CN108745401A - A kind of porous carbon of nitrogen phosphorus doping-phosphatization rhodium catalyst and the preparation method and application thereof - Google Patents
A kind of porous carbon of nitrogen phosphorus doping-phosphatization rhodium catalyst and the preparation method and application thereof Download PDFInfo
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- CN108745401A CN108745401A CN201810576506.5A CN201810576506A CN108745401A CN 108745401 A CN108745401 A CN 108745401A CN 201810576506 A CN201810576506 A CN 201810576506A CN 108745401 A CN108745401 A CN 108745401A
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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
- B01J27/24—Nitrogen compounds
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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
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- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- 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
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Abstract
The invention discloses a kind of porous carbon of nitrogen phosphorus doping-phosphatization rhodium catalysts and the preparation method and application thereof,It is related to catalyst technical field,By polyalcohol,Rhodium is former and the substance containing nitrogen phosphorus compound is dispersed in water and stirs to form mixed sols,The composite nano materials that phosphatization rhodium is supported in porous charcoal are prepared using a step high-temperature calcination,Wherein porous carbon support is by the nitrogen in compound,Phosphorus is modified,Phosphatization rhodium nanoparticles load nitrogen,On the porous carbon of phosphorus modification,The nano particle size of wherein phosphatization rhodium is about 4-8 nanosizeds,The synthetic method of the porous carbon of nitrogen phosphorus doping prepared by the present invention-phosphatization rhodium catalyst is simple,It is reproducible,It is easy to operate,With size uniform,Purity is high,Cost is lower than platinum carbon material,It the productive prospectings such as can industrialize completely,It is equally matched in the performance and platinum carbon performance of electrolysis aquatic products hydrogen,With very useful industrial value.
Description
Technical field
The invention belongs to catalyst technical fields, and in particular to a kind of porous carbon of nitrogen phosphorus doping-phosphatization rhodium catalyst and
Preparation method and application.
Background technology
With the fast development of world energy sources revolution, replaced using hydrogen energy source by the cleaning of representative, regenerative resource traditional
Stone fuel is the inexorable trend of 21 century development.Therefore, seem particularly urgent for the development and utilization of hydrogen energy source.Electrolysis water system
Hydrogen is to realize one of the main method of extensive hydrogen manufacturing at present, but it is to limit its industrialization that the presence of overpotential, which causes energy consumption excessive,
The bottleneck of development.Although business Pt/C catalyst is liberation of hydrogen catalyst best at present, low reserves and high price limit
Its scale application.Therefore, liberation of hydrogen catalysis of the current maximum challenge no more than exploitation high activity, high stability and low cost
Agent is for replacing business Pt/C catalyst.
Metal phosphide shows excellent stability and catalytic activity, but current metal phosphide is at reality
The room stage is tested, it is difficult to synthesize on a large scale.Metal Ru2 and Rh2P have the property mutually compared with business Pt/C catalyst, such as
Tsinghua University's teacher's Li Yadong project has just synthesized a kind of Rh2P, the Rh2P of such method synthesis in acid condition, catalytic
Can be due to business Pt/C catalyst, but can't be synthesized on a large scale since synthesis step is more complicated, so also in experiment
The room stage, so being badly in need of seeking a kind of extensive green simple method for synthesizing to prepare high performance phosphatization catalyst.
Invention content
According to the above-mentioned deficiencies of the prior art, the technical problem to be solved by the present invention is to propose a kind of letter of synthetic method and
The porous carbon for the nitrogen phosphorus doping that can be mass-produced-phosphatization rhodium catalyst and the preparation method and application thereof, in order to solve above-mentioned skill
Art problem, the technical solution adopted by the present invention are：
A kind of preparation method of the porous carbon of nitrogen phosphorus doping-phosphatization rhodium catalyst, the preparation method comprises the following steps：
1) organic matter of polyalcohol, phosphorus-nitrogen containing is added to the water mixing, obtains mixed solvent；
2) soluble rhodium salt is dissolved in the mixed solvent of step 1) preparation, after mixing, heating obtains colloidal sol colloid；
3) colloid for preparing step 2) is dried, and then high-temperature calcination obtains a nanometer phosphatization rhodium catalyst；
4) step 3) is obtained into phosphatization rhodium catalyst ethyl alcohol and water washing and drying.
