CN105536835A - Heteroatom-doped carbon-load iron carbide/ molybdenum or tungsten carbide catalyst and preparation method and application thereof - Google Patents
Heteroatom-doped carbon-load iron carbide/ molybdenum or tungsten carbide catalyst and preparation method and application thereof Download PDFInfo
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- CN105536835A CN105536835A CN201510962677.8A CN201510962677A CN105536835A CN 105536835 A CN105536835 A CN 105536835A CN 201510962677 A CN201510962677 A CN 201510962677A CN 105536835 A CN105536835 A CN 105536835A
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention belongs to the technical field of catalyst preparation, and in particular relates to a heteroatom-doped carbon-load iron carbide/ molybdenum or tungsten carbide catalyst and a preparation method and application thereof. The method comprises the following steps: (1) mixing molybdenum or tungsten heteropolyacid-containing @ metal-organic framework composite POMs @ MIL-100 (Fe) with melamine, and grinding; (2) under the protection of an inert gas, thermally treating at 800-1100 DEG C for 2-5h, cooling, and pickling with an acid to obtain heteroatom-doped carbon-load iron carbide/ molybdenum or tungsten carbide. The preparation method of the catalyst is simple in process, agglomeration of molybdenum or tungsten carbide nanoparticles can be maximally restricted, by doping of hetero atoms, more active sites can be introduced, the hydrogen production property of the material by electrolysis is excellent, and the heteroatom-doped carbon-load iron carbide/ molybdenum or tungsten carbide catalyst can be used in electro-catalytic oxygen reduction, lithium ion battery and other energy storage and conversion research fields.
Description
Technical field
The invention belongs to catalyst preparation technical field, be specifically related to a kind of carbon load cementite of Heteroatom doping/molybdenum carbide or tungsten catalyst and its preparation method and application.
Background technology
For solving energy crisis and problem of environmental pollution, Hydrogen Energy is subject to people's extensive concern as the oil-fired energy of the replacement be expected to most.Water electrolysis hydrogen production (liberation of hydrogen) is most economical and product hydrogen mode that is sustainable development.At present, the different liberation of hydrogen catalyst of best performance is platinum or platinum based catalyst, but it is expensive, and reserves are limited, hinders its application in practice.Therefore, finding the base metal eelctro-catalyst efficient, production cost is low is the key improving evolving hydrogen reaction efficiency.Researchers find that the materials such as non-noble metal sulfide, carbide have excellent Hydrogen Evolution Performance.Especially, late transition metal iron, cobalt, nickel etc. doping molybdenum base or tungsten-based catalyst be subject to researcher's extensive concern.But the existence of the problem such as reunion, low-density activated centre of nano particle still annoyings the synthesis of such material in building-up process.
Electrocatalytic Activity for Hydrogen Evolution Reaction agent should have transmits electronic capability preferably, and the material with carbon element with large specific area and loose structure is conducive to the transfer of electrolytical transmission and electronics.Especially, the porous carbon materials of Heteroatom doping is often selected as electrode material or carrier, for carrying transition metal nitride or carbide.Therefore, develop new synthetic method or develop new material and electrochemical energy is stored and transforms significant.In recent years, metal-organic framework materials (MOFs) is as the novel porous material of a class, developed rapidly, it has the feature such as bigger serface, porous, and as preparing the predecessor raw material of porous carbon materials, metal-organic framework composite can comprise different metallic atoms, can introduce different polyacid in its duct, there is the advantage of polyacid and MOFs simultaneously, organic ligand and the transition metal source of queueing discipline can be provided simultaneously.
Summary of the invention
In the face of the problems referred to above that prior art exists, for obtaining efficient, cheap base metal eelctro-catalyst, the invention provides a kind of carbon load cementite of Heteroatom doping/molybdenum carbide or tungsten catalyst and its preparation method and application.
The carbon load cementite/molybdenum carbide of Heteroatom doping or a preparation method for tungsten catalyst, it comprises the following steps:
(1) will mix with melamine, grind containing molybdenum or heteropoly tungstic acid metal-organic framework composite POMsMIL-100 (Fe);
(2) under the protection of inert gas, heat treatment 2 ~ 5h at 800 ~ 1100 DEG C, cooling, pickling, obtain carbon load cementite/molybdenum carbide or the tungsten of Heteroatom doping.
