CN110451479A - A kind of environment-friendly preparation method thereof of multi-stage porous carbon material - Google Patents
A kind of environment-friendly preparation method thereof of multi-stage porous carbon material Download PDFInfo
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- CN110451479A CN110451479A CN201910846459.6A CN201910846459A CN110451479A CN 110451479 A CN110451479 A CN 110451479A CN 201910846459 A CN201910846459 A CN 201910846459A CN 110451479 A CN110451479 A CN 110451479A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
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Abstract
The present invention relates to a kind of environment-friendly preparation method thereofs of multi-stage porous carbon material, belong to multi-stage porous carbon field of material preparation, steps are as follows: native starch is mixed with deionized water, is stirred evenly by step 1, is gelatinized 20~60 minutes in water bath with thermostatic control；Sample is sealed by step 2, is statically placed in 2~10 DEG C of environment and is brought back to life 1~3 day to generate porous gel；Step 3 carries out multiple exchange of solvent to the sample in step 2 with etoh solvent or acetone；Step 4 carries out acidification 1~3 day to sample with acidulant；Sample drying is obtained mesoporous carbon precursor by step 5；Resulting mesoporous carbon precursor is placed in tube furnace, 300~1000 DEG C is fired to by way of temperature programming by step 6, and then constant temperature 1~5 hour, obtains product.The advantages that present invention has preparation process more mild and easy, prepares raw material and process green, and hole is flourishing, large specific surface area.
Description
Technical field:
The invention belongs to multi-stage porous carbon field of material preparation, and in particular to a kind of green preparation side of multi-stage porous carbon material
Method.
Background technique:
Mesoporous carbon is due to specific surface area with higher, preferable hydrothermal stability, hydrophobicity and organophilic characteristic etc.
Property makes it have critically important application value in fields such as the exploitations of absorption, separation, catalysis and new function material.But
The development of meso-porous carbon material is perfect not enough, can't be widely applied in actual production and life, many problems demands
It solves, also has very big development space that people is worth to go to explore carefully.Most of all, with the development of Green Chemistry and to more
The pursuit of high quality of the life, people need constantly to look for it is environmentally protective and it is non-harmful prepare raw material and " three wastes " production
Process route low, yield is high.
Polysaccharide is nontoxic, natural abundant, degradable, is the important renewable resource of sustainable development.Starch be on the earth most
One of biopolymer abundant and one of the most common polysaccharide, as all organic materials, they can also be carbonized.
This also means that should not be limited only to using people as food for starch, research starch should be more got down in chemistry
The application of the other fields such as industry, field of medicaments even material science.In early days, the starch example that success is developed in non-food applications
Attached bag includes the filler in the mixture production as purifying ground mass plastic-substitute, it is also possible to make the raw material of production polylactic acid, but
It is starch in the application for being used as the fields such as composite material, chromatography, adsorbent and catalyst carrier by low surface area and low
The limitation of pore volume.In order to break this limitation, it has been found that the structure of starch can be broken by starch gel, thus
Increase the specific surface area and pore volume of starch.
Summary of the invention:
For the problems of the prior art, the present invention provides a kind of environment-friendly preparation method thereof of multi-stage porous carbon material, solves
The disadvantages of previous carbon material impurity content is high, pore structure is changeable and stable physical form is limited, it is made by the method
The carbon material obtained has the features such as more regular pore structure, large specific surface area.
To realize the above technical purpose, the technical scheme is that
Native starch is mixed with deionized water, is stirred evenly by step 1, is gelatinized 20~60 minutes in water bath with thermostatic control；
Sample is sealed by step 2, is statically placed in 2~10 DEG C of environment and is brought back to life 1~3 day to generate porous gel；
Step 3 carries out multiple exchange of solvent to the sample in step 2 with etoh solvent or acetone；
Step 4 carries out acidification 1~3 day to sample with acidulant；
Sample drying is obtained mesoporous carbon precursor by step 5；
Resulting mesoporous carbon precursor is placed in tube furnace by step 6, it is fired to 300 by way of temperature programming~
1000 DEG C, then constant temperature 1~5 hour, obtains product.
In the step 1, native starch are as follows: cornstarch, potato starch, starch from sweet potato, wheaten starch etc. are edible
The mass ratio of one of starch or several mixtures, native starch and deionized water is 1: 7~1: 20, and mixing speed is
The temperature of 100r/min~300r/min, water bath with thermostatic control are controlled at 40 DEG C~90 DEG C.
