CN103922306A - Method for preparing high-content nitrogen-doped porous carbon materia - Google Patents
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Abstract
The invention discloses a method for preparing a high-content nitrogen-doped porous carbon material. The method includes the following steps: drying and crushing a biomass raw material to obtain granules, performing a high temperature carbonization treatment in a nitrogen atmosphere, and then performing a high temperature ammoniation treatment in an ammonia atmosphere to obtain the high-content nitrogen-doped porous carbon material. The method disclosed by the invention is simple and effective, easy to operate, convenient for large-scale volume production and is suitable for application in industrial production; in a material preparation process, pore forming and nitrogen doping are performed at the same time and are finished in one step, and therefore the method is simple and effective.
Description
Technical field
The invention belongs to technical field of nano material, relate in particular to a kind of preparation method of high content nitrogen doped porous carbon material.
Background technology
Porous carbon materials refers to the carbon material with Different Pore Structures, and its aperture can regulate and control according to the requirement of practical application (as absorption molecular dimension etc.), make its size in nanometer level microporous between micron order macropore.Porous carbon materials has the character of carbon material, as high in chemical stability, good conductivity, the advantage such as cheap; Meanwhile, the introducing of pore structure makes it have the features such as specific surface area is large, pore passage structure is controlled, aperture is adjustable simultaneously.Its these advantages make it aspect energy storage and separated research, be subject to extensive concern, mainly concentrate on the aspects such as selective adsorption, ultracapacitor and lithium-sulfur cell of hydrogen storage, methane storing, carbonic acid gas.
To carbon material, carrying out nitrogen-doped modified is current more popular research topic, because adulterate in porous carbon nitrogen-atoms can greatly change material surface tissue, its pore passage structure of modulation, strengthen its wetting ability, affect material surface pKa value, improve the electric transmission speed of material, thereby expand porous carbon materials at the range of application (J.Phys.Chem.C2010 in each field, 114,8581; Carbon2011,49,844; J.Mater.Chem.2012,22,19726; ACS Appl.Mater.Interfaces2013,5,5630).Porous carbon materials is carried out to nitrogen-doped modified conventional method and mainly contain two kinds: a kind of is in synthetic carbon material process, directly adulterate nitrogen-atoms, i.e. original position nitrating (Carbon2002,40,1353; Chem.Mater.2005,17,124; Angew.Chem.Int.Ed.2006,45,4467); Another kind is, by nitrogenous precursor (as ammonia, acetonitrile, urea etc.), synthetic carbon material is carried out to aftertreatment, i.e. aftertreatment nitrating (Carbon1994,32,1507).Research shows, with various carbon materials of different nitrogen sources difference thermal treatment such as ammonia, urea and nitric acid, can in carbon material, introduce chemical nitrogen.Post treatment method can obtain nitrogenous surface functional group and structure nitrogen, but the doping of nitrogen is lower, generally below 3%.The porous carbon materials that obtains high nitrogen-containing need be used original position nitriding conventionally, in hard template method or soft template method are prepared porous carbon process, introduces nitrogenous precursor.The most frequently used nitrogenous precursor comprises amido carbohydrate, trimeric cyanamide, benzene methanamine etc.Although can obtain the porous carbon of high nitrogen-containing by the method for original position nitrating, also exist a lot of problems, such as: preparation process need to be used many organic chemical reagents, and price is relatively costly; Remove template procedure and need to use the highly corrosive agents such as hydrofluoric acid, process very complicated and environment are unfriendly, and therefore this method is not suitable for industrial application.Therefore porous carbon materials, how simply and effectively to prepare high nitrogen-containing is still to need to make great efforts the problem that solves at present.
Summary of the invention
The object of this invention is to provide a kind of easy to operately, with low cost, be applicable to the preparation method of large-scale commercial production high content nitrogen doped porous carbon material.
To achieve these goals, the present invention is by the following technical solutions:
The invention provides a kind of preparation method of high content nitrogen doped porous carbon material, comprise the following steps: after biomass material is dried, is pulverized, obtain particle, under nitrogen atmosphere, carry out high temperature cabonization processing, then under ammonia atmosphere, carry out high temperature ammonification processing, obtain high content nitrogen doped porous carbon material.