Wherein, adopt POMsMIL-100 (Fe) as predecessor, POMsMIL-100 (Fe) has the feature such as bigger serface, porous on the one hand, is conducive to the formation of porous carbon materials; Can transition metal atoms be introduced simultaneously, form small size, the finely dispersed transition metal based catalysts of porous carbon materials load; On the other hand, POMsMIL-100 (Fe) and melamine are ground, roasting (carbonization), the degree of graphitization of gained material with carbon element can be improved, thus improve its transmission electronic capability, and metallic atom can play its catalytic capability, finally form pattern, structure is unique, degree of graphitization is higher, the material with carbon element that conductive capability is stronger, its water electrolysis hydrogen production performance is better.
Described POMsMIL-100 (Fe) adopts solvent-thermal method to prepare, by heteropoly acid and Iron(III) chloride hexahydrate soluble in water, add trimethyl 1,3,5-benzene tri hydroxy acid ester and react, after centrifugation, adopt ethanol and ether to wash respectively.
Described heteropoly acid is phosphomolybdic acid, phosphotungstic acid, silicomolybdic acid or silico-tungstic acid.
The amount of described heteropoly acid is 0.5 ~ 3.5g, is preferably 1 ~ 3.2g; The quality of Iron(III) chloride hexahydrate is 1.5 ~ 3g, is preferably 1.7 ~ 2.5g; The quality of trimethyl 1,3,5-benzene tri hydroxy acid ester is 1 ~ 2.2g, is preferably 1.2 ~ 1.8g.
Described POMsMIL-100 (Fe) is 1:2 ~ 1:5 with the mass ratio of melamine, preferred 1:3 ~ 1:5.
Described inert gas is high pure nitrogen or argon gas.
Described heat treatment time is 2 ~ 5h, preferably 3 ~ 5h; Temperature is 800 ~ 900 DEG C.
Described pickling uses 0.5 ~ 1MH
2sO
4solution, preferably 0.5 ~ 0.8MH
2sO
4solution.
A kind of carbon load cementite/molybdenum carbide of the Heteroatom doping adopting described preparation method to obtain or tungsten catalyst.
A kind of carbon load cementite/molybdenum carbide of described Heteroatom doping or the application of tungsten catalyst in water electrolysis hydrogen production reaction.
Compared with prior art, the present invention has following excellent technique effect:
(1) the carbon load cementite/molybdenum carbide of the Heteroatom doping obtained by the present invention or tungsten catalyst nano-particles size less, be evenly distributed, there is loose structure, heteroatomic doping can introduce more avtive spots, change the electronic structure of carbon, its conductive capability is strengthened, and then have excellent water electrolysis hydrogen production performance, its take-off potential is 18 ~ 90mV (relative standard's hydrogen electrode), and Tafel slope is 45.2 ~ 70mVdec
-1, run the stability that 10 ~ 20h still keeps good continuously.
(2) industrial applicability: the carbon load cementite/molybdenum carbide of the Heteroatom doping obtained by the present invention or tungsten catalyst have excellent electrocatalysis characteristic, preparation method's technique is simple, significantly limit the reunion of molybdenum carbide or tungsten nano particle, process is easy to control, preparation cost is low, can be applicable to the research fields such as electrocatalytic oxidation reduction, the storage of lithium ion battery equal energy source and conversion.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method for the invention.
Fig. 2 is ESEM (SEM) photo of the carbon load cementite/molybdenum carbide of the embodiment of the present invention 1 gained Heteroatom doping.
Fig. 3 (a) ~ (b) is different multiplying transmission electron microscope (TEM) photo of the carbon load cementite/molybdenum carbide of the embodiment of the present invention 1 gained Heteroatom doping, wherein, Fig. 3 (b) is the amplification TEM photo of part in Fig. 3 (a).
Fig. 4 (a) ~ (b) is SEM and the TEM photo of the carbon load cementite/molybdenum carbide of the embodiment of the present invention 2 gained Heteroatom doping.
Detailed description of the invention
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that following embodiment is only for illustration of the present invention, and unrestricted the present invention.
Embodiment 1
The preparation of POMsMIL-100 (Fe): adopt 3.2g phosphomolybdic acid and 1.89g Iron(III) chloride hexahydrate to be dissolved in 50mL distilled water, add 1.36g trimethyl 1,3,5-benzene tri hydroxy acid ester, 72h is reacted at 130 DEG C, by centrifugation products obtained therefrom, ethanol and ether is adopted to wash respectively.
The preparation method of the carbon load cementite/molybdenum carbide sample of Heteroatom doping: POMsMIL-100 (Fe) is mixed with melamine (1:3), grinds; Under High Purity Nitrogen protection, 900 DEG C of heat treatment 3 ~ 5h, cooling, pickling, obtain final required sample.
