CN105668541A - Preparation method of dozens-of-gram hierarchical pore mono-dispersed 200-300nm bowl-shaped carbon material - Google Patents
Preparation method of dozens-of-gram hierarchical pore mono-dispersed 200-300nm bowl-shaped carbon material Download PDFInfo
- Publication number
- CN105668541A CN105668541A CN201511027612.0A CN201511027612A CN105668541A CN 105668541 A CN105668541 A CN 105668541A CN 201511027612 A CN201511027612 A CN 201511027612A CN 105668541 A CN105668541 A CN 105668541A
- Authority
- CN
- China
- Prior art keywords
- bowl
- preparation
- type material
- stage porous
- carbon element
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a dozens-of-gram hierarchical pore mono-dispersed 200-300nm bowl-shaped carbon material. The method comprises the following steps: carrying out a hydrothermal reaction in an alcohol-water system with in situ generated SiO2 as a template, phenolic resin as a carbon source, cetyltrimethylammonium bromide as a surfactant and NH3.H2O as a catalyst, carbonizing the obtained product, and etching the carbonized product to remove the template in order to obtain the hierarchical pore mono-dispersed bowl-shaped carbon material. The preparation method has the advantages of simplicity, low energy consumption, low cost and environmental protection, and the hierarchical pore mono-dispersed bowl-shaped carbon material is a bowl-shaped structure with the particle size of 200-300nm, and has the advantages of distribution of a large amount of disordered pores, narrow distribution of apertures, good dispersibility, large specific surface area, high output, realization of large scale production, and potential application prospect in the field of catalyst carriers.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, the preparation method being specifically related to the bowl-type material with carbon element of a kind of tens grams of level multi-stage porous single dispersing 200～300nm.
Background technology
Micro--meso-porous carbon material has the pore structure of uniqueness, big specific surface area, stronger absorbability and chemistry, thermodynamic stability, is widely used in fields such as optics, electronics, biology, catalysis, medical treatment. In recent years, it has been carried out substantial amounts of research by domestic and international researcher, and mesoporous material science has become as in the world across one of hot research fields of subject crossing such as chemistry, physics, material, biology, more becomes an important milestone of material science development. At present, mesoporous carbon can be divided into two big classes: ordered mesopore carbon and unordered mesoporous carbon. Ordered mesopore carbon preparation process length consuming time, condition is difficult to control to, and yield is extremely low, is only limitted in laboratory and prepares and use. Although the preparation process of unordered mesoporous carbon is relatively easy, but its pattern is difficult to control to, and pattern difference frequently can lead to performance difference. Therefore, the mesoporous carbon preparing regular pattern is particularly important. And both at home and abroad preparation method about mesoporous carbon mainly has soft template method and hard template method. Soft template method is to be self-assembled into regular mesoscopic structure by hydrogen bond, electrostatic or interaction between block copolymer and surfactant, the method does not require nothing more than surfactant has stronger interaction with carbon matrix precursor, removing can also be decomposed in carbonisation, and carbon matrix precursor is also required to self-polymerization and forms the high-molecular bone shelf structure of the three-dimensional net structure with certain mechanical strength, it is ensured that will not collapse removing surfactant back skeleton structure. And the selection of carbon precursor and surfactant is required higher by the method, and carbonisation loss is more, and yield is relatively low, length consuming time, is not suitable for mass production. Hard template method is the SiO generated with teos hydrolysis2It is assembled into certain structure as template with surfactant, adds suitable carbon source and prepare silicon-carbon complex by infusion process or CVD, remove SiO with NaOH solution or HF solution etches afterwards2Template, can obtain mesoporous carbon.Hard template method is the anti-phase duplication of inorganic template, material can carry out controlled regulation and control by changing the space size of template, shape and structure, but this synthetic method length consuming time, and step is various, easily so as to subside when removing template. Under normal circumstances, the mesoporous carbon prepared by both approaches is spherical, and yield is relatively low. But the bowl-type mesoporous carbon of preparation yield, high-specific surface area has no report.
