CN107126974A - ZIF 67 modifies Fe3O4The preparation and its application of ORR catalyst of@PZS core-shell particles - Google Patents
ZIF 67 modifies Fe3O4The preparation and its application of ORR catalyst of@PZS core-shell particles Download PDFInfo
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- CN107126974A CN107126974A CN201710423396.4A CN201710423396A CN107126974A CN 107126974 A CN107126974 A CN 107126974A CN 201710423396 A CN201710423396 A CN 201710423396A CN 107126974 A CN107126974 A CN 107126974A
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- shell particles
- zif
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- 239000002245 particle Substances 0.000 title claims abstract description 31
- 239000011258 core-shell material Substances 0.000 title claims abstract description 29
- 239000003054 catalyst Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000012986 modification Methods 0.000 claims abstract description 14
- 230000004048 modification Effects 0.000 claims abstract description 13
- 230000003197 catalytic effect Effects 0.000 claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- KZTYYGOKRVBIMI-UHFFFAOYSA-N S-phenyl benzenesulfonothioate Natural products C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 6
- -1 hydroxyl diphenyl sulphone Chemical compound 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 238000003763 carbonization Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 229920000557 Nafion® Polymers 0.000 claims description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical class CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- 239000000839 emulsion Substances 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 150000003512 tertiary amines Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 150000008614 2-methylimidazoles Chemical class 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 claims description 2
- 239000004005 microsphere Substances 0.000 abstract description 4
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 239000012621 metal-organic framework Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 208000021251 Methanol poisoning Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000010189 synthetic method Methods 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
- 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
-
- B01J35/33—
-
- B01J35/398—
Abstract
The present invention relates to the Fe that ZIF 67 is modified3O4Preparing and its as the application of ORR catalyst for@PZS core-shell particles, it is of the invention that Fe is prepared using solvent-thermal method3O4Magnetic microsphere, and prepare Fe using condensation methods as core3O4@PZS core-shell particles, realize ZIF 67 to Fe using in situ synthesis3O4The modification of@PZS core-shell particles.The magnetic microsphere of preparation is doped with Fe, Co, N, P and S multiple element, with good ORR catalytic activity, preferable cyclical stability and methanol tolerant, and multiple recycle can be absorbed by magnet.
Description
Technical field
The present invention relates to magnetic core-shell field of nanometer material technology and ORR catalytic fields, specifically prepared using solvent-thermal method
Surface has hydroxyl and the Fe of carboxyl modified3O4Magnetic microsphere, and prepare Fe using condensation methods as core3O4@PZS nucleocapsids
Microballoon, realizes ZIF-67 to Fe using in situ synthesis3O4The modification of@PZS core-shell particles, its ORR is improved using polyatom doping
Catalytic activity.
Background technology
The dynamics of redox reaction (ORR) is very slow, limits the electrochemistry such as fuel cell and metal-air battery
Conversion and storage device, although platinum and its alloy are considered as best ORR catalyst, its expensive price, relatively low storage
The key issues such as storage, poor durability, easy methanol poisoning effect hinder its large-scale practical application.Accordingly, it would be desirable to
The higher non-precious metal catalyst of a class catalytic activity is developed to replace platinum catalyst.
Fe3O4Nano-particle be it is a kind of be readily synthesized and surface-functionalized nano magnetic material, with good biology
The advantages of compatibility, biological degradability, low toxicity, repeatable recycling, it is widely used in the fields such as biomedical engineering, army
The fields such as thing, protection, catalysis.At present, Fe is prepared3O4The method of microballoon is a lot, mainly have coprecipitation, microemulsion method, hydro-thermal/
Solvent-thermal method, high-temperature decomposition, sonochemical method, electrochemical process and colloidal sol~gel method.The present invention mainly uses solvent-thermal method
Synthesize Fe3O4Microballoon.
Metal-organic framework (Metal-Orgaic Frameworks), abbreviation MOFs, be by organic ligand and metal from
The hybrid inorganic-organic materials with molecule inner pore that son or cluster are self-assembly of by coordinate bond.It is organic in MOFs
The arrangement of part and metal ion or cluster has obvious directionality, different framework pore structures can be formed, so that table
Reveal different absorption properties, optical property, electromagnetic property etc., MOFs shows huge development in terms of modern materials science
Potentiality and tempting development prospect.
The content of the invention
ZIF-67 modifications Fe is prepared it is an object of the invention to provide a kind of simple synthetic method3O4@PZS core-shell particles, and
It is used as ORR catalyst.