Preferably, in the step (1) water and polyalcohol volume ratio 1-100:0.1-1.
Preferably, the polyalcohol is containing glucose, chitosan, sucrose or any substance of maltose.
Preferably, the organic matter of the phosphorus-nitrogen containing be phosphorous and nitrogen organic matter or phosphorous organic matter with it is nitrogenous organic
The mixture of object.
Preferably, the organic matter containing nitrogen phosphorus is：Double sweet phosphorus, melamine and dibastic sodium phosphate, melamine and plant
Sour sodium, protein and phytic acid, urea and dibastic sodium phosphate combination.
Preferably, the soluble rhodium salinity is 0.05-100mol/L.
Further, the soluble rhodium salinity is 0.1-5mol/L.
Preferably, the temperature of the heating is 50-300 DEG C, time 0.5-20h.
Preferably, the temperature of the drying is 40-180 DEG C, time 1-48h.
Further, the temperature of the drying is 60-150 DEG C, time 3-24h.
Preferably, the temperature of the high-temperature calcination is 400-1600 DEG C, time 1-48h.
Further, the temperature of the high-temperature calcination is 600-1100 DEG C, time 2-16h.
A kind of porous carbon of nitrogen phosphorus doping-phosphatization rhodium catalyst, adopts and is prepared with the aforedescribed process.
A kind of application of the porous carbon of nitrogen phosphorus doping-phosphatization rhodium catalyst, is mainly used on energy electrolytic water device.
Compared with prior art, beneficial effects of the present invention：
1. the synthetic method of the porous carbon of nitrogen phosphorus doping prepared by the present invention-phosphatization rhodium catalyst is simple, of low cost, energy
It is enough preparations of industrialization, reproducible, easy to operate, the nanocomposite of phosphatization rhodium load is can be obtained under the action of polyalcohol
Catalyst, and the product prepared has size uniform, purity high, and the size of phosphatization rhodium catalyst is about 4-30nm.
2. the porous carbon of nitrogen phosphorus doping prepared by the present invention-phosphatization rhodium catalyst has special composite construction, there is nitrogen
The particle of 4-8 nanosizeds is loaded on the porous carbon of phosphorus doping, phosphatization rhodium nanoparticles are wrapped among porous carbon, Er Qieben
The material used in method is all environmentally protective, and preparation process not will produce any waste, and not any toxicity；Institute
There is raw material to be easy to get, cost is very low, and production procedure is simple, can prepare the catalyst material of feather weight, easy to spread and industrial
Change.
Description of the drawings
Fig. 1 is the X-ray diffraction coatings for the porous carbon phosphatization rhodium nano material that the obtained nitrogen phosphorus of the present invention mixes；
Fig. 2 is the electromicroscopic photograph for the porous carbon phosphatization rhodium nano material that the obtained nitrogen phosphorus of the present invention mixes；
Fig. 3 is the alkaline electrolysis aquatic products hydrogen for the porous carbon phosphatization rhodium nano material that the obtained nitrogen phosphorus of the present invention mixes
LSV schemes；
Fig. 4 is the acidic electrolysis aquatic products hydrogen for the porous carbon phosphatization rhodium nano material that the obtained nitrogen phosphorus of the present invention mixes
LSV schemes.
Specific implementation mode
It below by the description to embodiment, is described in further detail, to help those skilled in the art to this hair
Bright inventive concept, technical solution have more complete, accurate and deep understanding.
