CN109455701A - A kind of preparation method of the highly doped nitrogen phosphorus carbon nanosheet of highly effective hydrogen yield - Google Patents
A kind of preparation method of the highly doped nitrogen phosphorus carbon nanosheet of highly effective hydrogen yield Download PDFInfo
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- CN109455701A CN109455701A CN201811048554.3A CN201811048554A CN109455701A CN 109455701 A CN109455701 A CN 109455701A CN 201811048554 A CN201811048554 A CN 201811048554A CN 109455701 A CN109455701 A CN 109455701A
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- C01B32/00—Carbon; Compounds thereof
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
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- C01—INORGANIC CHEMISTRY
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Abstract
The present invention promotes the heteroatoms doping concentration such as nitrogen phosphorus in carbon material, and then increases the active site in carbon material, improves the catalytic activity of carbon material itself.It is dry by the way that by the nitrogen source of proper ratio, carbon source, phosphorus source is dissolved, is stirred, after the processes such as pyrolysis, obtain high concentration N-P doping carbon nanosheet.Preparation method of the present invention have raw material be easy to get, simple process, easy to operate, low in cost, advantages of environment protection, entire reaction process requires Preparation equipment low, conducive to industrialized production, the material of preparation has the nitrogen and phosphorus of high-dopant concentration, the performance that electro-catalysis produces hydrogen is effectively improved, there is actual industrial meaning.
Description
Technical field
Present invention relates particularly to a kind of preparation methods of the highly doped nitrogen phosphorus carbon nanosheet of highly effective hydrogen yield, belong to new energy material
The preparation technical field of material.
Background technique
In order to cope with the challenge of fossil fuel increasingly reduction, the conversion of electrochemistry renewable energy and storing technology and phase
The development for closing material is extremely urgent.Although noble metal-based catalysts are had excellent performance, it is low to be limited to noble metal reserves, it is at high cost and
It cannot achieve heavy industrialization application.Carbon material is a kind of rich reserves, and distribution is extensive, low in cost, is readily synthesized,
The numerous material of synthesis mode.Because excellent properties brought by its unique electronic structure in numerous industries by favor.But
It is in carbon material surface due to a lack of effective active site, the electro-catalysis H2-producing capacity of itself is very poor, can only be used as base
Bottom and other materials is compound promotes whole electro-catalysis H2-producing capacity, which greatly limits electro-catalysis to produce the fast of hydrogen electrode material
Speed development.Therefore how effectively to promote the active of substrate carbon material has for promoting whole electro-catalysis H2-producing capacity to pass
Important meaning.
Heteroatom adulterates carbon nanomaterial because of its rich, excellent electric conductivity, adjustable molecular structure and to acid
Property/alkaline environment tolerance and it is of interest by scientific research personnel.Especially two kinds of N, P elements with carbon with opposite electronegativity
In conjunction with by the synergistic effect between two hetero atoms, the unique electron donor property of carbon can be caused, enhance pi bond, thus greatly
The activity that its electro-catalysis produces hydrogen is improved greatly.Therefore, how effective " raising " nitrogen phosphorus atoms doping concentration becomes raising carbon materials
Expect a big approach of catalytic activity.However, researcher carries out the target of high concentration heteroatom doping also to carbon material at present
It cannot achieve, the codope carbon material system catalyst for producing hydrogen for efficient electro-catalysis also lacks design.
Therefore, the preparation method for exploring a kind of effective highly doped nitrogen phosphorus carbon nanosheet material has important reality meaning
Justice.The present invention passes through stirring --- drying --- process of pyrolysis by the heteroatoms such as introducing nitrogen phosphorus in carbon material, thus
The purpose for realizing effective " raising " nitrogen phosphorus atoms doping concentration, greatly improves the electro-catalysis H2-producing capacity of substrate carbon material.