To achieve these goals, the present invention takes following technical scheme：
Firstth, Fe3O4The preparation of@PZS core-shell particles
5~25mg hexachlorocyclotriph,sphazenes are added in 50mL single neck bottle, 25.2~126mg is to hydroxyl diphenyl sulphone (DPS), 30.2
The Fe for a diameter of 100~300nm that~151mg is prepared by solvent-thermal method3O4, 50mL acetonitriles or acetone are used as solvent, ultrasound
10min be completely dissolved with it is dispersed.Then sealed with rubber stopper, inject 0.5mL triethylamines rapidly with syringe or rub together
Other tertiary amines (tri-n-butyl amine or trioctylphosphine amine) of your amount are as acid binding agent, and 10s~1min is (different slightly poor according to solvent
Not, acetonitrile internal ratio is very fast, slow in acetone), form white emulsion.Then 50Hz ultrasounds, continue reaction 3 hours, then
8000rpm centrifuges 10min, is washed 2 times with acetone, ethanol and deionized water respectively, final product is 40 DEG C in vacuum drying oven
Dry.Secondth, ZIF-67 is to Fe3O4The modification of@PZS core-shell particles：
Take 10~60mg Fe3O4@PZS core-shell particles are dispersed in 10mL and contain 145.5~1455.1mg Co (NO3)2·
6H2In O methanol solution, ultrasonic disperse adds the methanol that 10mL contains 82.1~821.0mg2- methylimidazoles after 30min molten
Liquid, stands 30min at room temperature, then collects particle with magnet, is washed with ethanol 2 times, final product is 40 in vacuum drying oven
DEG C drying.
ZIF-67 modifies Fe3O4@PZS core-shell particles are as the application of ORR catalyst, and its specific method is：
Firstth, by the microballoon of synthesis in tube furnace 800~1000 DEG C of 1~3h of carbonization treatment under nitrogen atmosphere；
Secondth, the sample for taking 5.0mg steps one to obtain, it is 10% Nafion to add 1mL ethanol and 100 μ L mass fractions
Solution, ultrasonic 30min, makes it be uniformly dispersed, and obtains catalyst solution；
3rd, its ORR catalytic activity, cyclical stability and methanol tolerant is tested with electrochemical workstation, electrolyte is O2
The 0.1M KOH of saturation, 5~10mV of sweep speed s-1, rotary speed is 400-2500rpm.Compared with prior art, it is of the invention
Advantage be：
The preparation method of the present invention is simple, and raw material is cheap and easy to get, and it is many that the magnetic microsphere of preparation is doped with Fe, Co, N, P and S
Element is planted, with good ORR catalytic performances, preferable cyclical stability and methanol tolerant, can be absorbed and repeatedly returned by magnet
Receive and utilize.
Brief description of the drawings
Fig. 1 is the Fe prepared in embodiment 13O4The TEM figures of@PZS core-shell particles.
Fig. 2 is the Fe of the ZIF-67 modifications prepared in embodiment 13O4The TEM figures of@PZS core-shell particles.
Fig. 3 is the Fe of the ZIF-67 modifications prepared in embodiment 13O4The LSV curves of@PZS core-shell particles.
Fig. 4 is the Fe of the ZIF-67 modifications prepared in embodiment 13O4The stable circulation linearity curve of@PZS core-shell particles.
Fig. 5 is the Fe of the ZIF-67 modifications prepared in embodiment 13O4The methanol tolerant stability curve of@PZS core-shell particles.
Embodiment
The present invention presented below-ZIF-67 modifications Fe3O4The preparation and its application of ORR catalyst of@PZS core-shell particles
Embodiment.
Embodiment 1
10mg hexachlorocyclotriph,sphazenes are added in 50mL single neck bottle, 50.4mg is to hydroxyl diphenyl sulphone (DPS), and 60.4mg is by solvent
Diameter about 250nm prepared by hot method Fe3O4, 50mL acetonitriles or acetone are as solvent, and ultrasonic 10min is completely dissolved and uniformly
It is scattered.Then sealed with rubber stopper, inject 0.5mL triethylamines rapidly with syringe or (three just with other tertiary amines of mole
Butylamine or trioctylphosphine amine) as acid binding agent, about 10s~1min (difference is slightly had according to solvent difference, acetonitrile internal ratio is very fast,
It is slow in acetone), form white emulsion.Then 50Hz ultrasounds, continue reaction 3 hours, and then 8000rpm centrifuges 10min and received
Collect particle, washed 2 times with acetone, ethanol and deionized water respectively, final product 40 DEG C of dryings in vacuum drying oven.
