CN108314006A - A kind of ordered mesoporous carbon material and preparation method thereof - Google Patents

A kind of ordered mesoporous carbon material and preparation method thereof Download PDF

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CN108314006A
CN108314006A CN201810368228.4A CN201810368228A CN108314006A CN 108314006 A CN108314006 A CN 108314006A CN 201810368228 A CN201810368228 A CN 201810368228A CN 108314006 A CN108314006 A CN 108314006A
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carbon material
preparation
ordered mesoporous
mesoporous carbon
carbonization
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CN108314006B (en
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袁红
马秀花
王云杰
张泓
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North Minzu University
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    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract

The present invention provides a kind of ordered mesoporous carbon materials and preparation method thereof, belong to meso-porous carbon material field.Preparation method includes:Silica/template the composite material prepared using nonionic surfactant and acid solution and water are mixed to get carbonization substrate, then carbonization substrate is subjected to heating carbonization with the heating rate of 0.5~3 DEG C/min;Heating carbonization includes the carbonation stage of three heat preservations:The holding temperature of first carbonation stage is 140~150 DEG C, and soaking time is 0.7~1.3h;The holding temperature of second carbonation stage is 300~330 DEG C, and soaking time is 1.7~2.3h;The holding temperature of third carbonation stage is 350~520 DEG C, and soaking time is 12~14h;Second carbonation stage and third carbonation stage carry out under nitrogen atmosphere.This method is without additional addition carbon source, and preparation method is simple, and the duct of obtained meso-porous carbon material is arranged in high-sequential shape.

Description

A kind of ordered mesoporous carbon material and preparation method thereof
Technical field
The present invention relates to meso-porous carbon material fields, in particular to a kind of ordered mesoporous carbon material and preparation method thereof.
Background technology
Ordered mesopore carbon is a kind of novel mesoporous material.Ordered mesopore carbon has regularly arranged pore passage structure, endoporus Aperture belongs to mesoporous (2~50nm), and order is good, and specific surface area and hole hold larger, while having higher mechanical strength, relatively strong Adsorption capacity, good electric conductivity and ph stability, these features make ordered mesopore carbon do adsorbent, release agent, When catalyst, it is much smaller that fluid in the carbon material endoporus diffusional resistance is compared to the carbon materials such as active carbon, carbon fiber.Cause This, this ordered mesopore carbon is conducive to the mass transfer of fluid, so that absorption, separation, catalytic effect are better than common activated carbon Equal materials, especially for macromolecular substances.
In general, the preparation method of meso-porous carbon material, which is nanometer, pours into a mould hard template method, i.e., first prepare ordered mesoporous silica dioxide Hard template SBA-15, MCM-41 etc., then carbon source, such as sucrose, furfuryl alcohol, naphthalene, anthracene are filled by cast in the duct of template, Finally pass through high temperature cabonization, removes silica and obtain ordered mesopore carbon.Although this method successfully prepares ordered mesopore carbon Material, but preparation process complexity, especially the casting process poor controllability of carbon source, are easy to prepare non-ordered mesopore carbon, even There is micropore, the mesoporous and carbon material deposited.
In consideration of it, proposing this patent.
Invention content
The purpose of the present invention is to provide a kind of ordered mesoporous carbon materials and preparation method thereof, and this method is with non-ionic surface Activating agent is carbonized as template and carbon source by staged heating heating, without additional addition carbon source, preparation method letter It is single, and the duct of obtained meso-porous carbon material is arranged in high-sequential shape.
In order to realize that the above-mentioned purpose of the present invention, spy use following technical scheme:
A kind of preparation method of ordered mesoporous carbon material comprising:
Silica/template the composite material prepared using nonionic surfactant is mixed with acid solution and water Heating carbonization is carried out with the heating rate of 0.5~3 DEG C/min to carbonization substrate, then by carbonization substrate;
Heating carbonization includes the carbonation stage of three heat preservations:
The holding temperature of first carbonation stage is 140~150 DEG C, and soaking time is 0.7~1.3h;
The holding temperature of second carbonation stage is 300~330 DEG C, and soaking time is 1.7~2.3h;
The holding temperature of third carbonation stage is 350~520 DEG C, and soaking time is 12~14h;
Second carbonation stage and third carbonation stage carry out under nitrogen atmosphere.