Described biomass material is corn cob, coconut husk, the leaf of bamboo or fish-bone etc.
Described biomass material is dry, obtain after pulverizing particle be in loft drier at 100～150 ℃ time of drying be at least 24 hours, the rear particle size control that pulverizes and sieves is 25～880um.
During described high temperature cabonization is processed, the flow velocity of nitrogen is 0.5～1L/min, and temperature rise rate is 3～5 ℃/min, and temperature is 300～600 ℃, and the treatment time is 0.5～6 hour.
After described high temperature cabonization is processed, when temperature is 200-600 ℃, with ammonia, replace nitrogen at least three times.
During described high temperature ammonification is processed, the flow velocity of ammonia is 1～3L/min, and temperature is 400-900 ℃, and the treatment time is 1～10 hour, and temperature rise rate is 4～10 ℃/min.
After described high temperature ammonification is processed, when temperature is during lower than 400 ℃, stop passing into ammonia, ammonia is switched to nitrogen, under nitrogen atmosphere, continue to naturally cool to room temperature.
The specific surface area of described high content nitrogen doped porous carbon material is 400～1200m
2/ g.
The aperture of described high content nitrogen doped porous carbon material is 0.6～2nm.
The nitrogen content of described high content nitrogen doped porous carbon material is 1～13%.
The present invention compared with the existing technology, has the following advantages and beneficial effect:
1, method of the present invention utilizes the method for two step pyroprocessing to prepare nitrogen-doped porous carbon material, has broken through nitrogen-doped porous carbon material tradition preparation method's restriction, and carbonization and ammonifying process complete continuously, in ammonifying process, pore-creating and nitrogen doping are carried out simultaneously, and a step completes, and method is simple and effective.
2, the present invention be take natural biological raw material and is prepared porous carbon materials as fertile material, and raw material sources are extensive, with low cost.
3, the porous carbon materials that method of the present invention is prepared has high specific surface area, pore size distribution homogeneous, present typical pore characteristics, and there is high and controlled nitrogen content, at aspects such as the storage of gas and trapping, ultracapacitor and lithium-sulfur cells, have a good application prospect.
4, method of the present invention is simply effective, easy to operate, is convenient to large-scale mass production, is suitable for applying in industrial production; In material preparation process, pore-creating and nitrogen doping are carried out simultaneously, and a step completes, and method is simple and effective.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of high content nitrogen doped porous carbon material shown in embodiment 1.
Fig. 2 is the nitrogen adsorption desorption curve of the high content nitrogen doped porous carbon material that obtains of embodiment 1.
Fig. 3 is the pore size distribution curve of the high content nitrogen doped porous carbon material that obtains of embodiment 1.
Fig. 4 is the TEM figure of the high content nitrogen doped porous carbon material that obtains of embodiment 1.
Fig. 5 is the HRTEM figure of the high content nitrogen doped porous carbon material that obtains of embodiment 1.
Fig. 6 is the FT-IR curve of the high content nitrogen doped porous carbon material that obtains of embodiment 1.
Embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the present invention is further detailed explanation.
Embodiment 1
As shown in Figure 1, Fig. 1 is the schema of the preparation method of high content nitrogen doped porous carbon material shown in embodiment 1.
A kind of preparation method of high content nitrogen doped porous carbon material, comprise the following steps: biomass material corn cob is placed in to air dry oven, at 100 ℃, be at least 24 hours time of drying, the rear particle size control that pulverizes and sieves is 500um, the corn cob granule that is 500um by particle diameter is put into material boat, and material boat is placed in to atmosphere furnace; Sealing boiler tube is vacuumized, and then with nitrogen replacement twice, under nitrogen atmosphere, boiler tube is heated, and the flow velocity of nitrogen is 0.5L/min, and temperature rise rate is 5 ℃/min, from room temperature, be slowly warming up to 400 ℃, the treatment time is 3 hours, at 400 ℃, is incubated 3h; High temperature cabonization when temperature is 400 ℃, then vacuumizes boiler tube after processing fast, replaces nitrogen at least three times, and clean burner hearth with ammonia with ammonia; Under ammonia atmosphere, continue temperature programming and carry out high temperature ammonification processing, the flow velocity of ammonia is 1L/min, and temperature rises to 700 ℃ from 400 ℃, treatment time is 2 hours, temperature rise rate is 5 ℃/min, is incubated after 2h naturally cooling at 700 ℃, after high temperature ammonification is processed, when temperature is during lower than 400 ℃, stop passing into ammonia, ammonia is switched to nitrogen, under nitrogen atmosphere, continue to naturally cool to room temperature, obtain high content nitrogen doped porous carbon material.The specific surface area of high content nitrogen doped porous carbon material is 1200m
2/ g, pore size distribution homogeneous, is 0.6～2nm, nitrogen content is 8.87%.