The volume ratio of deionized water used is 1: 1~5: 1 in the amount and step 1 of solvent for use in the step 3, is guaranteed
Exchange of solvent effect.
In the step 4, available acidulant has: p-methyl benzenesulfonic acid, citric acid, succinic acid etc..
In the step 6, the rate of temperature programming is 2~10 DEG C/min.
The superiority that the present invention has:
1, experimental method is simple, and preparation process green is mild；
2, multi-stage porous carbon material specific surface area obtained is abundant, solves previous carbon material impurity content height, pore structure
The disadvantages of changeable.
Detailed description of the invention:
Fig. 1 is the electron-microscope scanning figure that multi-stage porous carbon material is made in the embodiment of the present invention 1；
Fig. 2 is the N that multi-stage porous carbon material is made in the embodiment of the present invention 12Adsorption desorption curve；
Fig. 3 is the graph of pore diameter distribution that multi-stage porous carbon material is made in the embodiment of the present invention 1.
Specific embodiment:
Further instruction is given to the present invention below by embodiment, but the present invention is not only limited to implement in detail below
Example.
Embodiment 1:
Step 1 mixes cornstarch and deionized water 1: 7 ratio in mass ratio, and the speed stirring of 100r/min is equal
It is even, 45min, the temperature 45 C of water bath with thermostatic control are gelatinized in water bath with thermostatic control；
Sample is sealed by step 2, is statically placed in 5 DEG C of environment and is brought back to life 2 days to generate porous gel；
Step 3 carries out multiple exchange of solvent with the acetone of 3 times of volumes of deionized water in step 1；
Step 4 carries out acidification 2 days to sample with acidulant p-methyl benzenesulfonic acid；
Sample drying is obtained mesoporous carbon precursor by step 5；
Resulting mesoporous carbon precursor is placed in tube furnace, by temperature programming according to the rate of 3 DEG C/min by step 6
800 DEG C are fired to, then constant temperature 3 hours, obtain product.
Embodiment 2:
Step 1 mixes cornstarch and deionized water 1: 10 ratio in mass ratio, and the speed stirring of 200r/min is equal
It is even, 30min, the temperature 50 C of water bath with thermostatic control are gelatinized in water bath with thermostatic control；
Sample is sealed by step 2, is statically placed in 5 DEG C of environment and is brought back to life 2 days to generate porous gel；
Step 3 carries out multiple exchange of solvent with the acetone of 2 times of volumes of deionized water in step 1；
Step 4 carries out acidification 2 days to sample with acidulant succinic acid；
Sample drying is obtained mesoporous carbon precursor by step 5；
Resulting mesoporous carbon precursor is placed in tube furnace, by temperature programming according to the rate of 4 DEG C/min by step 6
800 DEG C are fired to, then constant temperature 2 hours, obtain product.
Embodiment 3:
Step 1 mixes cornstarch and deionized water 1: 20 ratio in mass ratio, and the speed stirring of 300r/min is equal
It is even, 60min, the temperature 60 C of water bath with thermostatic control are gelatinized in water bath with thermostatic control；
Sample is sealed by step 2, is statically placed in 5 DEG C of environment and is brought back to life 2 days to generate porous gel；
Step 3 carries out multiple exchange of solvent with the ethyl alcohol of 5 times of volumes of deionized water in step 1；
Step 4 carries out acidification 3 days to sample with acidulant citric acid；
Sample drying is obtained mesoporous carbon precursor by step 5；
Resulting mesoporous carbon precursor is placed in tube furnace, by temperature programming according to the rate of 2 DEG C/min by step 6
1000 DEG C are fired to, then constant temperature 3 hours, obtain product.
The multi-stage porous carbon material prepared in embodiment is subjected to BET test, test result is as follows table:
| Title | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Specific surface area | 401.3245m2/g | 386.3022m2/g | 375.6338m2/g |
Above-described embodiment surface, using proper starch and water quality than can be prepared into specific surface area multi-stage porous carbon abundant
Material, during integral experiment, experiment condition green is mild, and experimental procedure is simple, can play in fields such as metal catalytic, absorption
Preferably application.
It should be noted that the announcement and elaboration of book, those skilled in the art in the invention may be used also according to the above description
To change and modify the above embodiment.Therefore, the invention is not limited to specific implementations disclosed and described above
Mode should also be as within scope of protection of the claims of the invention some equivalent modifications of the invention and change.