One kind ordered mesoporous carbon material made from above-mentioned preparation method, the aperture of the ordered mesoporous carbon material is 3.6~ 0.2~0.4cm of 4.0nm, Kong Rongwei3/g
Compared with prior art, beneficial effects of the present invention for example including:
The preparation method of this ordered mesoporous carbon material provided by the invention, using nonionic surfactant as template Silica/template composite material is prepared in agent, then multiple to the silica/template using staged heating heating Condensation material carries out situ catalytic carbonization.This method directly using the high nonionic surfactant of phosphorus content as carbon source, without Carbon source is additionally poured into a mould again, to effectively solve the hole of the carbon material caused by the poor controllability that carbon source is poured into a mould in the prior art The wide problem of diameter distribution.Meanwhile being carbonized using staged heating heating, temperature program is strictly controlled, carbonization bottom is made Silica/template composite material in object is slowly carbonized during heating, effectively prevent the portion of the simple substance carbon after carbonization Point duct caves in, and to form the meso-porous carbon material of high-sequential, can be used for adsorbing, be catalyzed, the fields such as sensor.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technology description to be briefly described.
Fig. 1 is the transmission electron microscope picture of ordered mesoporous carbon material prepared by the embodiment of the present invention 1.
Fig. 2 is feature nitrogen adsorption-desorption isotherm figure of ordered mesoporous carbon material prepared by the embodiment of the present invention 1.
Fig. 3 is the graph of pore diameter distribution of ordered mesoporous carbon material prepared by the embodiment of the present invention 1.
Fig. 4 is the transmission electron microscope picture of ordered mesoporous carbon material prepared by the embodiment of the present invention 2.
Fig. 5 is feature nitrogen adsorption-desorption isotherm figure of ordered mesoporous carbon material prepared by the embodiment of the present invention 2.
Fig. 6 is the graph of pore diameter distribution of ordered mesoporous carbon material prepared by the embodiment of the present invention 2.
Fig. 7 is the transmission electron microscope picture of ordered mesoporous carbon material prepared by the embodiment of the present invention 3.
Fig. 8 is feature nitrogen adsorption-desorption isotherm figure of ordered mesoporous carbon material prepared by the embodiment of the present invention 3.
Fig. 9 is the graph of pore diameter distribution of ordered mesoporous carbon material prepared by the embodiment of the present invention 3.
Figure 10 is the transmission electron microscope picture of ordered mesoporous carbon material prepared by the embodiment of the present invention 4.
Figure 11 is feature nitrogen adsorption-desorption isotherm figure of ordered mesoporous carbon material prepared by the embodiment of the present invention 4.
Figure 12 is the graph of pore diameter distribution of ordered mesoporous carbon material prepared by the embodiment of the present invention 4.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is The conventional products that can be obtained by commercially available purchase.
Present embodiment provides a kind of ordered mesoporous carbon material, and preparation method includes:
Step S1:Will using silica/template composite material and acid solution prepared by nonionic surfactant and Water is mixed to get carbonization substrate,
Further, nonionic surfactant includes containing only tri- kinds of elements of C, H, O and the high non-ionic surface of phosphorus content Activating agent, more preferably, nonionic surfactant are total for polyethylene oxide-polypropylene oxide-polyethylene oxide three block Polymers (i.e. P123), molecular formula PEO-PPO-PEO.This nonionic surfactant is compound in silica/template Template is used as in the preparation process of material.
Further, silica/template composite material and the mass ratio of acid solution and water are 1~1.5:0.1:10, Or it is 1.1~1.4:0.1:10, or be 1.2~1.3:0.1:10.
Further, acid solution is the mixed solution of concentrated sulfuric acid solution or the concentrated sulfuric acid and phosphotungstic acid.Wherein, concentrated sulfuric acid solution The concentrated sulfuric acid for being 98% for mass fraction.