Fig. 3 (a) ~ (b) be shown in by the TEM photo of gained sample, and nano-particles size obtained is as seen from the figure smaller, be evenly distributed.Its water electrolysis hydrogen production (liberation of hydrogen) performance is: take-off potential 18mV (relative standard's hydrogen electrode), Tafel slope is 45.2mVdec
-1, run 10h continuously and still keep good stability.
Embodiment 2
Preparation process in this example is substantially identical with above-described embodiment 1 with step, unlike: sintering temperature is adjusted to 1000 DEG C by 900 DEG C.Fig. 4 (a) ~ (b) be shown in by SEM and the TEM photo of gained sample.Its water electrolysis hydrogen production (liberation of hydrogen) performance is: take-off potential 80mV (relative standard's hydrogen electrode), Tafel slope is 59.2mVdec
-1, run 10h continuously and still keep good stability.
Claims (10)
1. the carbon load cementite/molybdenum carbide of Heteroatom doping or a preparation method for tungsten catalyst, is characterized in that, comprise the following steps:
(1) will mix with melamine, grind containing molybdenum or heteropoly tungstic acid metal-organic framework composite POMsMIL-100 (Fe);
(2) under the protection of inert gas, heat treatment 2 ~ 5h at 800 ~ 1100 DEG C, cooling, pickling, obtain carbon load cementite/molybdenum carbide or the tungsten of Heteroatom doping.
2. the carbon load cementite/molybdenum carbide of Heteroatom doping according to claim 1 or the preparation method of tungsten catalyst, it is characterized in that, described POMsMIL-100 (Fe) adopts solvent-thermal method to prepare, by heteropoly acid and Iron(III) chloride hexahydrate soluble in water, add trimethyl 1,3,5-benzene tri hydroxy acid ester reacts, and adopts ethanol and ether to wash after centrifugation respectively.
3. the carbon load cementite/molybdenum carbide of Heteroatom doping according to claim 1 and 2 or the preparation method of tungsten catalyst, it is characterized in that, described heteropoly acid is phosphomolybdic acid, phosphotungstic acid, silicomolybdic acid or silico-tungstic acid.
4. the carbon load cementite/molybdenum carbide of Heteroatom doping according to claim 1 and 2 or the preparation method of tungsten catalyst, is characterized in that, the amount of described heteropoly acid is 0.5 ~ 3.5g, is preferably 1 ~ 3.2g; The quality of Iron(III) chloride hexahydrate is 1.5 ~ 3g, is preferably 1.7 ~ 2.5g; The quality of trimethyl 1,3,5-benzene tri hydroxy acid ester is 1 ~ 2.2g, is preferably 1.2 ~ 1.8g.
5. the carbon load cementite/molybdenum carbide of Heteroatom doping according to claim 1 and 2 or the preparation method of tungsten catalyst, is characterized in that, described POMsMIL-100 (Fe) is 1:2 ~ 1:5 with the mass ratio of melamine, preferred 1:3 ~ 1:5.
6. the carbon load cementite/molybdenum carbide of Heteroatom doping according to claim 1 and 2 or the preparation method of tungsten catalyst, it is characterized in that, described inert gas is high pure nitrogen or argon gas.
7. the carbon load cementite/molybdenum carbide of Heteroatom doping according to claim 1 and 2 or the preparation method of tungsten catalyst, it is characterized in that, described heat treatment time is 2 ~ 5h, preferably 3 ~ 5h; Temperature is 800 ~ 900 DEG C.
8. the carbon load cementite/molybdenum carbide of Heteroatom doping according to claim 1 and 2 or the preparation method of tungsten catalyst, it is characterized in that, described pickling uses 0.5 ~ 1MH
2sO
4solution, preferably 0.5 ~ 0.8MH
2sO
4solution.
9. one kind adopts carbon load cementite/molybdenum carbide or the tungsten catalyst of the Heteroatom doping that preparation method obtains as described in claim 1-8 any one.