Claims (5)
1. the present invention relates to a kind of environment-friendly preparation method thereofs of multi-stage porous carbon material, which comprises the steps of:
Native starch is mixed with deionized water, is stirred evenly by step 1, is gelatinized 20~60 minutes in water bath with thermostatic control；
Sample is sealed by step 2, is statically placed in 2~10 DEG C of environment and is brought back to life 1~3 day to generate porous gel；
Step 3 carries out multiple exchange of solvent to the sample in step 2 with etoh solvent or acetone；
Step 4 carries out acidification 1~3 day to sample with acidulant；
Sample drying is obtained mesoporous carbon precursor by step 5；
Resulting mesoporous carbon precursor is placed in tube furnace, 300~1000 is fired to by way of temperature programming by step 6
DEG C, then constant temperature 1~5 hour, obtains product.
2. a kind of environment-friendly preparation method thereof of multi-stage porous carbon material according to claim 1, it is characterised in that: the step 1
In, native starch are as follows: one of edible starch such as cornstarch, potato starch, starch from sweet potato, wheaten starch is several
The mass ratio of the mixture of kind, native starch and deionized water is 1: 7~1: 20, and mixing speed is 100r/min~300r/
The temperature of min, water bath with thermostatic control are controlled at 40 DEG C~90 DEG C.
3. a kind of environment-friendly preparation method thereof of multi-stage porous carbon material according to claim 1, it is characterised in that: the step 3
The volume ratio of deionized water used is 1: 1~5: 1 in the amount and step 1 of middle solvent for use, guarantees exchange of solvent effect.
4. a kind of environment-friendly preparation method thereof of multi-stage porous carbon material according to claim 1, it is characterised in that: the step 4
In, available acidulant has: p-methyl benzenesulfonic acid, citric acid, succinic acid etc..
5. a kind of environment-friendly preparation method thereof of multi-stage porous carbon material according to claim 1, it is characterised in that: the step 6
In, the rate of temperature programming is 2~10 DEG C/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115974045A (en) * | 2022-12-06 | 2023-04-18 | 江西师范大学 | Method for preparing hard carbon by chemical gel synergistic basic metal oxide template method and application thereof |
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| US20030171633A1 (en) * | 2002-02-28 | 2003-09-11 | Teng Xu | Molecular sieve compositions, catalyst thereof, their making and use in conversion processes |
| US20090078913A1 (en) * | 2006-03-15 | 2009-03-26 | Rafael Luque | Carbonaceous materials |
| CN101941688A (en) * | 2009-07-10 | 2011-01-12 | 中国科学院大连化学物理研究所 | Method for preparing mesoporous carbon material |
| CN104118861A (en) * | 2014-07-14 | 2014-10-29 | 天津工业大学 | Preparation method of multilevel porous carbon with ultrahigh specific surface area |
| CN107359345A (en) * | 2017-08-01 | 2017-11-17 | 河南新太行电源股份有限公司 | A kind of preparation method and applications of cornstarch porous carbon@graphite |
-
2019
- 2019-09-09 CN CN201910846459.6A patent/CN110451479A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030171633A1 (en) * | 2002-02-28 | 2003-09-11 | Teng Xu | Molecular sieve compositions, catalyst thereof, their making and use in conversion processes |
| US20090078913A1 (en) * | 2006-03-15 | 2009-03-26 | Rafael Luque | Carbonaceous materials |
| CN101941688A (en) * | 2009-07-10 | 2011-01-12 | 中国科学院大连化学物理研究所 | Method for preparing mesoporous carbon material |
| CN104118861A (en) * | 2014-07-14 | 2014-10-29 | 天津工业大学 | Preparation method of multilevel porous carbon with ultrahigh specific surface area |
| CN107359345A (en) * | 2017-08-01 | 2017-11-17 | 河南新太行电源股份有限公司 | A kind of preparation method and applications of cornstarch porous carbon@graphite |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115974045A (en) * | 2022-12-06 | 2023-04-18 | 江西师范大学 | Method for preparing hard carbon by chemical gel synergistic basic metal oxide template method and application thereof |
| CN115974045B (en) * | 2022-12-06 | 2024-02-13 | 江西师范大学 | Method for preparing hard carbon by chemical gel synergistic alkaline metal oxide template method and application thereof |
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