Summary of the invention
The technical problem to be solved be in that to overcome existing micro--meso-porous carbon material preparation method exist easily reunite, the problem such as pattern is uncontrollable, yield poorly, synthesis step is complicated, there is provided a kind of simple, cost is low, it is possible to the method preparing the multi-stage porous single dispersing bowl-type material with carbon element that tens grams of level particle diameters are 200～300nm.
Solve above-mentioned technical problem and be the technical scheme is that addition NH in the mixed system of dehydrated alcohol and water3·H2O, cetyl trimethylammonium bromide, resorcinol, tetraethyl orthosilicate and mass fraction are the formalin of 37%, wherein cetyl trimethylammonium bromide and tetraethyl orthosilicate, resorcinol, formaldehyde, NH3·H2The mol ratio of O is 1:7.5～8.5:1.0～3.5:2.5～7.5:5～6, stirs, 80～100 times hydro-thermal reactions 12～36 hours, and centrifugation, dry, by gained powder body at N2700～900 DEG C of carbonizations 1～2 hour in atmosphere, then by the NaOH aqueous solution supersound process 1～2 hour of 1～3mol/L, obtain the multi-stage porous single dispersing bowl-type material with carbon element that particle diameter is 200～300nm.
The volume ratio of above-mentioned dehydrated alcohol and water is 1:1.5～4, it is preferable that the volume ratio of dehydrated alcohol and water is 1:2.5.
Above-mentioned cetyl trimethylammonium bromide, tetraethyl orthosilicate, resorcinol, formaldehyde, NH3·H2The mol ratio of O is preferably 1:8.05:3.35:6.95:5.25.
The concentration of above-mentioned NaOH aqueous solution is preferably 3mol/L.
The present invention was preferably in hydro-thermal reaction at 100 DEG C 12～36 hours, and optimum selection is hydro-thermal reaction 24 hours at 100 DEG C.
Optimum selection of the present invention by gained powder body at N2850 DEG C of carbonizations 2 hours in atmosphere.
Compared with prior art, the invention have the advantages that and beneficial effect:
1, the inventive method energy consumption is low, and cost is low, and environmental friendliness is simple to operate.
2, the bowl shaped structure that multi-stage porous single dispersing material with carbon element is particle diameter 200～300nm prepared by the present invention, and on it, distribution has hole unordered in a large number, even particle size distribution, pore-size distribution is narrower, and specific surface area is bigger.
3, the inventive method once can prepare the product of tens grams of levels, and product yield is high, and the regular appearance of products obtained therefrom, good dispersion, and soilless sticking phenomenon occurs, and is suitable for large-scale production, has potential application prospect in catalyst carrier.
Accompanying drawing explanation
Fig. 1 is the TEM figure of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 1 preparation.
Fig. 2 is the SEM figure of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 1 preparation.
Fig. 3 is the N of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 1 preparation2Isothermal physical absorption curve.
Fig. 4 is the graph of pore diameter distribution of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 1 preparation.
Fig. 5 is the TEM figure of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 2 preparation.
Fig. 6 is the TEM figure of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 3 preparation.
Fig. 7 is the TEM figure of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 4 preparation.
Fig. 8 is the TEM figure of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 5 preparation.
Fig. 9 is the TEM figure of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 6 preparation.
Figure 10 is the N of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 6 preparation2Isothermal physical absorption curve.
Figure 11 is the graph of pore diameter distribution of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 6 preparation.
Figure 12 is the TEM figure of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 7 preparation.
Figure 13 is the N of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 7 preparation2Isothermal physical absorption curve.
Figure 14 is the graph of pore diameter distribution of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 7 preparation.
Figure 15 is the TEM figure of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 8 preparation.
Figure 16 is the N of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 8 preparation2Isothermal physical absorption curve.
Figure 17 is the graph of pore diameter distribution of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 8 preparation.
Figure 18 is the TEM figure of the multi-stage porous single dispersing bowl-type material with carbon element of embodiment 9 preparation.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in more detail, but the scope of protection of present invention is not limited to these embodiments.