Take 30mg Fe3O4@PZS core-shell particles are dispersed in 10mL and contain 291.0mg Co (NO3)2·6H2O methanol solution
In, ultrasonic disperse adds the methanol solution that 10mL contains 410.5mg 2-methylimidazoles after 30min, 30min is stood at room temperature,
Then 8000rpm centrifuges 10min, is washed with ethanol 2 times, final product 40 DEG C of dryings in vacuum drying oven.
The Fe of ZIF-67 modifications3O4@PZS core-shell particles 800 DEG C of carbonization treatment 1h under nitrogen atmosphere in tube furnace.Take
The sample that 5.0mg carbonizations are obtained, adds 1mL ethanol and 100 μ L 5% Nafion solution, and ultrasonic 30min makes it scattered equal
It is even, obtain catalyst solution.
Its ORR catalytic activity, cyclical stability and methanol tolerant is tested with electrochemical workstation, electrolyte is O2Saturation
0.1M KOH, sweep speed 10mV s-1, rotary speed is 1600rpm.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, without departing from the inventive concept of the premise, can also make some improvements and modifications, these improvements and modifications also should be regarded as
In protection scope of the present invention.
Claims (4)
1.ZIF-67 modifies Fe3O4The preparation of@PZS core-shell particles, it is characterised in that comprise the following steps：
Firstth, Fe3O4The preparation of@PZS core-shell particles；
Secondth, ZIF-67 is to Fe3O4The modification of@PZS core-shell particles.
2. ZIF-67 according to claim 1 modifies Fe3O4The preparation of@PZS core-shell particles, it is characterised in that described
Fe3O4The preparation of@PZS core-shell particles：
Add 5~25mg hexachlorocyclotriph,sphazenes in 50mL single neck bottle, 25.2~126mg to hydroxyl diphenyl sulphone (DPS), 30.2~
The Fe for a diameter of 100~300nm that 151mg is prepared by solvent-thermal method3O4, 50mL acetonitriles or acetone are used as solvent, ultrasound
10min be completely dissolved with it is dispersed.Then sealed with rubber stopper, inject 0.5mL triethylamines rapidly with syringe or rub together
Other tertiary amines (tri-n-butyl amine or trioctylphosphine amine) of your amount are as acid binding agent, and 10s~1min is (different slightly poor according to solvent
Not, acetonitrile internal ratio is very fast, slow in acetone), form white emulsion.Then 50Hz ultrasounds, continue reaction 3 hours, then
8000rpm centrifuges 10min, is washed 2 times with acetone, ethanol and deionized water respectively, final product is 40 DEG C in vacuum drying oven
Dry.
3. ZIF-67 according to claim 1 modifies Fe3O4The preparation of@PZS core-shell particles, it is characterised in that described
ZIF-67 is to Fe3O4The modification of@PZS core-shell particles：
Take 10~60mg Fe3O4@PZS core-shell particles are dispersed in 10mL and contain 145.5~1455.1mg Co (NO3)2·6H2O's
In methanol solution, ultrasonic disperse adds the methanol solution that 10mL contains 82.1~821.0mg 2-methylimidazoles, room after 30min
Temperature is lower to stand 30min, then collects particle with magnet, is washed with ethanol 2 times, and final product is done for 40 DEG C in vacuum drying oven
It is dry.
4.ZIF-67 modifies Fe3O4@PZS core-shell particles as ORR catalyst application, it is characterised in that concretely comprise the following steps：
Firstth, by the microballoon of synthesis in tube furnace 800~1000 DEG C of 1~3h of carbonization treatment under nitrogen atmosphere；
Secondth, the sample for taking 5.0mg steps one to obtain, adds 1mL ethanol and 100 μ L mass fractions molten for 10% Nafion
Liquid, ultrasonic 30min, makes it be uniformly dispersed, and obtains catalyst solution；
3rd, its ORR catalytic activity, cyclical stability and methanol tolerant is tested with electrochemical workstation, electrolyte is O2Saturation
0.1M KOH, 5~10mV of sweep speed s-1, rotary speed is 400-2500rpm.
