000 claims 1
- 229960001471 sodium selenite Drugs 0.000 claims 1
- 235000015921 sodium selenite Nutrition 0.000 claims 1
- 239000011781 sodium selenite Substances 0.000 claims 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims 1
- 239000011941 photocatalyst Substances 0.000 abstract description 7
- 239000002077 nanosphere Substances 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 5
- 150000002506 iron compounds Chemical class 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000000670 limiting effect Effects 0.000 abstract description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000004220 aggregation Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 239000000969 carrier Substances 0.000 abstract 1
- 230000000379 polymerizing effect Effects 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 15
- 239000000243 solution Substances 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 238000004506 ultrasonic cleaning Methods 0.000 description 5
- 239000002800 charge carrier Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910021205 NaH2PO2 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical class [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
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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
- B01J35/33—Electric or magnetic 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
- B01J35/30—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
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Abstract
The invention belongs to the technical field of nano material preparation, and particularly relates to a nano iron compound loaded conductive polymer nanosphere and a preparation method thereof. The preparation method of the nanometer Fe-based compound load conductive polymer comprises the steps of oxidizing and polymerizing a conductive polymer monomer by ferric ions, and then carrying out high-temperature post-treatment on the residual Fe ions to obtain a target product. The invention has the advantage that ferric ions not only realize the oxidative polymerization of pyrrole monomers, but also serve as a precursor of a cocatalyst. In addition, the formed porous conductive polymer nanosphere not only can serve as a conductive carrier, but also has a limiting effect on the size of an iron compound, so that the photocatalytic and electrocatalytic activities of the nanosphere are obviously improved. After the composite structure is further loaded on various semiconductors, the separation and utilization efficiency of current carriers is hopefully greatly promoted, and the aggregation of graphite-phase carbon nitride can be inhibited, so that the photocatalytic activity of the composite structure is obviously improved, and a new strategy is provided for designing high-efficiency photocatalysts.
Description
Technical Field
The invention relates to a preparation method of a multifunctional nano Fe-based compound loaded conductive polymer, and the composite particles have high conductivity and redox characteristics and can be used as electrocatalysis and photocatalysis energy conversion catalysts.
Background
The problems of energy shortage and environmental pollution in the world are increasingly remarkable, the search for green, environment-friendly and renewable new energy becomes urgent, and the development of hydrogen energy with high combustion value, cleanness and high efficiency is considered to be one of ideal ways for replacing fossil energy. The hydrogen production by water electrolysis is the simplest and feasible hydrogen production method. And on the basis of control cost and efficiency improvement, hydrogen energy conversion is often promoted by designing an efficient electrocatalyst. The solar photocatalytic water splitting hydrogen production is a potential hydrogen energy development means.
The transition metal phosphide has an electronic structure similar to that of a Pt-based metal, and can exhibit excellent electrocatalytic activity during an electrocatalytic reaction. The Fe element has abundant reserves and low price, and phosphide thereof has great application prospect in the aspect of being used as an electrolytic water catalyst, and can show good hydrogen evolution or oxygen evolution catalytic performance in the process of electrolyzing water, so that the Fe element is applied to a hydrogen evolution or oxygen evolution reaction catalyst. In addition, catalysis is a surface-based reaction, and preparing a small-sized catalyst is beneficial to increasing the number of surface active sites, however, a green approach for preparing a nanocatalyst without introducing impurities is still a challenge.
The conductive polymer comprises polypyrrole (PPy), Polyaniline (PANI) and the like, and can be used as a high-speed transport channel of charge carriers like conductive media such as graphene, xylene, porous carbon and the like. Has been widely used in electrocatalytic reactions. In addition, conducting polymers typically exhibit a narrow band gap, and both the redox plateau and the band gap can be further manipulated by chemical means. The introduction of the conductive polymer can improve the efficiency of charge carrier transport and separation. Therefore, it is of great interest to develop a polymerization method of a conductive polymer having an appropriate morphology.