Embodiment 1
Adding 0.15mL (2.16mmol) mass fraction in the mixed solution of 15mL water and 6mL dehydrated alcohol is the NH of 27%3·H2O, 0.15g (0.41mmol) CTAB, 0.15g (1.34mmol) resorcinol, stir, it is subsequently adding 0.75mL (3.30mmol) TEOS, stirring 10 minutes, adding 0.21mL (2.85mmol) mass fraction is the formalin of 37%, stirs, hydro-thermal reaction 24 hours at 100 DEG C, centrifugation, solid dries 10 hours at 80 DEG C, by dried gained powder body at N2850 DEG C of carbonizations 2 hours in atmosphere, then the powder body after carbonization is added room temperature supersound process 2 hours in the NaOH aqueous solution of 15mL3mol/L, products therefrom deionized water wash uses absolute ethanol washing three times to neutrality, 80 DEG C of freeze-day with constant temperature 10 hours, grind, obtain 0.1g multi-stage porous single dispersing bowl-type material with carbon element.
Obtained product adopts JEM-2100 (Japan) type transmission electron microscope, cold field emission scanning electron microscope FETEM (SU8020) and full-automatic specific surface area and micropore physical adsorption appearance (QUASORB-SI-4, Quantachrome company of the U.S.) carry out pattern and specific surface area and pore structure, aperture, pore volume sign, result is shown in Fig. 1～4. By Fig. 1 and Fig. 2 it can be seen that product is good dispersion, is of a size of the bowl shaped structure of 200～250nm, and on it, distribution has hole unordered in a large number. The specific surface area calculating products therefrom according to Fig. 3 BET method is 2822m2g-1, utilizing the pore volume that 2D-NLDFT model calculates is 2.8cm3g-1, the graph of pore diameter distribution of Fig. 4 can be seen that product is multi-stage porous nano-carbon material, haveThe micropore of left and right, also hasOn a small quantityLeft and right mesoporous.
Embodiment 2
Adding 0.15mL (2.16mmol) mass fraction in the mixed solution of 15mL water and 6mL dehydrated alcohol is the NH of 27%3·H2O, 0.15g (0.41mmol) CTAB, 0.05g (0.45mmol) resorcinol, stir, it is subsequently adding 0.75mL (3.30mmol) TEOS, stirring 10 minutes, adding 0.07mL (0.95mmol) mass fraction is the formalin of 37%, stirs, hydro-thermal reaction 24 hours at 100 DEG C, centrifugation, solid dries 10 hours at 80 DEG C, by dried gained powder body at N2850 DEG C of carbonizations 2 hours in atmosphere, then the powder body after carbonization is added room temperature supersound process 2 hours in the NaOH aqueous solution of 15mL3mol/L, products therefrom deionized water wash uses absolute ethanol washing three times to neutrality, 80 DEG C of freeze-day with constant temperature 10 hours, grind, obtain multi-stage porous single dispersing bowl-type material with carbon element (see Fig. 5) of 230～300nm.
Embodiment 3
Adding 0.15mL (2.16mmol) mass fraction in the mixed solution of 15mL water and 6mL dehydrated alcohol is the NH of 27%3·H2O, 0.15g (0.41mmol) CTAB, 0.10g (0.90mmol) resorcinol, stir, it is subsequently adding 0.75mL (3.30mmol) TEOS, stirring 10 minutes, adding 0.14mL (1.90mmol) mass fraction is the formalin of 37%, stirs, hydro-thermal reaction 24 hours at 100 DEG C, centrifugation, solid dries 10 hours at 80 DEG C, by dried gained powder body at N2850 DEG C of carbonizations 2 hours in atmosphere, then the powder body after carbonization is added room temperature supersound process 2 hours in the NaOH aqueous solution of 15mL3mol/L, products therefrom deionized water wash uses absolute ethanol washing three times to neutrality, 80 DEG C of freeze-day with constant temperature 10 hours, grind, obtain multi-stage porous single dispersing bowl-type material with carbon element (see Fig. 6) of 290～300nm.
