CN116062733A - Method for preparing ordered mesoporous carbon in one step - Google Patents
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 32
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 13
- 238000005530 etching Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 13
- 238000000967 suction filtration Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000005087 graphitization Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002808 molecular sieve Substances 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 238000003763 carbonization Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 230000020477 pH reduction Effects 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 238000003786 synthesis reaction Methods 0.000 abstract description 7
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- 238000000151 deposition Methods 0.000 abstract description 3
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- 239000002243 precursor Substances 0.000 description 7
- 239000003575 carbonaceous material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 3
- 229930006000 Sucrose Natural products 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000005720 sucrose Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 150000001345 alkine derivatives Chemical class 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
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- 239000010457 zeolite Substances 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
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- 239000003990 capacitor Substances 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
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- 101150017073 cmk1 gene Proteins 0.000 description 1
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- 239000012467 final product Substances 0.000 description 1
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- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910003480 inorganic solid Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910001463 metal phosphate Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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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Abstract
The invention provides a novel method for preparing ordered mesoporous carbon, which is used for realizing one-step synthesis of ordered mesoporous carbon. And directly depositing carbon by activating an Al ion active site and using proper temperature and introduced acetylene gas concentration, and etching the template to obtain the ordered mesoporous carbon. The synthesized ordered mesoporous carbon is formed by stacking two-dimensional hexagonal carbon rods. The invention can shorten the synthesis time, reduce the material consumption, reduce the cost, and has simple and easy operation and no pollution. The invention can be popularized to the preparation of other ordered mesoporous carbon.
Description
Technical Field
The invention belongs to the field of porous carbon materials, and particularly relates to a preparation method of ordered mesoporous carbon. The method is characterized in that: the method comprises the steps of activating an Al ion active site, introducing a carbon source and carbonizing in a reaction furnace in one step by using proper temperature and introduced acetylene gas concentration, and etching a template to obtain the ordered mesoporous carbon.
Background
According to the definition of the International Union of Pure and Applied Chemistry (IUPAC), porous materials can be classified simply by pore size: the porous material with the pore diameter smaller than 2nm is a Microporous material, and comprises zeolite (Zeolite), metal Organic Frameworks (MOFs) and the like; macropore (Macroporous) materials with the pore diameter larger than 50nm mainly represent aerogel, porous ceramics and the like; mesoporous (mesopore) materials with pore diameters between 2 and 50 nm. Compared with micropores, the mesoporous has larger pore diameter and is more suitable for the chemical reaction process participated by macromolecules; compared with macropores, mesopores have larger specific surface area and more active sites, and show unique nano-confinement effect. The carbon-based material has important importance in the field of materials, and the performance of the material can be greatly changed by introducing ordered mesopores into a carbon-based framework, so that the carbon-based material has important practical significance. Ordered mesoporous carbon is a new material with uniform pore diameter, highly ordered nano pore canal and high specific surface area. Although the development of mesoporous materials is extremely rapid, by 2005, the synthesized materials are almost inorganic solids including silica, metal oxides, phosphates and the like, but carbon-based materials most used in daily life are reported to be less, and huge defects exist, so that the preparation of ordered mesoporous carbon has great significance.
The method for preparing ordered mesoporous carbon mainly comprises two methods: soft template method, hard template method. In 2005, the group Zhao Dongyuan of the university of double denier (angel. Chem. Int. Ed.,2005,44,7053) was first to realize a breakthrough in the soft template method, which synthesized ordered mesoporous carbon using a pre-polymerized polymer-phenolic resin as a precursor. Later, researchers developed synthesis methods such as solvent evaporation induced self-assembly (EISA), aqueous phase wet method, hydrothermal method and mechanical grinding method, and developed a series of ordered mesoporous carbon with different pore structures, microcosmic morphologies and functions. However, the internal reaction, reaction mechanism and synthesis process of the method are very complex, and the method has the defects of difficult precursor selection, more reaction processes, difficult control of the reaction processes and the like.