Disclosure of Invention
The invention utilizes ferric ions to carry out oxidative polymerization of conductive polymer monomers such as pyrrole and the like, and also serves as a precursor of a catalyst, thereby simplifying the preparation steps. Meanwhile, the PPy prepared by the method has a porous spherical shape, and can play a role in limiting the size of the iron compound when being used as a skeleton loaded by the nano iron compound, thereby greatly improving the specific surface area of the catalyst and providing a large number of active sites for reaction. After the nano-material is loaded on carbon nitride, the photocatalytic efficiency is obviously improved, and the application of the inorganic composite nano-material in the field of photocatalytic hydrogen production is expanded.
In order to achieve the above purpose, the specific technical scheme of the invention is as follows:
(1) the preparation of the nano Fe-based compound loaded conductive polymer is carried out according to the following steps of 1-1000 parts of polymer monomer and ferric salt: 1-1000 parts of the Fe-based compound loaded conductive polymer, namely dissolving a certain amount of ferric salt in 1-100 ml of deionized water, performing ultrasonic treatment on the solution for 5-100 min by using an ultrasonic cleaning machine, slowly dripping a certain amount of polymer monomer in the ultrasonic process, stirring the mixed solution at 30-100 ℃ for 1-50 h, cleaning with deionized water for 0-10 times, drying at 30-100 ℃ to obtain solid powder, uniformly mixing the solid powder with 1-1000 mg of phosphate, heating the solid powder at 100-1000 ℃ for 0.5-12 h, cleaning with deionized water for 0-10 times, and drying at 30-100 ℃ to obtain the Fe-based compound loaded conductive polymer.
（2） g-C3N4Preparation of a Nano-Fe-based Compound Supported conducting Polymer according to g-C3N41-1000 parts of polymer monomer and iron salt: 1-1000: 1-1000, dispersing a certain amount of ferric salt and a certain amount of semiconductor photocatalyst in 1-100 ml of deionized water, carrying out ultrasonic treatment on the solution for 5-100 min by using an ultrasonic cleaning machine, slowly dripping a certain amount of polymer monomer in the ultrasonic process, stirring the mixed solution at 30-100 ℃ for 1-50 h, cleaning the mixed solution for 0-10 times by using deionized water, drying the mixed solution at 30-100 ℃ to obtain solid powder, uniformly mixing the solid powder with 1-1000 mg of phosphate, heating the solid powder at 100-1000 ℃ for 0.5-12 h, cleaning the solid powder by using deionized water for 0-10 times, and drying the solid powder at 30-100 ℃ to obtain the nano Fe-based compound negative ionA semiconductor photocatalyst supported on a conducting polymer.
Preferably, the iron salt in steps (1) and (2) comprises one or more of ferric sulfate, ferric acetate, ferric citrate, potassium ferricyanide, ferric fluoride, potassium ferrite hexahydroate, ferric chloride, ferric nitrate and crystalline hydrates thereof.
Preferably, the phosphate in steps (1) and (2) comprises one or more of sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium hydrogen phosphate, and potassium dihydrogen phosphate.
Preferably, the polymer monomers in steps (1) and (2) include pyrrole, aniline, thiophene and the like.
The invention has the beneficial effects that:
(1) ferric ions not only realize the polymerization of polymer monomers, but also serve as a precursor of a cocatalyst, and the porous PPy nanospheres can promote the electric conduction and inhibit the size of FeP particles, thereby showing better electrocatalytic performance.
(2) Loading PPy-FeP to g-C3N4On the semiconductor photocatalyst, PPy and FeP can be respectively used as a charge carrier and a high-performance cocatalyst, so that the utilization rate of the charge carrier is greatly promoted, and g-C can be inhibited3N4To improve its photocatalytic activity.
Drawings
FIG. 1 is a high-resolution transmission electron micrograph of PPy-FeP prepared in example 1
FIG. 2 shows g-C prepared in example 23N4-PANI-Fe2O3XRD pattern of
FIG. 3 is g-C prepared in example 33N4-PPy-FeP TEM image
FIG. 4 shows the electrochemical decomposition aqueous Performance of PPy-FeP prepared in example 1
FIG. 5 g-C prepared in example 33N4PPy-FeP photocatalytic hydrogen production performance.