Summary of the invention
The object of the invention is exactly to overcome the problems of the above-mentioned prior art, and providing one kind can be effective in carbon material
The method for adulterating nitrogen and phosphorus atoms, this method passes through stirring --- drying --- process of pyrolysis is realized mixes in carbon nanosheet
The nitrogen phosphorus heteroatom of the miscellaneous high concentration being evenly distributed, greatly improves the electro-catalysis H2-producing capacity of substrate carbon material, to meet
Currently to the demand of new energy materials.
The object of the invention can be achieved through the following technical solutions:
A kind of preparation method of the highly doped nitrogen phosphorus carbon nanosheet of highly effective hydrogen yield, including the following steps:
(1) a certain proportion of nitrogen source, phosphorus source and carbon source are placed in the deionized water of certain volume, at 40~100 DEG C
Then solution is placed in drying in baking oven and obtains predecessor A by 30~90 minutes formation clear solutions of magnetic agitation1。
(2) by predecessor A1Be transferred in tube furnace under protective atmosphere, 600~1100 DEG C high-temperature process 30 minutes to 5
After hour, the carbon material of heteroatom doping is just obtained after cooled to room temperature.
Nitrogen source described above is glycine, urea, melamine, azo-bis-isobutyl cyanide, one of chitin or several
Kind.；Phosphorus source is sodium phosphate, sodium metaphosphate, triphenyl phosphorus, phytic acid, one or more of red phosphorus；Carbon source is carbon black, graphene,
Sodium carbonate, sodium bicarbonate, one of sodium oxalate or a variety of.
The obtained electrode using high concentration N-P doping carbon nanosheet as electro-catalysis highly effective hydrogen yield produced according to the present invention
Material, structure novel.The material can not only effectively promote the doping concentration of nitrogen phosphorus in carbon material, and mixing in high concentration N-P
Under the influence of miscellaneous amount, H2-producing capacity is splendid in an acidic solution.
The present invention is based on the heteroatoms doping concentrations such as nitrogen phosphorus in promotion carbon material, and then it is living to increase the catalysis in carbon material
Property site, improve carbon material itself catalytic activity.By the way that by the nitrogen source of proper ratio, carbon source, phosphorus source is dissolved, stirring is mixed
It closes, it is dry, after the processes such as pyrolysis, obtain high concentration N-P doping carbon nanosheet.Preparation method of the present invention have raw material be easy to get, work
Skill is simple and convenient to operate, is low in cost, advantages of environment protection, and entire reaction process requires Preparation equipment low, is conducive to industry
Metaplasia produces, and the material of preparation has the nitrogen and phosphorus of high-dopant concentration, effectively improves the performance that electro-catalysis produces hydrogen, has practical
Industrial significance.
Detailed description of the invention
Fig. 1 is the Raman map of the carbon material of highly doped nitrogen phosphorus prepared by embodiment 1；
Fig. 2 is the x-ray photoelectron spectroscopy figure of the carbon material of highly doped nitrogen phosphorus prepared by embodiment 2；
Fig. 3 is the transmission electron microscope figure of the carbon material of highly doped nitrogen phosphorus prepared by embodiment 3；
Fig. 4 is the linear scan curve of the carbon material of highly doped nitrogen phosphorus prepared by embodiment 4.
Specific embodiment
Below in conjunction with attached drawing, the present invention is described in detail, helps to understand the present invention, but the present invention is not limited merely to
Following embodiment.
Embodiment 1
(1) urea and carbon black for being 4:1 by mass ratio, the sodium metaphosphate of 0.1~1g are placed in the deionized water of certain volume
In, 60 DEG C of magnetic agitations, 90 minutes formation clear solutions are dried to obtain predecessor A in an oven1。
(2) by predecessor A1It is transferred in tube furnace under protective atmosphere, 700 DEG C after high-temperature process 3 hours, natural cooling
Just the carbon material of heteroatom doping is obtained after to room temperature.
Fig. 1 is the Raman map of highly doped nitrogen phosphorus carbon material obtained by the present embodiment, is as can be seen from the figure obtained
Material be the lamella carbon material with graphene phase, and with a large amount of defect states presence.