Embodiment 4
Adding 0.15mL (2.16mmol) mass fraction in the mixed solution of 12mL water and 8mL dehydrated alcohol is the NH of 27%3·H2O, 0.15g (0.41mmol) CTAB, 0.15g (1.34mmol) resorcinol, stir, it is subsequently adding 0.75mL (3.30mmol) TEOS, stirring 10 minutes, adding 0.21mL (2.85mmol) mass fraction is the formalin of 37%, stirs, hydro-thermal reaction 36 hours at 80 DEG C, centrifugation, solid dries 10 hours at 80 DEG C, by dried gained powder body at N2700 DEG C of carbonizations 2 hours in atmosphere, then the powder body after carbonization is added room temperature supersound process 1 hour in the NaOH aqueous solution of 15mL3mol/L, products therefrom deionized water wash uses absolute ethanol washing three times to neutrality, 80 DEG C of freeze-day with constant temperature 10 hours, grind, obtain multi-stage porous single dispersing bowl-type material with carbon element (see Fig. 7) of 250～300nm.
Embodiment 5
Adding 0.15mL (2.16mmol) mass fraction in the mixed solution of 15mL water and 5mL dehydrated alcohol is the NH of 27%3·H2O, 0.15g (0.41mmol) CTAB, 0.15g (1.34mmol) resorcinol, stir, it is subsequently adding 0.75mL (3.30mmol) TEOS, stirring 10 minutes, adding 0.21mL (2.85mmol) mass fraction is the formalin of 37%, stirs, hydro-thermal reaction 12 hours at 100 DEG C, centrifugation, solid dries 10 hours at 80 DEG C, by dried gained powder body at N2900 DEG C of carbonizations 1 hour in atmosphere, then the powder body after carbonization is added room temperature supersound process 2 hours in the NaOH aqueous solution of 15mL1mol/L, products therefrom deionized water wash uses absolute ethanol washing three times to neutrality, 80 DEG C of freeze-day with constant temperature 10 hours, grind, obtain multi-stage porous single dispersing bowl-type material with carbon element (see Fig. 8) of 200～230nm.
Embodiment 6
Adding 1.5mL (21.60mmol) mass fraction in the mixed solution of 150mL water and 60mL dehydrated alcohol is the NH of 27%3·H2O, 1.5g (4.10mmol) CTAB, 1.5g (13.40mmol) resorcinol, stir, it is subsequently adding 7.5mL (33.00mmol) TEOS, stirring 10 minutes, adding 2.1mL (28.50mmol) mass fraction is the formalin of 37%, stirs, hydro-thermal reaction 24 hours at 100 DEG C, centrifugation, solid dries 10 hours at 80 DEG C, by dried gained powder body at N2850 DEG C of carbonizations 2 hours in atmosphere, then the powder body after carbonization is added room temperature supersound process 2 hours in the NaOH aqueous solution of 50mL3mol/L, products therefrom deionized water wash uses absolute ethanol washing three times to neutrality, 80 DEG C of freeze-day with constant temperature 10 hours, grind, obtain 2.6g multi-stage porous single dispersing bowl-type material with carbon element.As seen from Figure 9, compared with embodiment 1, even if raw material dosage increases by 10 times, product is still for good dispersion, the bowl shaped structure being of a size of 200～220nm. The specific surface area calculating products therefrom according to Figure 10 BET method is 1018m2g-1, utilizing the pore volume that 2D-NLDFT model calculates is 1.5cm3g-1, the graph of pore diameter distribution of Figure 11 can be seen that product is multi-stage porous nano-carbon material, haveThe micropore of left and right, also hasAnd it is a small amount ofThe meso-hole structure of left and right.