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Cited By (9)
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|---|---|---|---|---|
| CN108525648A (en) * | 2018-04-09 | 2018-09-14 | 东华理工大学 | A kind of method of amination magnetism poly phosphazene adsorbent and preparation and separation and enriched uranium |
| CN108752637A (en) * | 2018-08-01 | 2018-11-06 | 河北大学 | A kind of ZIF-8 encapsulation hexachlorocyclotriph,sphazene fire retardant, preparation method and application and fire retarding epoxide resin |
| CN109065895A (en) * | 2018-07-26 | 2018-12-21 | 北京化工大学常州先进材料研究院 | The preparation of iron cobalt codope carbon nitrogen core-shell particles material and its application in terms of electro-catalysis |
| CN109705329A (en) * | 2018-12-28 | 2019-05-03 | 广东工业大学 | A kind of ring opening catalyst and its preparation method and application that can be recycled |
| CN110459776A (en) * | 2019-08-02 | 2019-11-15 | 北京化工大学常州先进材料研究院 | The preparation of FeCo hollow carbon micro-sphere material and its application in terms of electro-catalysis |
| CN110452547A (en) * | 2019-08-26 | 2019-11-15 | 北京理工大学 | ZIF-67 polysulfones ball fire retardant and preparation method thereof |
| CN112774713A (en) * | 2021-01-25 | 2021-05-11 | 华南理工大学 | Bimetallic core-shell catalyst for electrocatalysis-synergetic hydrogen production and preparation method and application thereof |
| CN112831174A (en) * | 2021-02-20 | 2021-05-25 | 青岛理工大学 | Preparation and application of ZnO @ MOF @ polyphosphazene flame retardant |
| CN112892574A (en) * | 2021-01-25 | 2021-06-04 | 华南理工大学 | Multi-element heterojunction core-shell catalyst suitable for electro-Fenton and preparation method and application thereof |
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| CN108525648A (en) * | 2018-04-09 | 2018-09-14 | 东华理工大学 | A kind of method of amination magnetism poly phosphazene adsorbent and preparation and separation and enriched uranium |
| CN108525648B (en) * | 2018-04-09 | 2020-12-01 | 东华理工大学 | Aminated magnetic polyphosphazene adsorbent and method for preparing, separating and enriching uranium |
| CN109065895A (en) * | 2018-07-26 | 2018-12-21 | 北京化工大学常州先进材料研究院 | The preparation of iron cobalt codope carbon nitrogen core-shell particles material and its application in terms of electro-catalysis |
| CN108752637B (en) * | 2018-08-01 | 2020-02-14 | 河北大学 | ZIF-8 packaged hexachlorocyclotriphosphazene flame retardant, preparation method and application thereof, and flame-retardant epoxy resin |
| CN108752637A (en) * | 2018-08-01 | 2018-11-06 | 河北大学 | A kind of ZIF-8 encapsulation hexachlorocyclotriph,sphazene fire retardant, preparation method and application and fire retarding epoxide resin |
| CN109705329A (en) * | 2018-12-28 | 2019-05-03 | 广东工业大学 | A kind of ring opening catalyst and its preparation method and application that can be recycled |
| CN109705329B (en) * | 2018-12-28 | 2021-02-12 | 广东工业大学 | Recyclable ring-opening catalyst and preparation method and application thereof |
| CN110459776A (en) * | 2019-08-02 | 2019-11-15 | 北京化工大学常州先进材料研究院 | The preparation of FeCo hollow carbon micro-sphere material and its application in terms of electro-catalysis |
| CN110452547A (en) * | 2019-08-26 | 2019-11-15 | 北京理工大学 | ZIF-67 polysulfones ball fire retardant and preparation method thereof |
| CN112774713A (en) * | 2021-01-25 | 2021-05-11 | 华南理工大学 | Bimetallic core-shell catalyst for electrocatalysis-synergetic hydrogen production and preparation method and application thereof |
| CN112892574A (en) * | 2021-01-25 | 2021-06-04 | 华南理工大学 | Multi-element heterojunction core-shell catalyst suitable for electro-Fenton and preparation method and application thereof |
| CN112831174A (en) * | 2021-02-20 | 2021-05-25 | 青岛理工大学 | Preparation and application of ZnO @ MOF @ polyphosphazene flame retardant |
| CN112831174B (en) * | 2021-02-20 | 2022-05-06 | 青岛理工大学 | Preparation and application of ZnO @ MOF @ polyphosphazene flame retardant |
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