Preferably, acid solution is the mixed solution of the concentrated sulfuric acid and phosphotungstic acid, the wherein matter of the concentrated sulfuric acid (98%) and phosphotungstic acid Amount is than being (98~99):(1~2).
In the present embodiment, term " silica/template composite material " refers to containing nonionic surfactant Ordered mesoporous silicon-dioxide material.
Further, the set-up procedure of silica/template composite material includes:
By the mixed material formed by the nonionic surfactant and water, hydrochloric acid and tetraethyl orthosilicate in 35~45 18~30h, then 42~54h of crystallization at 90~110 DEG C, filtering are stirred at DEG C.
Preferably, mixed material is stirred to 20~28h at 37~43 DEG C, or mixed material is stirred at 39~41 DEG C Mix 22~26h;Then static 45~51h of crystallization at 94~106 DEG C again, or at 98~102 DEG C static crystallization 47~ 49h。
Further, in mixed material, nonionic surfactant, water, hydrochloric acid and tetraethyl orthosilicate mass ratio be 2 ~3.5:15:60:4.25;Or the mass ratio is 2.3~3.0:15:60:4.25;Or it is 2.5~2.7:15:60:4.25.
Step S2:Carbonization substrate is subjected to heating carbonization with the heating rate of 0.5~3 DEG C/min again;
Heating carbonization includes the carbonation stage of three heat preservations:
The holding temperature of (1) first carbonation stage is 140~150 DEG C, and soaking time is 0.7~1.3h;
The holding temperature of (2) second carbonation stages is 300~330 DEG C, and soaking time is 1.7~2.3h;
(3) holding temperature of third carbonation stage is 350~520 DEG C, and soaking time is 12~14h;
Wherein, the first carbonation stage can carry out under air atmosphere, can also carry out under nitrogen atmosphere, to remove carbon elimination Change H the and O elements in substrate.Second carbonation stage and third carbonation stage carry out under nitrogen atmosphere, avoid in carbonization substrate C element reacted during heating with oxygen generate CO2It escapes.
Further, third carbonation stage includes II sections of I sections of heat preservation and heat preservation;
The holding temperature of I sections of heat preservation is 340~460 DEG C, and soaking time is 5.5~6.5h;
The holding temperature of II sections of heat preservation is 490~520 DEG C, and soaking time is 6.5~7.5h;
Further, keeping the temperature I sections includes:By through the second carbonation stage carbonization after carbonized stock be warming up to 340~360 DEG C, 1.5~2.5h is kept the temperature, then is warming up to 390~410 DEG C, 1.5~2.5h of heat preservation, it is further heated up to 440~460 DEG C, heat preservations 1.5 ~2.5h.
Further, further include will be carbonized through third carbonation stage gained carbonized stock 8~12wt% (or for 9~ 11wt% is either 10wt%) HF solution in impregnate 1~3 day or impregnate 1.5~2.5 days.By being soaked in HF solution Stain removes silica inorganic hole wall, obtains ordered mesoporous carbon material.
The feature and performance of the present invention are described in further detail with reference to embodiments:
Embodiment 1
The present embodiment provides a kind of ordered mesoporous carbon material, preparation method includes:
A. silica/template composite material is prepared:
It is 2 in mass ratio by nonionic surfactant P123, deionized water, hydrochloric acid and tetraethyl orthosilicate:15:60: 4.25 mixing, stir for 24 hours at 40 DEG C, later in 100 DEG C of crystallization 48h, then are washed with deionized to neutrality, in 80 DEG C of dryings After obtain white solid to get.
B. carbonisation:
By the silica of gained/template composite material and the concentrated sulfuric acid (98%), water according to mass ratio 1.5:0.1:10 It is uniformly mixed and obtains carbonization substrate, be then carbonized according to following heating heating conditions:
Carbonization substrate is heated into 1h in air atmosphere at 140 DEG C, is then warming up to 330 DEG C of holding 2h under nitrogen atmosphere, then It is warming up to 350 DEG C of holdings 2h, 400 DEG C of holdings 2h, 450 DEG C of holdings 2h, 500 DEG C of holding 7h respectively.The above temperature-rise period heating speed Degree keeps 1 DEG C/min, dark brown solid after obtained carbonization.
