CN108314001B - Preparation method of high and medium porosity carbon - Google Patents
Preparation method of high and medium porosity carbon Download PDFInfo
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- CN108314001B CN108314001B CN201810175286.5A CN201810175286A CN108314001B CN 108314001 B CN108314001 B CN 108314001B CN 201810175286 A CN201810175286 A CN 201810175286A CN 108314001 B CN108314001 B CN 108314001B
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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Abstract
The invention discloses a preparation method of carbon with high and medium porosity. The preparation method comprises the following steps: mixing a sulfuric acid solution and tetraethoxysilane, and stirring to obtain a solution A; according to the weight ratio of ethyl orthosilicate: adding sucrose into the solution A according to a mass ratio of sucrose = 1-4: 1, stirring to obtain a solution B, and sealing the solution B until gel is formed; drying the obtained gel, and then pre-oxidizing for 2-4 hours at 200-300 ℃; heating the product obtained after pre-oxidation to 600-900 ℃ at a speed of 5 ℃/min under an inert atmosphere, and keeping the temperature constant for 2-4 hours to obtain a carbon-silicon compound; and mixing the carbon-silicon compound with hydrofluoric acid, stirring, carrying out suction filtration, and drying to obtain the silicon-carbon composite. The invention has wide raw material source, environment protection and excellent product performance.
Description
Technical Field
The invention relates to the technical field of carbon material preparation, in particular to a preparation method of carbon with high and medium porosity.
Background
With the rapid development of the industry in China, more and more wastewater is discharged by the industry, and the wastewater is generally difficult to treat due to stable structure and long retention period. Wherein, the adsorption method is a main method for treating industrial wastewater due to the advantages of simple operation, good effect and the like; meanwhile, global warming is one of the serious problems facing the world. Therefore, the treatment of carbon dioxide, the main gas responsible for its greenhouse effect, is also very important and urgent. Wherein, the adsorption method has the advantages of cyclic utilization, low energy consumption and the like, and is effective CO2And (4) a separation treatment technology.
The porous carbon material is an excellent adsorbing material due to the characteristics of developed pore structure and high specific surface area, so that the porous carbon material has very good application in the aspects of sewage treatment and air purification, and the key influencing the performance of the porous carbon material is the size of the specific surface area, the structure and the shape of pores and the like.
At present, most of raw materials for preparing porous carbon are wood, coal and the like, which wastes resources and pollutes the environment, and the pore structure and the shape of the formed porous carbon are difficult to meet the requirements of specific occasions (such as sewage treatment, electrode material manufacturing and the like). Therefore, it is highly desirable to provide a method for preparing a porous carbon material with both social and economic benefits.
Disclosure of Invention
The invention aims to provide a preparation method of high and medium porosity carbon, which is eco-friendly, low in cost and excellent in performance.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of carbon with high and medium porosity is designed, and comprises the following steps:
(1) mixing a sulfuric acid solution and tetraethoxysilane according to the weight ratio of the sulfuric acid solution to tetraethoxysilane of 1-2 mL:1g, and stirring to obtain a solution A;
(2) according to the weight ratio of ethyl orthosilicate: adding sucrose into the solution A obtained in the step (1) according to a mass ratio of sucrose = 1-4: 1, stirring to obtain a solution B, and sealing the solution B until gel is formed;
(3) drying the gel obtained in the step (2), and then pre-oxidizing for 2-4 hours at 200-300 ℃;
(4) heating the product pre-oxidized in the step (4) to 600-900 ℃ at a speed of 5 ℃/min in an inert atmosphere, and keeping the constant temperature for 2-4 hours to obtain a carbon-silicon compound;
(5) and (4) mixing the carbon-silicon compound obtained in the step (4) with hydrofluoric acid, stirring, carrying out suction filtration, and drying to obtain the silicon-carbon composite.
Preferably, in the step (1), the pH value of the sulfuric acid solution is 2-4.
Preferably, in the step (1), the stirring is magnetic stirring, and the stirring time is 2-4 hours.
Preferably, in the step (3), the drying temperature is 100-110 ℃, and the drying time is 12-30 h.