Embodiment 7
Adding 3.0mL (43.20mmol) mass fraction in the mixed solution of 300mL water and 120mL dehydrated alcohol is the NH of 27%3·H2O, 3.0g (8.20mmol) CTAB, 3.0g (26.80mmol) resorcinol, stir, it is subsequently adding 15.0mL (66.00mmol) TEOS, stirring 10 minutes, adding 4.2mL (57.00mmol) mass fraction is the formalin of 37%, stirs, hydro-thermal reaction 24 hours at 100 DEG C, centrifugation, solid dries 10 hours at 80 DEG C, by dried gained powder body at N2850 DEG C of carbonizations 2 hours in atmosphere, then the powder body after carbonization is added room temperature supersound process 2 hours in the NaOH aqueous solution of 100mL3mol/L, products therefrom deionized water wash uses absolute ethanol washing three times to neutrality, 80 DEG C of freeze-day with constant temperature 10 hours, grind, obtain 5.8g multi-stage porous single dispersing bowl-type material with carbon element. As seen from Figure 12, compared with embodiment 1, even if raw material dosage increases by 20 times, product is still good dispersion, is of a size of the bowl shaped structure of 220～250nm, and pattern and size do not change. The specific surface area calculating products therefrom according to Figure 13 BET method is 990m2g-1, utilizing the pore volume that 2D-NLDFT model calculates is 1.3cm3g-1, the graph of pore diameter distribution of Figure 14 can be seen that product is multi-stage porous nano-carbon material, haveWithThe micropore of left and right, also hasAndThe meso-hole structure of left and right.
Embodiment 8
Adding 9.0mL (129.6mmol) mass fraction in the mixed solution of 900mL water and 360mL dehydrated alcohol is the NH of 27%3·H2O, 9.0g (24.6mmol) CTAB, 9.0g (80.4mmol) resorcinol, stir, it is subsequently adding 45.0mL (198mmol) TEOS, stirring 10 minutes, adding 12.6mL (171mmol) mass fraction is the formalin of 37%, stirs, hydro-thermal reaction 24 hours at 100 DEG C, centrifugation, solid dries 10 hours at 80 DEG C, by dried gained powder body at N2850 DEG C of carbonizations 2 hours in atmosphere, then the powder body after carbonization is added room temperature supersound process 2 hours in the NaOH aqueous solution of 400mL3mol/L, products therefrom deionized water wash uses absolute ethanol washing three times to neutrality, 80 DEG C of freeze-day with constant temperature 10 hours, grind, obtain 18g multi-stage porous single dispersing bowl-type material with carbon element. As seen from Figure 15, compared with embodiment 1, even if raw material dosage increases by 60 times, product is still good dispersion, is of a size of the bowl shaped structure of about 300nm, and pattern and size do not change. The specific surface area calculating products therefrom according to Figure 16 BET method is 750m2g-1, utilizing the pore volume that 2D-NLDFT model calculates is 1.5cm3g-1, the graph of pore diameter distribution of Figure 17 can be seen that product is multi-stage porous nano-carbon material, haveWithThe micropore of left and right, also hasAndThe meso-hole structure of left and right.
Embodiment 9
Adding 18.0mL (259.20mmol) mass fraction in the mixed solution of 1800mL water and 720mL dehydrated alcohol is the NH of 27%3·H2O, 18.0g (49.20mmol) CTAB, 18.0g (160.80mmol) resorcinol, stir, it is subsequently adding 90.0mL (396.00mmol) TEOS, stirring 10 minutes, adding 25.2mL (351.60mmol) mass fraction is the formalin of 37%, stirs, hydro-thermal reaction 24 hours at 100 DEG C, centrifugation, solid dries 10 hours at 80 DEG C, by dried gained powder body at N2850 DEG C of carbonizations 2 hours in atmosphere, then the powder body after carbonization is added room temperature supersound process 2 hours in the NaOH aqueous solution of 800mL3mol/L, products therefrom deionized water wash uses absolute ethanol washing three times to neutrality, 80 DEG C of freeze-day with constant temperature 10 hours, grind, obtain 31g multi-stage porous single dispersing bowl-type material with carbon element.As seen from Figure 18, compared with embodiment 1, even if raw material dosage increases by 120 times, product is still good dispersion, is of a size of the bowl shaped structure of about 220～250nm, and pattern and size do not change.
By above-described embodiment 6～9 it can be seen that after amplifying production, the inventive method still can obtain high yield, be of a size of the multi-stage porous single dispersing bowl-type material with carbon element of 200～300nm, and what the inventive method industrial mass was described prepares multi-stage porous single dispersing bowl-type material with carbon element.