C. silica is removed:
Obtained dark brown solid is immersed in 10% HF solution, 40h, filtering, deionization washing is stirred at room temperature It washs to neutral, drying, obtains ordered mesoporous carbon material.
Material characterization result is as shown in Figures 1 to 3:
Fig. 1 is the electron microscope of the ordered mesoporous carbon material, and as seen from Figure 1, prepared carbon material has orderly duct Structure.
Fig. 2 be the ordered mesoporous carbon material feature nitrogen adsorption-desorption isotherm figure, the visible apparent hysteresis loops of Fig. 2, Show there is mesoporous presence in prepared carbon material.
Fig. 3 is the graph of pore diameter distribution of the ordered mesoporous carbon material, as seen from Figure 3, pore-size distribution in prepared carbon material It is single, aperture 3.6nm.
In conjunction with Fig. 1~Fig. 3 it is found that this carbon material manufactured in the present embodiment is ordered into meso-porous carbon material, surface area is 340m2/ g, Kong Rongwei 0.2cm3/g。
Embodiment 2
The present embodiment provides a kind of ordered mesoporous carbon material, preparation method includes:
A. silica/template composite material is prepared:
It is 2.5 in mass ratio by nonionic surfactant P123, deionized water, hydrochloric acid and tetraethyl orthosilicate:15: 60:4.25 mixing, stir for 24 hours at 40 DEG C, later in 100 DEG C of crystallization 48h, then are washed with deionized to neutrality, at 80 DEG C Obtained after drying white solid to get.
B. carbonisation:
By the silica of gained/template composite material and mixed acid, (98% concentrated sulfuric acid is with phosphotungstic acid according to quality Than 99:1 is mixed to get), water is according to mass ratio 1.5:0.1:10 be uniformly mixed obtain carbonization substrate, then according to it is following heating plus Heat condition is carbonized:
Carbonization substrate is heated into 1h in air atmosphere at 150 DEG C, is then warming up to 320 DEG C of holding 2h under nitrogen atmosphere, then It is warming up to 350 DEG C of holdings 2h, 400 DEG C of holdings 2h, 450 DEG C of holdings 2h, 500 DEG C of holding 7h respectively.The above temperature-rise period heating speed Degree keeps 1 DEG C/min, dark brown solid after obtained carbonization.
C. silica is removed:
Obtained dark brown solid is immersed in 10% HF solution, 40h, filtering, deionization washing is stirred at room temperature It washs to neutral, drying, obtains ordered mesoporous carbon material.
Material characterization result is as shown in figures 4-6:
Fig. 4 is the electron microscope of the ordered mesoporous carbon material, from fig. 4, it can be seen that prepared carbon material has orderly duct Structure.
Fig. 5 be the ordered mesoporous carbon material feature nitrogen adsorption-desorption isotherm figure, the visible apparent hysteresis loops of Fig. 5, Show there is mesoporous presence in prepared carbon material.
Fig. 6 is the graph of pore diameter distribution of the ordered mesoporous carbon material, as seen from Figure 6, pore-size distribution in prepared carbon material It is single, aperture 4.0nm.
In conjunction with Fig. 4~Fig. 6 it is found that this carbon material manufactured in the present embodiment is ordered into meso-porous carbon material, surface area is 618m2/ g, Kong Rongwei 0.4cm3/g。
Embodiment 3
The present embodiment provides a kind of ordered mesoporous carbon material, preparation method includes:
A. silica/template composite material is prepared:
It is 3 in mass ratio by nonionic surfactant P123, deionized water, hydrochloric acid and tetraethyl orthosilicate:15:60: 4.25 mixing, stir for 24 hours at 40 DEG C, later in 100 DEG C of crystallization 48h, then are washed with deionized to neutrality, in 80 DEG C of dryings After obtain white solid to get.