Preferably, in the step (3), the pre-oxidation time is 3 h.
Preferably, in the step (4), the constant temperature time is 3 h.
Preferably, in the step (4), the inert gas is at least one selected from the group consisting of ammonia, nitrogen, hydrogen, and argon.
Preferably, in the step (5), the hydrofluoric acid is an excess hydrofluoric acid with a concentration of 40%.
Preferably, in the step (5), the drying time is 5 to 10 hours.
Compared with the prior art, the invention has the beneficial technical effects that:
1. the invention creatively adopts cane sugar (biological source) as the carbon source, has wide source and low price, and can avoid environmental pollution and resource waste caused by using wood and coal.
2. The high and medium porosity carbon prepared by the invention has high medium porosity and specific surface area.
3. The high and medium porosity carbon prepared by the invention has developed effective gaps, excellent spatial structure shape and excellent adsorption performance.
Drawings
FIG. 1 is an XRD pattern of high and medium porosity carbon materials prepared in examples 4-7;
FIG. 2 is a plot of the nitrogen adsorption-desorption isotherms of the high and medium porosity carbon materials prepared in examples 1-4;
FIG. 3 is a graph showing the pore size distribution of the high and medium porosity carbon materials prepared in examples 1 to 4;
FIG. 4 is a plot of the nitrogen adsorption-desorption isotherms of the high and medium porosity carbon materials prepared in examples 4-7;
FIG. 5 is a graph of pore size distribution for the high and medium porosity carbon materials prepared in examples 4-7;
FIG. 6 is a standard graph of a methylene blue solution.
Detailed Description
The following examples are intended to illustrate the present invention in detail and should not be construed as limiting the scope of the present invention in any way.
The instruments and devices referred to in the following examples are conventional instruments and devices unless otherwise specified; the materials and reagents involved, unless otherwise specified, were purchased from conventional chemical stores; the related testing and preparation methods are conventional methods unless otherwise specified.
EXAMPLE 1 preparation of high and Medium porosity carbon
Adding 6 mL of sulfuric acid with the pH value of 2 into a conical flask, then adding 4 g of Tetraethoxysilane (TEOS), then placing the conical flask filled with the sulfuric acid and the tetraethoxysilane on a magnetic stirrer, stirring for 3 hours to enable the solution to be uniform and transparent, then weighing 4 g of cane sugar, adding the cane sugar into the conical flask, continuing stirring to enable the cane sugar to be completely dissolved, then pouring the formed mixed solution into a test tube, and sealing to enable the mixed solution to be gelled.
After a uniform and transparent gel is formed, the test tube containing the gel is broken, the gel is taken out and put into a beaker for drying. The dried gel was pre-oxidized in a muffle furnace at 250 ℃ for 3 hours and then in N2And (3) under the atmosphere, heating to 900 ℃ at the speed of 5 ℃/min, keeping the temperature for 3 hours for carbonization, and then naturally cooling to obtain the carbon-silicon composite.
And (3) stirring the carbon-silicon composite by using excessive 40% hydrofluoric acid (HF) for 16 h, carrying out suction filtration, and then drying at 100 ℃ for 8 h to obtain the high-mesoporosity carbon material. And recording the high and medium porosity carbon as SAC-1-900, wherein 1 represents the mass ratio of ethyl orthosilicate to sucrose, and 900 represents the carbonization temperature.
EXAMPLE 2 preparation of high and Medium porosity carbon
The difference from example 1 is: the mass of tetraethoxysilane is 8 g, namely the mass ratio of tetraethoxysilane to sucrose is 2, and the rest is the same as that of the example 1. The resulting material was designated SAC-2-900.
EXAMPLE 3 preparation of high and Medium porosity carbon
The difference from example 1 is: the mass of tetraethoxysilane was 12 g, that is, the mass ratio of tetraethoxysilane to sucrose was 3, and the rest was the same as in example 1. The resulting material was designated SAC-3-900.