Embodiment 1
The preparation method of the porous carbon of nitrogen phosphorus doping-phosphatization rhodium catalyst, specific as follows in the present embodiment：
1) into the water of 20 volumes, 1 volume of glucose, double 2 weight of sweet phosphorus is added, is uniformly mixed, is configured to mix
Solvent；
2) 2 volume of radium chloride is added in the mixed solvent, magnetic agitation 1h is configured to uniform mixed solution, and heats
To 150 DEG C, 2h is kept, mixed solution is become into colloidal sol colloid, it is cooling；
3) colloidal sol colloid will be obtained, is put into inside baking oven 60 DEG C, 48h is kept be dried to turning yellow powder, it will be yellow
Color powder grinds and is crossed with grinder 400 molecules of interest sieve, collects the product of grinding, is then placed in 600 DEG C of stove calcining
8h obtains porous carbon-phosphatization rhodium nano material of the nitrogen phosphorus doping of black；
4) it after cleaning the nano material of black water and ethyl alcohol several times, is dried in 100 DEG C of baking oven, you can obtain nitrogen
The porous carbon of phosphorus doping-phosphatization rhodium nanostructured materials catalyst.
The porous carbon of prepared nitrogen phosphorus doping-phosphatization rhodium nanostructured materials catalyst has special composite construction, has
The particle of the porous upper load 10-12nm sizes of nitrogen phosphorus doping, phosphatization rhodium nanoparticles are wrapped among porous carbon.
Using porous carbon-phosphatization rhodium nanostructured materials catalyst of 1 obtained nitrogen phosphorus doping of case study on implementation as electrolysis aquatic products
Hydrogen catalyst, simulation electrolysis water testing procedure are as follows：Porous carbon-phosphatization rhodium the nano material for weighing the nitrogen phosphorus doping prepared is urged
Agent 5mg is put into sample bottle, and the Nifom solution of the ethanol solution and 15 μ L of 485mL is added, and is put into ultrasound point in ultrasonic machine
It dissipates, then pipettes the solution that 10 μ L are prepared with liquid-transfering gun, drop on the electrode, is dried.Then the H of 0.5M/L is configured2SO4Solution
Aqueous solution with the KOH of 1M/L is as electrolyte.Using the overpotential for measuring electrolysis aquatic products hydrogen on electrochemical workstation CHI760
And its stability, obtain 10A/cm in acid condition2Under overpotential be 40me, 10A/cm under the conditions of alkalinity2Under mistake
Potential is 20meV.
Embodiment 2
The present embodiment with embodiment 1, unlike in the present embodiment,
Raw materials used step (1) is 20 volume of water, 2 weight of flour, 2 volume of 0.5 volume of melamine and phytic acid；
2 volume of rhodium nitrate is added in step (2), is heated to 120 DEG C, keeps 15h；
Step (3) drying temperature is 80 DEG C, time 48h, and calcination temperature is 1100 DEG C, time 8h；
Step (4) drying temperature is 110 DEG C.
The porous carbon of prepared nitrogen phosphorus doping-phosphatization rhodium nanostructured materials catalyst has special composite construction, has
The particle of the porous upper load 5-12nm sizes of nitrogen phosphorus doping, phosphatization rhodium nanoparticles are wrapped among porous carbon.
Using porous carbon-phosphatization rhodium nanostructured materials catalyst of 2 obtained nitrogen phosphorus doping of case study on implementation as electrolysis aquatic products
Hydrogen catalyst, test result is as follows for simulation electrolysis water：10A/cm in acid condition2Under overpotential be 30me, in alkalinity
Under the conditions of 10A/cm2Under overpotential be 17meV.
Embodiment 3
The present embodiment with embodiment 1, unlike in the present embodiment,
Raw materials used step (1) is 40 volume of water, 5 weight of starch, 3 volume of 2 weight of urea and phytic acid；
3 volume of rhodium nitrate is added in step (2), is heated to 90 DEG C, keeps 20h；
Step (3) drying temperature is 100 DEG C, time 48h, and calcination temperature is 1000 DEG C, time 8h；
Step (4) drying temperature is 110 DEG C.
The porous carbon of prepared nitrogen phosphorus doping-phosphatization rhodium nanostructured materials catalyst has special composite construction, has
The particle of the porous upper load 10-30nm sizes of nitrogen phosphorus doping, phosphatization rhodium nanoparticles are wrapped among porous carbon.