Detailed Description
The technical solution of the present invention is described below by specific examples, but the technical solution of the present invention is not limited to the specific examples.
The technical solution of the present invention is described below by way of specific examples, but the technical solution of the present invention is not limited to the examples.
Example 1:
preparation of the nano FeP loaded PPy conductive polymer: dissolving 20 mg of ferric chloride in 40 ml of deionized water, carrying out ultrasonic treatment on the solution for 30 min by using an ultrasonic cleaning machine, slowly dropping 5 mu l of pyrrole in the ultrasonic process, stirring the mixed solution at 40 ℃ for 10 h, cleaning the mixed solution for 1 time by using the deionized water, drying the mixed solution at 60 ℃ to obtain solid powder, mixing the solid powder with 50 mg of NaH2PO2Mixing well, heating the above solid powder at 350 deg.C for 2 h, washing with deionized water for 1 time, and oven drying at 60 deg.C to obtain PPy-FeP. The morphology of the prepared PPy-FeP sample is analyzed, and a high-resolution transmission electron microscope photo is shown in figure 1. As can be seen from FIG. 1, PPy has a porous spherical morphology, and is used as a FeP-loaded framework, and FeP nanoparticles with small particle sizes are uniformly distributed on PPy nanospheres and have abundant reaction sites. The electrochemical hydrogen evolution performance of the catalyst is tested, the overpotential of hydrogen evolution of the catalyst is better than that of FeP and PPy which exist independently, and the electrochemical hydrogen evolution map is shown in figure 4.
Example 2:
nano Fe2O3Preparing load polyaniline: 200 mg of g-C3N4Dissolving 20 mg of ferric chloride in 40 ml of deionized water, carrying out ultrasonic treatment on the solution for 30 min by using an ultrasonic cleaning machine, slowly dropping aniline monomers with different volumes (10, 20,50 mu l) in the ultrasonic process, stirring the mixed solution at 40 ℃ for 10 h, cleaning the mixed solution for 1 time by using the deionized water, drying the mixed solution at 60 ℃ to obtain solid powder, heating the solid powder in 500 ℃ air for 2 h, cleaning the mixed solution for 1 time by using the deionized water, and drying the solid powder at 60 ℃ to obtain g-C3N4-PANI-Fe2O3. For g to C prepared3N4-PANI-Fe2O3The sample is subjected to phase composition analysis, and the X-ray diffraction pattern is shown as figure 2. From FIG. 2, Fe can be observed2O3And g-C3N4Characteristic diffraction peak of, and g-C3N4-PANI-Fe2O3The characteristic diffraction peak of (A) is represented by g-C3N4And Fe2O3The characteristic diffraction peaks of (A) are superposed, which shows that PANI-Fe2O3Successfully load to g-C3N4The above.
Example 3:
preparation of a semiconductor photocatalyst supported by a nano Fe-based compound-supported conducting polymer: 200 mg of g-C3N4And dispersing 0, 10, 20 and 50 mg of ferric chloride in 40 ml of deionized water, performing ultrasonic treatment on the solution for 30 min by using an ultrasonic cleaning machine, slowly dropping 5 mu l of pyrrole in the ultrasonic process, stirring the mixed solution at 40 ℃ for 10 h, cleaning the mixed solution for 1 time by using deionized water, drying the mixed solution at 60 ℃ to obtain solid powder, and mixing the solid powder with 50 mg of NaH2PO2Mixing, heating the solid powder at 350 deg.C for 2 hr, washing with deionized water for 1 time, and oven drying at 60 deg.C to obtain g-C3N4-PPy，g-C3N4-PPy-FeP 10wt%，g-C3N4-PPy-FeP 20wt%，g-C3N4-PPy-FeP 50 wt%. In this example g-C3N4Can be replaced by sulfide such as cadmium sulfide or oxide such as titanium oxide. For g to C prepared3N4Morphology analysis is carried out on the-PPy-FeP 20wt% composite photocatalyst, and a TEM photograph is shown in FIG. 3. As can be seen in FIG. 3, g-C3N4PPy nanospheres wrapping FeP nanoparticles in the PPy-FeP composite photocatalyst are uniformly embedded in g-C3N4The nano-chip has abundant reaction sites. The sample is subjected to photocatalytic hydrogen production performance test under the irradiation of visible light, and the fact that the addition of PPy-FeP effectively improves g-C3N4In which g-C3N4The PPy-FeP 20wt% has the optimal photocatalytic performance, and the hydrogen production rate is shown in figure 5.