EXAMPLE 4 preparation of high and Medium porosity carbon
The difference from example 1 is: the mass of tetraethoxysilane was 16 g, that is, the mass ratio of tetraethoxysilane to sucrose was 4, and the rest was the same as in example 1. The resulting material was designated SAC-4-900.
EXAMPLE 5 preparation of high and Medium porosity carbon
The difference from example 3 is: the carbonization temperature was 800 ℃ and the rest was the same as in example 3. The resulting material was designated SAC-3-800.
EXAMPLE 6 preparation of high and Medium porosity carbon
The difference from example 3 is: the carbonization temperature was 700 ℃ and the rest was the same as in example 3. The resulting material was designated SAC-3-700.
Example 7 preparation of high and Medium porosity carbon
The difference from example 3 is: the carbonization temperature was 700 ℃ and the rest was the same as in example 3. The resulting material was designated SAC-3-600.
Example 8 carbonization yield of high and medium porosity carbon products prepared in examples 1-7
The carbonization yield of the products prepared in the examples 1 to 7 is shown in the following table 1, wherein the carbonization yield is the quality of the obtained high and medium porosity carbon/the quality of the sucrose after pre-oxidation.
Example 9 XRD testing of the high and mesoporous carbon materials prepared in examples 4-7 was performed
XRD testing of the carbon materials prepared in examples 5-7 was carried out using an X-ray diffractometer having an instrument model D8 ADVANCE manufactured by Bruker, Germany. The test condition is 35 kV of voltage, and the range of the scanning angle is 10-90 degrees.
FIG. 1 shows XRD test results of the carbon materials with high and medium porosity obtained in examples 5-7, and it can be seen from FIG. 1 that the microcrystalline structure of the carbon materials with high and medium porosity obtained in examples 5-7 is an amorphous carbon structure.
Example 10 specific surface area and pore size testing of the high and medium porosity carbons prepared in examples 1-7
The specific surface area and pore size were measured using a specific surface area pore size measuring instrument of 2QDS-MP-30 manufactured by Congta instruments, USA. 50 mg of the high and medium porosity carbon prepared in examples 2 to 9 were weighed and degassed at 250 ℃ for 12 hours under vacuum. The specific surface area of the material is calculated by using a Brunauer-Emmett-Teller (BET) method, the specific surface area and the volume of micropores are calculated by using a t-plot method, and the pore size distribution is analyzed by using a BJH theory.
The adsorption and desorption isotherms of the high and medium porosity carbon materials prepared in examples 1 to 4 are shown in figure 2, and the pore size distribution diagram is shown in figure 3; the adsorption and desorption isotherms of the high and medium porosity carbon materials prepared in examples 4 to 7 are shown in figure 4; the aperture profile is shown in figure 5.
As is apparent from FIGS. 3 and 5, the high and medium porosity carbon materials prepared in examples 1 to 7 have a predominant mesopore size, which is mainly distributed between 2.5 nm and 6 nm.
By N of figures 2 and 42The pore structure parameters of the sample calculated from the adsorption-desorption isotherm and the high and medium porosity carbon materials prepared in examples 1 to 7 are shown in table 2 below.
As can be seen from Table 2 above, the high and medium porosity carbon materials prepared in examples 1-7 have large specific surface areas and pore volumes.
EXAMPLE 11 adsorption Performance testing of the high and mesoporous carbon prepared in examples 1-7
Weighing 10 mg of methylene blue on an electronic balance, and placing the methylene blue in a 100 mL volumetric flask; then, distilled water was added to the scale to prepare a methylene blue solution having a concentration of 100 mg/L. The methylene blue solution with the concentration of 100 mg/L is respectively diluted into standard solutions with different concentrations, such as 1 mg/L, 2 mg/L, 3 mg/L, 4 mg/L, 5 mg/L, 6 mg/L and the like, and then the absorbance of the standard solutions is tested to prepare a methylene blue standard curve, as shown in figure 6.
Respectively weighing 10 mg of the high and medium porosity carbon materials prepared in examples 1 to 7, placing the carbon materials in a 50 mL conical flask, respectively adding 20 mL of methylene blue solution with the concentration of 50 mg/L, shaking the mixture at room temperature for 20 min, taking supernatant, placing the supernatant into a centrifuge for centrifugation, taking the supernatant after centrifugation, measuring the absorbance of the supernatant by using a spectrophotometer, and calculating the adsorption capacity, wherein the results are shown in the following table 3.