Embodiment 2
(1) melamine and urea for being 2:1 by mass ratio, the sodium phosphate of 0.5~2g are placed in the deionization of certain volume
In water, 70 DEG C of magnetic agitations, 90 minutes formation clear solutions are dried to obtain predecessor A in an oven1。
(2) by predecessor A1It is transferred in tube furnace under protective atmosphere, 800 DEG C after high-temperature process 3 hours, natural cooling
Just the carbon material of heteroatom doping is obtained after to room temperature.
Fig. 2 is the x-ray photoelectron spectroscopy figure of the carbon material of highly doped nitrogen phosphorus obtained by the present embodiment, can from figure
See, nitrogen and phosphorus content is contained in resulting materials, and nitrogen content is 3.91%, phosphorus content 6.77%.
Embodiment 3
It (1) is 4:1 melamine and carbon black by mass ratio, the phytic acid of 0.1~10ml is placed in the deionized water of certain volume
In, 70 DEG C of magnetic agitations, 90 minutes formation clear solutions are dried to obtain predecessor A in an oven1。
(2) by predecessor A1It is transferred in tube furnace under protective atmosphere, 900 DEG C after high-temperature process 5 hours, natural cooling
Just the carbon material of heteroatom doping is obtained after to room temperature.
Fig. 3 is the transmission electron microscope figure of the carbon material of highly doped nitrogen phosphorus obtained by the present embodiment, as seen from the figure, should
The microscopic appearance of carbon material is lamellar structure.
Embodiment 4
It (1) is 4:1 melamine and glycine by mass ratio, the phytic acid of 0.1~10ml is placed in the deionization of certain volume
In water, 70 DEG C of magnetic agitations, 90 minutes formation clear solutions are dried to obtain predecessor A in an oven1。
(2) by predecessor A1It is transferred in tube furnace under protective atmosphere, 900 DEG C after high-temperature process 2 hours, natural cooling
Just the carbon material of heteroatom doping is obtained after to room temperature.
Fig. 4 is the linear scan curve of the carbon material of highly doped nitrogen phosphorus obtained by the present embodiment, it can be seen that in 10mA
Overpotential needed for the material is only 270mv under the current density of cm-2.
Embodiment 5
It (1) is 4:1 melamine and sodium carbonate by mass ratio, the triphenyl phosphorus of 0.1~0.5g is placed in going for certain volume
In ionized water, 70 DEG C of magnetic agitations, 90 minutes formation clear solutions are dried to obtain predecessor A in an oven1。
(2) by predecessor A1It is transferred in tube furnace under protective atmosphere, 900 DEG C after high-temperature process 2 hours, natural cooling
Just the carbon material of heteroatom doping is obtained after to room temperature.
Embodiment 6
(1) by mass ratio be 4:1 melamine and sodium bicarbonate, the red phosphorus of 0.1~0.5g, be placed in certain volume go from
In sub- water, 70 DEG C of magnetic agitations, 90 minutes formation clear solutions are dried to obtain predecessor A in an oven1。
(2) by predecessor A1It is transferred in tube furnace under protective atmosphere, 900 DEG C after high-temperature process 2 hours, natural cooling
Just the carbon material of heteroatom doping is obtained after to room temperature.
In conclusion a kind of preparation method of the highly doped nitrogen phosphorus carbon nanosheet material of highly effective hydrogen yield of the invention, the party
Method effectively improves the active site of carbon material surface, in turn by synthesizing high concentration N-P doped carbon nanometer sheet material
The electro-catalysis for greatly improving carbon material produces the performance of hydrogen, further applies new energy field.
Claims (8)
1. a kind of preparation method of the highly doped nitrogen phosphorus carbon nanosheet material of highly effective hydrogen yield, includes the following steps:
(1) a certain proportion of nitrogen source, phosphorus source and carbon source are placed in the deionized water of certain volume, the magnetic force at 40~100 DEG C
30~90 minutes formation clear solutions are stirred, solution is finally placed in drying in baking oven and obtains predecessor A1.
(2) predecessor A1 is transferred in tube furnace under protective atmosphere, 600~1100 DEG C high-temperature process 30 minutes to 5 hours
Afterwards, the carbon material of heteroatom doping is just obtained after cooled to room temperature.