Claims (9)
1. The preparation method of the nano Fe-based compound supported conductive polymer is characterized by comprising the following steps: ferric ions are used for realizing the polymerization of a conductive polymer monomer and are used as a precursor of a catalyst; the porous structure of the conductive polymer can be used as a carrier of Fe ions to further bind a precursor of the Fe compound catalyst.
2. The preparation of nanosized Fe-based compound supported conducting polymer according to claim 1, wherein the preparation method comprises the steps of:
(1) according to the preparation of the nano Fe-based compound loaded conductive polymer, a certain amount of trivalent ferric salt is dissolved in deionized water according to different mass proportions of a polymer monomer and the trivalent ferric salt, and a proper amount of pyrrole, thiophene and aniline monomers are slowly dropped in the ultrasonic or stirring process;
(2) fully stirring the mixed solution at 30-100 ℃, washing with deionized water for 0-10 times, further drying to obtain solid powder, uniformly mixing the solid powder alone or with a proper amount of phosphorus source, sulfur source, Se source and the like, heating the solid powder at 100-1000 ℃ for 0.5-12 h, and naturally cooling to obtain the Fe-based compound-supported conducting polymer with the nanometer size.
3. A nano Fe-based compound according to claim 2, characterized by a small size of about 1 to 100 nm, and said Fe-based compound comprises elementary substance, iron oxide, carbide, nitride, phosphide, sulfide, selenide, etc.
4. The conductive polymer according to claim 2, wherein the conductive polymer is oxidized and polymerized by ferric ions, and specifically comprises conductive polymers such as polypyrrole, polythiophene and polyaniline.
5. The Fe-based nanocomposite supported conducting polymer and the preparation method thereof as claimed in claim 2, wherein the iron salt includes a precursor of ferric ion, such as one or more of ferric sulfate, ferric acetate, ferric citrate, potassium ferricyanide, ferric fluoride, potassium ferrite hexahydrate, ferric chloride, ferric nitrate and their crystalline hydrates.
6. The nano Fe-based compound supported conductive polymer and the method of preparing the same as claimed in claim 2, wherein the phosphate comprises one or more of sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate; the sulfur source comprises one or more of inorganic and organic sulfur sources such as sulfur powder, thiourea, thioacetamide, sulfate, mercaptan and the like; the selenium source comprises Se powder and one or more of inorganic and organic selenium sources represented by sodium selenite and dimethyl selenium.
7. The nano Fe-based compound supported conducting polymer and the preparation method thereof as claimed in claim 2, wherein the temperature range of the high temperature treatment is from room temperature to 1000 ℃; the processing atmosphere is air, argon, nitrogen, hydrogen, helium and other single or mixed gas.
8. The nano Fe-based compound supported conductive polymer as claimed in claim 1, which can be used for electrocatalytic water decomposition, CO2Reduction, N2Reduction, oxygen reduction and other energy conversion reactions.
9. The nano Fe-based compound-supported conductive polymer as claimed in claim 1, which is loaded as a cocatalyst to a catalyst such as g-C3N4Sulfide, oxide and other semiconductors to raise their carrier transmission and utilization efficiency, so that it can be used in photocatalytic water decomposition and CO decomposition2Reduction, N2Reduction, organic-inorganic pollutant degradation, micromolecule conversion and the like.
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