Claims (8)
1. the preparation method of the bowl-type material with carbon element of one kind tens grams level multi-stage porous single dispersing 200～300nm, it is characterised in that: in the mixed system of dehydrated alcohol and water, add NH3·H2O, cetyl trimethylammonium bromide, resorcinol, tetraethyl orthosilicate and mass fraction are the formalin of 37%, wherein cetyl trimethylammonium bromide and tetraethyl orthosilicate, resorcinol, formaldehyde, NH3·H2The mol ratio of O is 1:7.5～8.5:1.0～3.5:2.5～7.5:5～6, stirs, 80～100 times hydro-thermal reactions 12～36 hours, and centrifugation, dry, by gained powder body at N2700～900 DEG C of carbonizations 1～2 hour in atmosphere, then by the NaOH aqueous solution supersound process 1～2 hour of 1～3mol/L, obtain the multi-stage porous single dispersing bowl-type material with carbon element that particle diameter is 200～300nm.
2. the preparation method of the bowl-type material with carbon element of tens grams of level multi-stage porous single dispersing 200～300nm according to claim 1, it is characterised in that: the volume ratio of described dehydrated alcohol and water is 1:1.5～4.
3. the preparation method of the bowl-type material with carbon element of tens grams of level multi-stage porous single dispersing 200～300nm according to claim 1, it is characterised in that: the volume ratio of described dehydrated alcohol and water is 1:2.5.
4. the preparation method of the bowl-type material with carbon element of tens grams of level multi-stage porous single dispersing 200～300nm according to claims 1 to 3 any one, it is characterised in that: described cetyl trimethylammonium bromide, tetraethyl orthosilicate, resorcinol, formaldehyde, NH3·H2The mol ratio of O is 1:8.05:3.35:6.95:5.25.
5. the preparation method of the bowl-type material with carbon element of tens grams of level multi-stage porous single dispersing 200～300nm according to claim 4 any one, it is characterised in that: hydro-thermal reaction 12～36 hours at 100 DEG C.
6. the preparation method of the bowl-type material with carbon element of tens grams of level multi-stage porous single dispersing 200～300nm according to claim 4 any one, it is characterised in that: hydro-thermal reaction 24 hours at 100 DEG C.
7. the preparation method of the bowl-type material with carbon element of tens grams of level multi-stage porous single dispersing 200～300nm according to claim 1, it is characterised in that: by gained powder body at N2850 DEG C of carbonizations 2 hours in atmosphere.
8. the preparation method of the bowl-type material with carbon element of tens grams of level multi-stage porous single dispersing 200～300nm according to claim 1, it is characterised in that: the concentration of described NaOH aqueous solution is 3mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511027612.0A CN105668541A (en) | 2015-12-31 | 2015-12-31 | Preparation method of dozens-of-gram hierarchical pore mono-dispersed 200-300nm bowl-shaped carbon material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511027612.0A CN105668541A (en) | 2015-12-31 | 2015-12-31 | Preparation method of dozens-of-gram hierarchical pore mono-dispersed 200-300nm bowl-shaped carbon material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105668541A true CN105668541A (en) | 2016-06-15 |
Family
ID=56298255
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511027612.0A Pending CN105668541A (en) | 2015-12-31 | 2015-12-31 | Preparation method of dozens-of-gram hierarchical pore mono-dispersed 200-300nm bowl-shaped carbon material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105668541A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244493A (en) * | 2018-09-04 | 2019-01-18 | 海南师范大学 | The preparation method of nitrogen, sulphur co-doped nano carbon bowl |
| CN114735696A (en) * | 2022-06-09 | 2022-07-12 | 国家电投集团氢能科技发展有限公司 | Hollow bowl-shaped carbon carrier and preparation method thereof, platinum-based catalyst and membrane electrode |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100297389A1 (en) * | 2009-05-20 | 2010-11-25 | Ut-Battelle, Llc | Mesoporous carbon materials |