B. carbonisation:
By the silica of gained/template composite material and mixed acid, (98% concentrated sulfuric acid is with phosphotungstic acid according to quality Than 99:1 is mixed to get), water is according to mass ratio 1:0.1:10 be uniformly mixed obtain carbonization substrate, then according to following heatings heating Condition is carbonized:
Carbonization substrate is heated into 1h in air atmosphere at 140 DEG C, is then warming up to 310 DEG C of holding 2h under nitrogen atmosphere, then It is warming up to 350 DEG C of holdings 2h, 400 DEG C of holdings 2h, 450 DEG C of holdings 2h, 500 DEG C of holding 7h respectively.The above temperature-rise period heating speed Degree keeps 1 DEG C/min, dark brown solid after obtained carbonization.
C. silica is removed:
Obtained dark brown solid is immersed in 10% HF solution, 40h, filtering, deionization washing is stirred at room temperature It washs to neutral, drying, obtains ordered mesoporous carbon material.
Material characterization result is as shown in figs. 7-9:
Fig. 7 is the electron microscope of the ordered mesoporous carbon material, and as seen from Figure 7, prepared carbon material has orderly duct Structure.
Fig. 8 be the ordered mesoporous carbon material feature nitrogen adsorption-desorption isotherm figure, the visible apparent hysteresis loops of Fig. 8, Show there is mesoporous presence in prepared carbon material.
Fig. 9 is the graph of pore diameter distribution of the ordered mesoporous carbon material, as seen from Figure 9, pore-size distribution in prepared carbon material It is single, aperture 3.9nm.
In conjunction with Fig. 7~Fig. 9 it is found that this carbon material manufactured in the present embodiment is ordered into meso-porous carbon material, surface area is 273m2/ g, Kong Rongwei 0.2cm3/g。
Embodiment 4
The present embodiment provides a kind of ordered mesoporous carbon material, preparation method includes:
A. silica/template composite material is prepared:
It is 3.5 in mass ratio by nonionic surfactant P123, deionized water, hydrochloric acid and tetraethyl orthosilicate:15: 60:4.25 mixing, stir for 24 hours at 40 DEG C, later in 100 DEG C of crystallization 48h, then are washed with deionized to neutrality, at 80 DEG C Obtained after drying white solid to get.
B. carbonisation:
By the silica of gained/template composite material and the concentrated sulfuric acid (98%), water according to mass ratio 1.5:0.1:10 It is uniformly mixed and obtains carbonization substrate, be then carbonized according to following heating heating conditions:
Carbonization substrate is heated into 1h in air atmosphere at 150 DEG C, is then warming up to 300 DEG C of holding 2h under nitrogen atmosphere, then It is warming up to 350 DEG C of holdings 2h, 400 DEG C of holdings 2h, 450 DEG C of holdings 2h, 500 DEG C of holding 7h respectively.The above temperature-rise period heating speed Degree keeps 1 DEG C/min, dark brown solid after obtained carbonization.
C. silica is removed:
Obtained dark brown solid is immersed in 10% HF solution, 40h, filtering, deionization washing is stirred at room temperature It washs to neutral, drying, obtains ordered mesoporous carbon material.
Material characterization result is as shown in Figure 10~Figure 12:
Figure 10 is the electron microscope of the ordered mesoporous carbon material, and as seen from Figure 10, prepared carbon material has orderly hole Road structure.
Figure 11 is feature nitrogen adsorption-desorption isotherm figure of the ordered mesoporous carbon material, the visible apparent lag of Figure 11 Ring shows there is mesoporous presence in prepared carbon material.
Figure 12 is the graph of pore diameter distribution of the ordered mesoporous carbon material, as seen from Figure 12, aperture point in prepared carbon material Cloth is single, aperture 3.8nm.