As shown in Figure 2, Fig. 2 is the nitrogen adsorption desorption curve of the high content nitrogen doped porous carbon material that obtains of embodiment 1.Can find out that this curve is typical I type thermoisopleth, this illustrative material presents typical pore characteristics, and the specific surface area of this material reaches 1200m
2/ g.
As shown in Figure 3, Fig. 3 is the pore size distribution curve of the high content nitrogen doped porous carbon material that obtains of embodiment 1.As can be seen from Fig., this material mesopore mainly be take micropore as main, and aperture is mainly distributed between 0.6-2nm.
As shown in Figure 4 and Figure 5, Fig. 4 is the TEM figure of the high content nitrogen doped porous carbon material that obtains of embodiment 1; Fig. 5 is the HRTEM figure of this material.As can be seen from Figure 4, a large amount of slit-type nanoporouss are evenly distributed on carbon base body.As can be seen from Figure 5, carbon material presents turbostratic, and local microcosmos area presents certain ordered structure.
As shown in Figure 6, Fig. 6 is the FT-IR curve of the high content nitrogen doped porous carbon material that obtains of embodiment 1.Can find out, corn cob carbide presents the characteristic peak of Mierocrystalline cellulose, hemicellulose and xylogen, mainly take the stretching vibration of C-H and C=O as main.The infrared spectra of the nitrogen-doped porous carbon material that two step pyroprocessing make is completely different from corn cob carbide, demonstrates different surface functional groups.1120cm
-1, 1568cm
-1and 1928cm
-1three principal oscillation peaks at place are respectively to be caused by the outer formation vibration of N-H face, the vibration of N-H in-plane deformation and N-H stretching vibration, and this explanation has successfully been doped in carbon skeleton by this preparation method's nitrogen element.Nitrogen element is mainly that the form with amino and imino-exists.By ultimate analysis, test discovery, the nitrogen-doped porous carbon material obtaining by the present embodiment has high nitrogen content, and nitrogen content reaches 8.87%.
Embodiment 2
A kind of preparation method of high content nitrogen doped porous carbon material, comprise the following steps: biomass material corn cob is placed in to air dry oven, at 100 ℃, be at least 24 hours time of drying, the rear particle size control that pulverizes and sieves is 500um, the corn cob granule that is 500um by particle diameter is put into material boat, and material boat is placed in to atmosphere furnace; Sealing boiler tube is vacuumized, and then with nitrogen replacement twice, under nitrogen atmosphere, boiler tube is heated, and the flow velocity of nitrogen is 0.5L/min, and temperature rise rate is 5 ℃/min, from room temperature, be slowly warming up to 300 ℃, the treatment time is 3 hours, at 300 ℃, is incubated 3h; High temperature cabonization when temperature is 300 ℃, then vacuumizes boiler tube after processing fast, replaces nitrogen at least three times, and clean burner hearth with ammonia with ammonia; Under ammonia atmosphere, continue temperature programming and carry out high temperature ammonification processing, the flow velocity of ammonia is 1L/min, and temperature rises to 800 ℃ from 300 ℃, treatment time is 3 hours, temperature rise rate is 5 ℃/min, is incubated after 3h naturally cooling at 800 ℃, after high temperature ammonification is processed, when temperature is during lower than 400 ℃, stop passing into ammonia, ammonia is switched to nitrogen, under nitrogen atmosphere, continue to naturally cool to room temperature, obtain high content nitrogen doped porous carbon material.The specific surface area of high content nitrogen doped porous carbon material is 1178m
2/ g, pore size distribution homogeneous, is 0.6～2nm, nitrogen content is 12.24%.