Using porous carbon-phosphatization rhodium nanostructured materials catalyst of 3 obtained nitrogen phosphorus doping of case study on implementation as electrolysis aquatic products
Hydrogen catalyst, test result is as follows for simulation electrolysis water：10A/cm in acid condition2Under overpotential be 40me, in alkalinity
Under the conditions of 10A/cm2Under overpotential be 25meV.
Embodiment 4
The present embodiment with embodiment 1, unlike in the present embodiment,
Raw materials used step (1) is 30 volume of water, 4 weight of corn flour, 2 weight of albumen powder, 2 weight of sodium phosphate；
2 volume of rhodium nitrate is added in step (2), is heated to 70 DEG C, keeps 20h；
Step (3) drying temperature is 100 DEG C, time 48h, and calcination temperature is 900 DEG C, time 8h；
Step (4) drying temperature is 100 DEG C.
The porous carbon of prepared nitrogen phosphorus doping-phosphatization rhodium nanostructured materials catalyst has special composite construction, has
The particle of the porous upper load 5-15nm sizes of nitrogen phosphorus doping, phosphatization rhodium nanoparticles are wrapped among porous carbon.
Using porous carbon-phosphatization rhodium nanostructured materials catalyst of 4 obtained nitrogen phosphorus doping of case study on implementation as electrolysis aquatic products
Hydrogen catalyst, test result is as follows for simulation electrolysis water：10A/cm in acid condition2Under overpotential be 36me, in alkalinity
Under the conditions of 10A/cm2Under overpotential be 24meV.
Embodiment 5
The present embodiment with embodiment 1, unlike in the present embodiment,
Raw materials used step (1) is 25 volume of water, 3 weight of mealy potato, 2 weight of 2 weight of imidazoles and sodium phytate；
4 volume of acetylacetone,2,4-pentanedione rhodium is added in step (2), is heated to 120 DEG C, keeps 10h；
Step (3) drying temperature is 105 DEG C, time 48h, and calcination temperature is 950 DEG C, time 10h；
Step (4) drying temperature is 100 DEG C.
The porous carbon of prepared nitrogen phosphorus doping-phosphatization rhodium nanostructured materials catalyst has special composite construction, has
The particle of the porous upper load 5-13nm sizes of nitrogen phosphorus doping, phosphatization rhodium nanoparticles are wrapped among porous carbon.
Using porous carbon-phosphatization rhodium nanostructured materials catalyst of 5 obtained nitrogen phosphorus doping of case study on implementation as electrolysis aquatic products
Hydrogen catalyst, test result is as follows for simulation electrolysis water：10A/cm in acid condition2Under overpotential be 33me, in alkalinity
Under the conditions of 10A/cm2Under overpotential be 27meV.
Porous carbon-phosphatization rhodium catalyst that the present invention prepares nitrogen phosphorus doping is similar with business platinum carbon performance, and stablizes
Performance is better than business platinum carbon, and preparation method is simple, large batch of can produce, so may be implemented to be commercialized completely, Fig. 1-4 is
Each performance map of the porous carbon of nitrogen phosphorus doping prepared by the present invention-phosphatization rhodium nanostructured materials catalyst.
The present invention is exemplarily described above in conjunction with specific embodiment, it is clear that the present invention implements not by upper
The limitation of mode is stated, if the improvement of the various unsubstantialities of inventive concept and technical scheme of the present invention progress is used, or
It is not improved by the present invention design and technical solution directly apply to other occasions, protection scope of the present invention it
It is interior.Protection scope of the present invention should be determined by the scope of protection defined in the claims.
Claims (10)
1. a kind of preparation method of the porous carbon of nitrogen phosphorus doping-phosphatization rhodium catalyst, which is characterized in that the preparation method includes
Following steps：
1) organic matter of polyalcohol, phosphorus-nitrogen containing is added to the water mixing, obtains mixed solvent；
2) soluble rhodium salt is dissolved in the mixed solvent of step 1) preparation, after mixing, heating obtains colloidal sol colloid；
3) colloid for preparing step 2) is dried, and then high-temperature calcination obtains a nanometer phosphatization rhodium catalyst；
4) step 3) is obtained into phosphatization rhodium catalyst ethyl alcohol and water washing and drying.