In conjunction with Figure 10~Figure 12 it is found that this carbon material manufactured in the present embodiment is ordered into meso-porous carbon material, surface area is 275m2/ g, Kong Rongwei 0.2cm3/g。
Embodiment 5
The present embodiment provides a kind of ordered mesoporous carbon material, preparation method includes:
A. silica/template composite material is prepared:
It is 3.5 in mass ratio by nonionic surfactant P123, deionized water, hydrochloric acid and tetraethyl orthosilicate:15: 60:4.25 mixing, 30h is stirred at 35 DEG C, later in 110 DEG C of crystallization 42h, then is washed with deionized to neutrality, at 80 DEG C Obtained after drying white solid to get.
B. carbonisation:
By the silica of gained/template composite material and the concentrated sulfuric acid (98%), water according to mass ratio 1.5:0.1:10 It is uniformly mixed and obtains carbonization substrate, be then carbonized according to following heating heating conditions:
Carbonization substrate is heated into 1.3h in nitrogen atmosphere at 145 DEG C, is then warming up to 320 DEG C of holdings under nitrogen atmosphere 1.7h, then it is warming up to 350 DEG C of holding 14h.The above temperature-rise period heating rate keeps 3 DEG C/min, dark brown after obtained carbonization Color solid.
C. silica is removed:
Obtained dark brown solid is immersed in 8% HF solution, 72h, filtering, deionized water washing is stirred at room temperature To neutral, drying, ordered mesoporous carbon material is obtained.
Embodiment 6
The present embodiment provides a kind of ordered mesoporous carbon material, preparation method includes:
A. silica/template composite material is prepared:
It is 3.5 in mass ratio by nonionic surfactant P123, deionized water, hydrochloric acid and tetraethyl orthosilicate:15: 60:4.25 mixing, 18h is stirred at 45 DEG C, later in 90 DEG C of crystallization 54h, then is washed with deionized to neutrality, is done at 80 DEG C Obtained after dry white solid to get.
B. carbonisation:
By the silica of gained/template composite material and the concentrated sulfuric acid (98%), water according to mass ratio 1.5:0.1:10 It is uniformly mixed and obtains carbonization substrate, be then carbonized according to following heating heating conditions:
Carbonization substrate is heated into 0.7h in air atmosphere at 145 DEG C, is then warming up to 310 DEG C of holdings under nitrogen atmosphere 2.3h, then it is warming up to 520 holding 12h.The above temperature-rise period heating rate keeps 0.5 DEG C/min, dark brown after obtained carbonization Color solid.
C. silica is removed:
Obtained dark brown solid is immersed in 12% HF solution, is stirred at room temperature for 24 hours, filtering, deionization washing It washs to neutral, drying, obtains ordered mesoporous carbon material.
Embodiment 7
The present embodiment provides a kind of ordered mesoporous carbon materials, and preparation method is similar to Example 1, the difference is that carbon Heating heating condition when change:
Carbonization substrate is heated into 1h in air atmosphere at 150 DEG C, is then warming up to 300 DEG C of holding 2h under nitrogen atmosphere, then It is warming up to 340 DEG C of holding 6.5h respectively, 520 DEG C keep 6.5.The above temperature-rise period heating rate keeps 1.5 DEG C/min, obtains Carbonization after dark brown solid.
Embodiment 8
The present embodiment provides a kind of ordered mesoporous carbon materials, and preparation method is similar to Example 1, the difference is that carbon Heating heating condition when change:
Carbonization substrate is heated into 1h in air atmosphere at 150 DEG C, is then warming up to 300 DEG C of holding 2h under nitrogen atmosphere, then It is warming up to 460 DEG C of holdings 5.5h, 490 DEG C of holding 7.5h respectively.The above temperature-rise period heating rate keeps 2 DEG C/min, obtains Carbonization after dark brown solid.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims Including belonging to all such changes and modifications in the scope of the invention.