Embodiment 3
A kind of preparation method of high content nitrogen doped porous carbon material, comprise the following steps: biomass material coconut husk is placed in to air dry oven, at 150 ℃, be at least 24 hours time of drying, the rear particle size control that pulverizes and sieves is 880um, the coconut husk particle that is 880um by particle diameter is put into material boat, and material boat is placed in to atmosphere furnace; Sealing boiler tube is vacuumized, and then with nitrogen replacement twice, under nitrogen atmosphere, boiler tube is heated, and the flow velocity of nitrogen is 1L/min, and temperature rise rate is 3 ℃/min, from room temperature, be slowly warming up to 300 ℃, the treatment time is 0.5 hour, at 300 ℃, is incubated 3h; High temperature cabonization when temperature is 300 ℃, then vacuumizes boiler tube after processing fast, replaces nitrogen at least three times, and clean burner hearth with ammonia with ammonia; Under ammonia atmosphere, continue temperature programming and carry out high temperature ammonification processing, the flow velocity of ammonia is 2L/min, and temperature rises to 400 ℃ from 300 ℃, treatment time is 1 hour, temperature rise rate is 4 ℃/min, is incubated after 2h naturally cooling at 400 ℃, after high temperature ammonification is processed, when temperature is during lower than 400 ℃, stop passing into ammonia, ammonia is switched to nitrogen, under nitrogen atmosphere, continue to naturally cool to room temperature, obtain high content nitrogen doped porous carbon material.The specific surface area of high content nitrogen doped porous carbon material is 400m
2/ g, pore size distribution homogeneous, is 0.6～2nm, nitrogen content is 1%.
Embodiment 4
A kind of preparation method of high content nitrogen doped porous carbon material, comprise the following steps: the biomass material leaf of bamboo is placed in to air dry oven, at 125 ℃, be at least 24 hours time of drying, the rear particle size control that pulverizes and sieves is 25um, the leaf of bamboo particle that is 25um by particle diameter is put into material boat, and material boat is placed in to atmosphere furnace; Sealing boiler tube is vacuumized, and then with nitrogen replacement twice, under nitrogen atmosphere, boiler tube is heated, and the flow velocity of nitrogen is 0.75L/min, and temperature rise rate is 4 ℃/min, from room temperature, be slowly warming up to 600 ℃, the treatment time is 6 hours, at 600 ℃, is incubated 3h; High temperature cabonization when temperature is 600 ℃, then vacuumizes boiler tube after processing fast, replaces nitrogen at least three times, and clean burner hearth with ammonia with ammonia; Under ammonia atmosphere, continue temperature programming and carry out high temperature ammonification processing, the flow velocity of ammonia is 3L/min, and temperature rises to 900 ℃ from 600 ℃, treatment time is 10 hours, temperature rise rate is 10 ℃/min, is incubated after 2h naturally cooling at 900 ℃, after high temperature ammonification is processed, when temperature is during lower than 400 ℃, stop passing into ammonia, ammonia is switched to nitrogen, under nitrogen atmosphere, continue to naturally cool to room temperature, obtain high content nitrogen doped porous carbon material.The specific surface area of high content nitrogen doped porous carbon material is 600m
2/ g, pore size distribution homogeneous, is 0.6～2nm, nitrogen content is 6%.