2. preparation method as described in claim 1, it is characterised in that: the nitrogen source is glycine, urea, melamine, idol
Two isobutyl cyanogen of nitrogen, one or more of chitin.
3. preparation method as described in claim 1, it is characterised in that: phosphorus source is sodium phosphate, sodium metaphosphate, triphenyl
Phosphorus, phytic acid, one or more of red phosphorus.
4. preparation method as described in claim 1, it is characterised in that: the carbon source is carbon black, graphene, sodium carbonate, carbonic acid
Hydrogen sodium, one of sodium oxalate or a variety of.
5. preparation method as described in claim 1, it is characterised in that: the ratio of the nitrogen source carbon source is between 4:1~1:1.
6. preparation method as described in claim 1, it is characterised in that: the first step whipping temp is between 40~100 DEG C.
7. preparation method as described in claim 1, it is characterised in that: the first step mixing time 30~90 minutes it
Between.
8. preparation method as described in claim 1, it is characterised in that: the second step high-temperature process temperature 600~
Between 1100 DEG C；Reaction time is 0.5~5 hour.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970043A (en) * | 2019-04-08 | 2019-07-05 | 中国石油大学(华东) | Nitrogen-phosphor codoping carbon nanosheet and preparation method thereof, alkali metal-ion battery electrode, alkali metal-ion battery and electric device |
| CN111841595A (en) * | 2019-04-28 | 2020-10-30 | 中国科学院福建物质结构研究所 | Nitrogen-phosphorus co-doped carbon dioxide reduction electro-catalysis material and preparation method and application thereof |
| CN112479199A (en) * | 2020-11-24 | 2021-03-12 | 太原科技大学 | Preparation method of nitrogen, phosphorus and oxygen co-doped porous graphitized carbon nanosheet |
| CN114477172A (en) * | 2022-03-07 | 2022-05-13 | 大连工业大学 | Preparation method and application of straw-based porous carbon with honeycomb-shaped pore structure |
| CN114497600A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Nitrogen-phosphorus doped carbon material, platinum-carbon catalyst, and preparation methods and applications thereof |
| CN114774962A (en) * | 2022-05-11 | 2022-07-22 | 澄川绿氢新能源(济南)有限公司 | Solar photoelectrochemistry water decomposition photoelectrode and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109970043A (en) * | 2019-04-08 | 2019-07-05 | 中国石油大学(华东) | Nitrogen-phosphor codoping carbon nanosheet and preparation method thereof, alkali metal-ion battery electrode, alkali metal-ion battery and electric device |
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| CN111841595A (en) * | 2019-04-28 | 2020-10-30 | 中国科学院福建物质结构研究所 | Nitrogen-phosphorus co-doped carbon dioxide reduction electro-catalysis material and preparation method and application thereof |
| CN111841595B (en) * | 2019-04-28 | 2022-06-10 | 中国科学院福建物质结构研究所 | Nitrogen-phosphorus co-doped carbon dioxide reduction electro-catalysis material and preparation method and application thereof |
| CN114497600A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Nitrogen-phosphorus doped carbon material, platinum-carbon catalyst, and preparation methods and applications thereof |
| CN114497600B (en) * | 2020-10-23 | 2024-06-11 | 中国石油化工股份有限公司 | Nitrogen-phosphorus doped carbon material, platinum-carbon catalyst, and preparation methods and applications thereof |
| CN112479199A (en) * | 2020-11-24 | 2021-03-12 | 太原科技大学 | Preparation method of nitrogen, phosphorus and oxygen co-doped porous graphitized carbon nanosheet |
| CN114477172A (en) * | 2022-03-07 | 2022-05-13 | 大连工业大学 | Preparation method and application of straw-based porous carbon with honeycomb-shaped pore structure |
| CN114774962A (en) * | 2022-05-11 | 2022-07-22 | 澄川绿氢新能源(济南)有限公司 | Solar photoelectrochemistry water decomposition photoelectrode and preparation method and application thereof |
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