Claims (10)

1. a kind of preparation method of ordered mesoporous carbon material, which is characterized in that it includes:
Silica/template the composite material prepared using nonionic surfactant and acid solution and water are mixed to get carbon Change substrate, then the carbonization substrate is subjected to heating carbonization with the heating rate of 0.5~3 DEG C/min;
The heating carbonization includes the carbonation stage of three heat preservations:
The holding temperature of first carbonation stage is 140~150 DEG C, and soaking time is 0.7~1.3h;
The holding temperature of second carbonation stage is 300~330 DEG C, and soaking time is 1.7~2.3h;
The holding temperature of third carbonation stage is 350~520 DEG C, and soaking time is 12~14h;
Second carbonation stage and the third carbonation stage carry out under nitrogen atmosphere.
2. the preparation method of ordered mesoporous carbon material according to claim 1, which is characterized in that the third carbonation stage Including II sections of I sections of heat preservation and heat preservation;
The holding temperature of I sections of the heat preservation is 340~460 DEG C, and soaking time is 5.5~6.5h;
The holding temperature of II sections of the heat preservation is 490~520 DEG C, and soaking time is 6.5~7.5h.
3. the preparation method of ordered mesoporous carbon material according to claim 2, which is characterized in that I sections of the heat preservation includes:
Carbonized stock after second carbonation stage carbonization is warming up to 340~360 DEG C, 1.5~2.5h of heat preservation, then is warming up to 390~410 DEG C, 1.5~2.5h of heat preservation, it is further heated up to 440~460 DEG C, 1.5~2.5h of heat preservation.
4. the preparation method of ordered mesoporous carbon material according to claim 1, which is characterized in that the non-ionic surface is lived Property agent includes polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer.
5. the preparation method of ordered mesoporous carbon material according to claim 1, which is characterized in that in the carbonization substrate, The silica/template composite material is 1~1.5 with the mass ratio of the acid solution and the water:0.1:10.
6. the preparation method of ordered mesoporous carbon material according to claim 1, which is characterized in that the acid solution is dense sulphur The mixed solution of acid solution or the concentrated sulfuric acid and phosphotungstic acid.
7. the preparation method of ordered mesoporous carbon material according to claim 6, which is characterized in that the concentrated sulfuric acid with it is described The mass ratio of phosphotungstic acid is 98~99:1~2.
8. the preparation method of ordered mesoporous carbon material according to claim 1, which is characterized in that further including will be through described The carbonized stock of three carbonation stages carbonization gained impregnates 1~3 day in the HF solution of 8~12wt%.
9. the preparation method of ordered mesoporous carbon material according to claim 1, which is characterized in that the silica/mould The preparation method of plate agent composite material includes:
By the mixed material formed by the nonionic surfactant and water, hydrochloric acid and tetraethyl orthosilicate at 35~45 DEG C Stir 18~30h, then 42~54h of crystallization at 90~110 DEG C, filtering.
10. a kind of ordered mesoporous carbon material made from claim 1~9 any one of them preparation method, which is characterized in that The aperture of the ordered mesoporous carbon material is 3.6~4.0nm, 0.2~0.4cm of Kong Rongwei3/g。
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Cited By (5)

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CN109553110A (en) * 2018-10-29 2019-04-02 山东大学 A kind of method that in-situ carburization prepares mesoporous Si-C composite material
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CN109553110A (en) * 2018-10-29 2019-04-02 山东大学 A kind of method that in-situ carburization prepares mesoporous Si-C composite material
CN109659154A (en) * 2018-12-26 2019-04-19 武汉工程大学 A kind of preparation method and applications of Carbon-based supercapacitor electrode material
CN109879269A (en) * 2019-04-12 2019-06-14 湖南师范大学 A method of using bamboo powder as the synthesising mesoporous carbon material of carbon source
CN109879269B (en) * 2019-04-12 2022-08-19 湖南师范大学 Method for synthesizing mesoporous carbon material by using bamboo powder as carbon source
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CN110170327B (en) * 2019-05-21 2022-04-19 南京工业大学 Mesoporous C/SiO2Supported heteropolyacid catalyst and preparation method and application thereof
CN113522345A (en) * 2021-07-22 2021-10-22 太原理工大学 Ordered mesoporous Al-SBA-15 supported sulfated zirconia solid acid material and preparation and application thereof

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