Embodiment 5
A kind of preparation method of high content nitrogen doped porous carbon material, comprise the following steps: biomass material fish-bone is placed in to air dry oven, at 130 ℃, be at least 24 hours time of drying, the rear particle size control that pulverizes and sieves is 480um, the fish-bone particle that is 480um by particle diameter is put into material boat, and material boat is placed in to atmosphere furnace; Sealing boiler tube is vacuumized, and then with nitrogen replacement twice, under nitrogen atmosphere, boiler tube is heated, and the flow velocity of nitrogen is 0.6L/min, and temperature rise rate is 4 ℃/min, from room temperature, be slowly warming up to 500 ℃, the treatment time is 4.5 hours, at 500 ℃, is incubated 3h; High temperature cabonization when temperature is 500 ℃, then vacuumizes boiler tube after processing fast, replaces nitrogen at least three times, and clean burner hearth with ammonia with ammonia; Under ammonia atmosphere, continue temperature programming and carry out high temperature ammonification processing, the flow velocity of ammonia is 2L/min, and temperature rises to 650 ℃ from 500 ℃, treatment time is 7 hours, temperature rise rate is 7 ℃/min, is incubated after 2h naturally cooling at 650 ℃, after high temperature ammonification is processed, when temperature is during lower than 400 ℃, stop passing into ammonia, ammonia is switched to nitrogen, under nitrogen atmosphere, continue to naturally cool to room temperature, obtain high content nitrogen doped porous carbon material.The specific surface area of high content nitrogen doped porous carbon material is 800m
2/ g, pore size distribution homogeneous, is 0.6～2nm, nitrogen content is 8%.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not departing from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. the preparation method of a high content nitrogen doped porous carbon material, it is characterized in that: comprise the following steps: after biomass material is dried, is pulverized, obtain particle, under nitrogen atmosphere, carry out high temperature cabonization processing, then under ammonia atmosphere, carry out high temperature ammonification processing, obtain high content nitrogen doped porous carbon material.
2. the preparation method of high content nitrogen doped porous carbon material according to claim 1, is characterized in that: described biomass material is corn cob, coconut husk, the leaf of bamboo or fish-bone.
3. the preparation method of high content nitrogen doped porous carbon material according to claim 1, it is characterized in that: described biomass material is dry, obtain after pulverizing particle be in loft drier at 100～150 ℃ time of drying be at least 24 hours, the rear particle size control that pulverizes and sieves is 25～880um.
4. the preparation method of high content nitrogen doped porous carbon material according to claim 1, it is characterized in that: during described high temperature cabonization is processed, the flow velocity of nitrogen is 0.5～1L/min, and temperature rise rate is 3～5 ℃/min, temperature is 300～600 ℃, and the treatment time is 0.5～6 hour.
5. the preparation method of high content nitrogen doped porous carbon material according to claim 1, is characterized in that: after described high temperature cabonization is processed, when temperature is 200-600 ℃, with ammonia, replace nitrogen at least three times.
6. the preparation method of high content nitrogen doped porous carbon material according to claim 1, it is characterized in that: during described high temperature ammonification is processed, the flow velocity of ammonia is 1～3L/min, and temperature is 400-900 ℃, treatment time is 1～10 hour, and temperature rise rate is 4～10 ℃/min.
7. the preparation method of high content nitrogen doped porous carbon material according to claim 1, it is characterized in that: after described high temperature ammonification is processed, when temperature is during lower than 400 ℃, stop passing into ammonia, ammonia is switched to nitrogen, under nitrogen atmosphere, continue to naturally cool to room temperature.
8. the preparation method of high content nitrogen doped porous carbon material according to claim 1, is characterized in that: the specific surface area of described high content nitrogen doped porous carbon material is 400～1200m
2/ g.
9. the preparation method of high content nitrogen doped porous carbon material according to claim 1, is characterized in that: the aperture of described high content nitrogen doped porous carbon material is 0.6～2nm.
10. the preparation method of high content nitrogen doped porous carbon material according to claim 1, is characterized in that: the nitrogen content of described high content nitrogen doped porous carbon material is 1～13%.
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| CN110104647B (en) * | 2019-05-07 | 2023-01-24 | 吉林农业大学 | Preparation method and application of biomass-based nitrogen-doped microporous carbon material |
| CN111573672A (en) * | 2020-07-10 | 2020-08-25 | 西南大学 | Preparation method and application of nitrogen-doped thin-layer hierarchical pore activated carbon material |
| CN113398977A (en) * | 2021-07-08 | 2021-09-17 | 青岛大学 | Nitrogen-doped carbon catalyst prepared by taking waste cigarette ends as carbon source and preparation method and application thereof |
| CN113398977B (en) * | 2021-07-08 | 2023-10-24 | 青岛大学 | Nitrogen-doped carbon catalyst prepared by taking waste cigarette ends as carbon source, and preparation method and application thereof |
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