| CN102642843A (en) * | 2012-05-10 | 2012-08-22 | 北京理工大学 | Method for simultaneously preparing multilevel-structure mesoporous silicon dioxide and carbon nano material |
| CN104909351A (en) * | 2015-06-02 | 2015-09-16 | 上海应用技术学院 | Nitrogen-doped mesoporous carbon sphere nanomaterial and preparation method thereof |
-
2015
- 2015-12-31 CN CN201511027612.0A patent/CN105668541A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100297389A1 (en) * | 2009-05-20 | 2010-11-25 | Ut-Battelle, Llc | Mesoporous carbon materials |
| CN102642843A (en) * | 2012-05-10 | 2012-08-22 | 北京理工大学 | Method for simultaneously preparing multilevel-structure mesoporous silicon dioxide and carbon nano material |
| CN104909351A (en) * | 2015-06-02 | 2015-09-16 | 上海应用技术学院 | Nitrogen-doped mesoporous carbon sphere nanomaterial and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244493A (en) * | 2018-09-04 | 2019-01-18 | 海南师范大学 | The preparation method of nitrogen, sulphur co-doped nano carbon bowl |
| CN114735696A (en) * | 2022-06-09 | 2022-07-12 | 国家电投集团氢能科技发展有限公司 | Hollow bowl-shaped carbon carrier and preparation method thereof, platinum-based catalyst and membrane electrode |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102642843B (en) | Method for simultaneously preparing multilevel-structure mesoporous silicon dioxide and carbon nano material | |
| CN103738969B (en) | Mesoporous silica and preparation method thereof | |
| Chen et al. | Synthesis of mesoporous silica with different pore sizes for cellulase immobilization: Pure physical adsorption | |
| CN101618869B (en) | Method for preparing small-size meso-porous hollow carbon sphere | |
| CN105502342A (en) | Method for preparing nanometer hollow carbon spheres with dopamine serving as carbon source | |
| CN105621384B (en) | A kind of synthetic method of carbon material | |
| CN102718205A (en) | Method for preparing three-dimensional hierarchical porous carbon | |
| Sun et al. | Mesoporous silica–carbon composites fabricated by a universal strategy of hydrothermal carbonization: controllable synthesis and applications | |
| CN105731424A (en) | Preparation method and application of nitrogen-doped nanoscale hollow carbon ball material | |
| CN104128163A (en) | Preparation method of microporous-mesoporous MIL-101 material and application thereof | |
| CN103223331A (en) | Preparation method of Ni (Co,Fe)-supported magnetic mesoporous carbon material with high adsorption performance on dyes | |
| Zhao et al. | Fabrication of mesoporous zeolite microspheres by a one-pot dual-functional templating approach | |
| Xie et al. | Kinetics-controlled synthesis of hierarchically porous materials with tunable properties from diverse building blocks | |
| CN111874889A (en) | Cellular three-dimensional network structure hierarchical pore carbon material and preparation method thereof | |
| CN102849750A (en) | Mesoporous silica with radial tunnels and preparation method thereof | |
| Zhang et al. | High electrocapacitive performance of bowl-like monodispersed porous carbon nanoparticles prepared with an interfacial self-assembly process | |
| CN105668541A (en) | Preparation method of dozens-of-gram hierarchical pore mono-dispersed 200-300nm bowl-shaped carbon material | |
| CN102275898B (en) | High-thermostability ordered mesoporous carbon material and preparation method thereof | |
| Zhang et al. | Performance of carbon-modified Pd/SBA-15 catalyst for 2-ethylanthraquinone hydrogenation | |
| CN105110381A (en) | Method for preparing nanopore alpha-Fe2O3 | |
| CN105645374B (en) | A kind of preparation method of meso-porous carbon material | |
| CN104741051A (en) | Method for preparing sugar-based carbon microsphere at low temperature | |
| CN105731414B (en) | A kind of method for preparing meso-porous carbon material | |
| CN104909384B (en) | Mordenite having diatomite morphology and multi-level pore channel structure, and preparation method thereof | |
| CN106622177A (en) | Spherical porous adsorbent based on carbon nanotubes as well as preparation method and application of spherical porous adsorbent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160615 |
|
| RJ01 | Rejection of invention patent application after publication |