10. the carbon load cementite/molybdenum carbide of a Heteroatom doping as claimed in claim 9 or the application of tungsten catalyst in water electrolysis hydrogen production reaction.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637288A (en) * | 2016-12-27 | 2017-05-10 | 复旦大学 | Nitrogen-doped graphite-loaded phosphorus-doped molybdenum carbide nanowire electrocatalytic hydrogen production catalyst and preparation method thereof |
| US20170173565A1 (en) * | 2014-05-16 | 2017-06-22 | Dow Global Technologies Llc | Process for synthesizing iron carbide fischer-tropsch catalysts |
| CN107572498A (en) * | 2017-09-29 | 2018-01-12 | 程杰 | A kind of carbide doping porous charcoal and preparation method thereof |
| CN107815699A (en) * | 2017-11-10 | 2018-03-20 | 上海应用技术大学 | A kind of POMs C composites, preparation method and application |
| CN107999108A (en) * | 2017-12-13 | 2018-05-08 | 中国石油大学(华东) | Molybdenum carbide or tungsten carbide catalyst of a kind of nitrogen-phosphor codoping carbon load and its preparation method and application |
| CN109112570A (en) * | 2018-08-03 | 2019-01-01 | 闽南师范大学 | A kind of poly cyanamid composite electrode and preparation method thereof suitable for efficient electro-catalysis |
| CN109174188A (en) * | 2018-09-07 | 2019-01-11 | 常州大学 | A kind of preparation of Heteroatom doping carbon material/Ni-MOF composite electrocatalyst |
| CN109626670A (en) * | 2018-12-13 | 2019-04-16 | 中国科学技术大学苏州研究院 | A kind of porous Fe/C/N composite material and preparation method |
| CN110368969A (en) * | 2019-08-20 | 2019-10-25 | 南昌航空大学 | A kind of preparation method and applications loading Heteroatom doping molybdenum carbide liberation of hydrogen catalyst on carbon paper or carbon cloth |
| CN110923746A (en) * | 2018-09-20 | 2020-03-27 | 天津大学 | Nano-porous Fe-P-C material, preparation method thereof and application thereof in hydrogen production by water electrolysis |
| CN111215104A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Phosphorus-doped carbon-loaded molybdenum-tungsten carbide catalyst, and preparation and application thereof |
| CN111790453A (en) * | 2019-04-08 | 2020-10-20 | 湖北大学 | Cobalt/tungsten bimetallic organic frame cathode hydrogen evolution composite material and preparation method thereof |
| CN114100648A (en) * | 2021-11-23 | 2022-03-01 | 昭通学院 | Synthetic method of ZnMo-MOF-derived carbon-coated molybdenum carbide |
| CN114790297A (en) * | 2022-04-02 | 2022-07-26 | 东南大学 | Crystal state reduction-oxidation cluster-based complex and preparation method and application thereof |
| CN114904546A (en) * | 2022-05-17 | 2022-08-16 | 江西师范大学 | Ni/P-Mo @ Mo for producing hydrogen by hydrolyzing ammonia borane 2 C composite nano catalyst and preparation method and application thereof |
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Cited By (21)
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| US20170173565A1 (en) * | 2014-05-16 | 2017-06-22 | Dow Global Technologies Llc | Process for synthesizing iron carbide fischer-tropsch catalysts |
| US9833774B2 (en) * | 2014-05-16 | 2017-12-05 | Dow Global Technologies Llc | Process for synthesizing iron carbide Fischer-Tropsch catalysts |
| CN106637288A (en) * | 2016-12-27 | 2017-05-10 | 复旦大学 | Nitrogen-doped graphite-loaded phosphorus-doped molybdenum carbide nanowire electrocatalytic hydrogen production catalyst and preparation method thereof |
| CN107572498A (en) * | 2017-09-29 | 2018-01-12 | 程杰 | A kind of carbide doping porous charcoal and preparation method thereof |
| CN107815699A (en) * | 2017-11-10 | 2018-03-20 | 上海应用技术大学 | A kind of POMs C composites, preparation method and application |
| CN107999108B (en) * | 2017-12-13 | 2019-01-18 | 中国石油大学(华东) | Molybdenum carbide or tungsten carbide catalyst of a kind of load of nitrogen-phosphor codoping carbon and its preparation method and application |
| CN107999108A (en) * | 2017-12-13 | 2018-05-08 | 中国石油大学(华东) | Molybdenum carbide or tungsten carbide catalyst of a kind of nitrogen-phosphor codoping carbon load and its preparation method and application |
| CN109112570B (en) * | 2018-08-03 | 2019-07-30 | 闽南师范大学 | A kind of poly cyanamid composite electrode and preparation method thereof suitable for efficient electro-catalysis |
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| CN110923746A (en) * | 2018-09-20 | 2020-03-27 | 天津大学 | Nano-porous Fe-P-C material, preparation method thereof and application thereof in hydrogen production by water electrolysis |
| CN111215104A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Phosphorus-doped carbon-loaded molybdenum-tungsten carbide catalyst, and preparation and application thereof |
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Application publication date: 20160504 |