2. the preparation method of the porous carbon of nitrogen phosphorus doping according to claim 1-phosphatization rhodium catalyst, which is characterized in that
The volume ratio 1-100 of water and polyalcohol in the step (1):0.1-1.
3. the preparation method of the porous carbon of nitrogen phosphorus doping according to claim 1-phosphatization rhodium catalyst, which is characterized in that
The polyalcohol is containing glucose, chitosan, sucrose or any substance of maltose.
4. the preparation method of the porous carbon of nitrogen phosphorus doping according to claim 1-phosphatization rhodium catalyst, which is characterized in that
The organic matter of the phosphorus-nitrogen containing is the mixture of phosphorous and nitrogen organic matter or phosphorous organic matter and nitrogenous organic matter.
5. the preparation method of the porous carbon of nitrogen phosphorus doping according to claim 1-phosphatization rhodium catalyst, which is characterized in that
The soluble rhodium salinity is 0.05-100mol/L.
6. the preparation method of the porous carbon of nitrogen phosphorus doping according to claim 1-phosphatization rhodium catalyst, which is characterized in that
The temperature of the heating is 50-300 DEG C, time 0.5-20h.
7. the preparation method of the porous carbon of nitrogen phosphorus doping according to claim 1-phosphatization rhodium catalyst, which is characterized in that
The temperature of the drying is 40-180 DEG C, time 1-48h, and the temperature of the drying is 600-1100 DEG C, time 2-16h.
8. the preparation method of the porous carbon of nitrogen phosphorus doping according to claim 1-phosphatization rhodium catalyst, which is characterized in that
The temperature of the high-temperature calcination is 400-1600 DEG C, time 1-48h.
9. a kind of porous carbon of nitrogen phosphorus doping-phosphatization rhodium catalyst, which is characterized in that any described using claim 1-8
Method is prepared.
10. a kind of application of the porous carbon of the nitrogen phosphorus doping described in claim 9-phosphatization rhodium catalyst, which is characterized in that main
It applies on energy electrolytic water device.
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Cited By (6)
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| CN111298815A (en) * | 2018-12-12 | 2020-06-19 | 中国科学院深圳先进技术研究院 | Platinum/phosphorus catalyst and preparation method and application thereof |
| CN111434607A (en) * | 2019-01-11 | 2020-07-21 | 国家纳米科学中心 | Metal phosphide and heteroatom-doped porous carbon composite material and preparation and application thereof |
| CN112209376A (en) * | 2019-07-09 | 2021-01-12 | 中国矿业大学(北京) | Preparation method of multi-heteroatom doped mesoporous carbon based on plant protein |
| CN112695343A (en) * | 2020-12-15 | 2021-04-23 | 桐乡市吉曼尔信息技术有限公司 | Preparation method and application of hydrogen evolution electrocatalyst of biomass-based graphitized porous carbon |
| CN114592211A (en) * | 2022-02-28 | 2022-06-07 | 西安交通大学 | Composite material with BCN (bulked continuous carbon) nanotubes loaded with rhodium phosphide nanoparticles as well as preparation method and application of composite material |
| WO2022120687A1 (en) * | 2020-12-10 | 2022-06-16 | 深圳先进技术研究院 | Phosphorus-activated platinum-based catalyst, preparation method therefor, and application thereof |
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| CN112695343A (en) * | 2020-12-15 | 2021-04-23 | 桐乡市吉曼尔信息技术有限公司 | Preparation method and application of hydrogen evolution electrocatalyst of biomass-based graphitized porous carbon |
| CN114592211A (en) * | 2022-02-28 | 2022-06-07 | 西安交通大学 | Composite material with BCN (bulked continuous carbon) nanotubes loaded with rhodium phosphide nanoparticles as well as preparation method and application of composite material |
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Application publication date: 20181106 |