While the present invention has been described in detail with reference to the drawings and the embodiments, those skilled in the art will understand that various specific parameters in the above embodiments can be changed without departing from the spirit of the present invention, and a plurality of specific embodiments are formed, which are common variation ranges of the present invention, and will not be described in detail herein.
Claims (7)
1. A preparation method of carbon with high and medium porosity comprises the following steps:
(1) mixing and stirring a sulfuric acid solution with a pH value of 2-4 and tetraethoxysilane according to a weight ratio of 1-2 mL to 1g to obtain a solution A;
(2) according to the weight percentage of tetraethoxysilane: adding sucrose into the solution A according to the mass ratio of sucrose = 1-4: 1, mixing and stirring to obtain a solution B, and sealing the solution B until gel is formed;
(3) drying the gel obtained in the step (2), and then pre-oxidizing for 2-4 hours at 200-300 ℃;
(4) heating the pre-oxidized product to 600-900 ℃ at the speed of 5 ℃/min in an inert gas atmosphere, and keeping the constant temperature for 2-4 hours to obtain a carbon-silicon compound;
(5) and (4) adding excessive hydrofluoric acid with the weight percentage concentration of 40% into the carbon-silicon composite obtained in the step (4), mixing and stirring, performing suction filtration, and drying the solid residue to obtain the carbon-silicon composite.
2. The method for preparing carbon with high and medium porosity according to claim 1, wherein in the step (1), the stirring is magnetic stirring, and the stirring time is 2-4 h.
3. The method for preparing carbon with high and medium porosity according to claim 1, wherein in the step (3), the drying temperature is 100-110 ℃ and the drying time is 12-30 h.
4. The method for preparing carbon having a high and medium porosity according to claim 1, wherein in the step (3), the pre-oxidation time is 3 hours.
5. The method for preparing carbon with high and medium porosity according to claim 1, wherein the constant temperature time in the step (4) is 3 h.
6. The method for preparing carbon with high and medium porosity according to claim 1, wherein in the step (4), the inert gas is at least one of nitrogen and argon.
7. The method for preparing carbon with high and medium porosity according to claim 1, wherein in the step (5), the drying time is 5-10 h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899959A (en) * | 2006-07-19 | 2007-01-24 | 中国石油化工股份有限公司 | Method for preparing ordered mesoporous carbon |
| CN101362598A (en) * | 2008-08-27 | 2009-02-11 | 暨南大学 | Synthetic process of ordered mesoporous carbon material |
| CN102897748A (en) * | 2012-10-29 | 2013-01-30 | 中国石油大学(华东) | Method for preparing high-mesoporosity starch-based mesoporous carbon |
| CN103482596A (en) * | 2012-06-12 | 2014-01-01 | 北京化工大学 | Preparation method and application of ordered mesoporous carbon |
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| JP6202450B2 (en) * | 2013-11-29 | 2017-09-27 | 国立研究開発法人物質・材料研究機構 | NF or RO membrane made of hard carbon membrane, filtration filter, two-layer bonded filtration filter, and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899959A (en) * | 2006-07-19 | 2007-01-24 | 中国石油化工股份有限公司 | Method for preparing ordered mesoporous carbon |
| CN101362598A (en) * | 2008-08-27 | 2009-02-11 | 暨南大学 | Synthetic process of ordered mesoporous carbon material |
| CN103482596A (en) * | 2012-06-12 | 2014-01-01 | 北京化工大学 | Preparation method and application of ordered mesoporous carbon |
| CN102897748A (en) * | 2012-10-29 | 2013-01-30 | 中国石油大学(华东) | Method for preparing high-mesoporosity starch-based mesoporous carbon |
Non-Patent Citations (1)
| Title |
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| "模板法中孔炭材料的制备与表征";栾光贵 等;《炭素技术》;20061231;第25卷(第1期);第10-14页 * |
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