Compared with a soft template method, the hard template method has no strict requirement on interaction between the template agent and the precursor, and has the advantages of less reaction process, simple mechanism, convenient and accurate control of the reaction process and the like. Researchers synthesized CMK-1 (j.Phys.chem.b. 1999,103,7743), CMK-2 (adv.mater., 2000,12,359), CMK-3 (j.am.chem.soc., 2000,122,10712), CMK-4 (j.phys.chem.b., 2002,106,1256), CMK-5 (nature, 2001,412,169) and the like successively with MCM-48 as a template and sucrose as a precursor, SBA-1 as a template and sucrose as a carbon precursor, SBA-15 as a template and sucrose as a precursor, MCM-48 as a template and acetylene as a precursor. However, in all the above methods, the precursor needs to be pre-acidified, carbonized, then carbon is deposited, and finally the template is etched to obtain the ordered mesoporous carbon. Therefore, the hard template method is long in time consumption, complicated in steps and low in yield. Therefore, it is important to simplify the preparation route.
Aiming at the defects of the prior art and the needs of research and application in the field, the invention provides a method for preparing ordered mesoporous carbon, which realizes one-step synthesis of ordered mesoporous carbon, and can shorten the synthesis time, reduce the materials, reduce the cost, and has the advantages of simplicity, easiness in operation and no pollution.
Disclosure of Invention
The invention provides a method for preparing ordered mesoporous carbon in one step. And directly depositing carbon by activating an Al ion active site and using proper temperature and introduced acetylene gas concentration, and etching the template to obtain the ordered mesoporous carbon. The method can shorten the synthesis time, reduce the cost, and is simple and easy to operate and pollution-free. The synthesized ordered mesoporous carbon has good application in the aspect of super capacitors.
According to the preparation method, an Al-MCM-41 molecular sieve is used as a template agent, acetylene is used as a carbon source, and OMCs are synthesized. The Al-MCM-41 sample was placed in a CVD horizontal furnace and the temperature was slowly raised to 400-500 ℃. Then introducing acetylene gas into the furnace, and preserving the temperature for 2-3 hours. Continuously raising the temperature to 800-900 ℃, and preserving the heat for 3-6 hours. And then using a mixed solution of HCl with the mass fraction of 1.5-2% and HF with the mass fraction of 2.5-3% to dissolve the Al-MCM-41 skeleton, thus obtaining the final product.
The method comprises the following specific steps:
step one: taking 80-100mg of Al-MCM-41 (Si/Al=25) template agent, putting into a CVD horizontal furnace, and introducing N 2 And (5) discharging air impurities after 10 min. Heating to 400-500 ℃ at the speed of 5-10 ℃/min, introducing acetylene gas with the volume fraction of 20-30% for 2-3h, continuously heating to 800-900 ℃ at the speed of 5-10 ℃/min after the reaction is finished, preserving heat for 3-6h to improve the graphitization degree, taking out after natural cooling, and introducing N in the whole process 2 。
Step two: 400-500ml of mixed solution of 1.5-2% HCl and 2.5-3% HF is prepared, the mixed solution is stirred and etched for 2 times at constant speed by a plastic bottle at normal temperature, each time for 2 hours, suction filtration is carried out after the etching is finished, distilled water is used for washing for a plurality of times in the suction filtration process, so as to ensure that the mixed solution is removed completely, and the mixed solution is dried in a vacuum box at 60-70 ℃ for 12 hours, so that the product is finally obtained.
The invention has the beneficial effects that: the invention can finish acidification, carbonization and carbon deposition in one step in the preparation process, has mild conditions and simple operation, avoids the defects of complicated steps and long synthesis time of the traditional method, and provides a simple method for preparing ordered mesoporous carbon. The method can be popularized to the preparation of other carbon materials. The ordered mesoporous carbon has wide application value in the fields of energy storage, catalysis and the like.
Drawings
The invention will be further described with reference to the drawings and examples.
FIG. 1 is an X-ray diffraction pattern of the ordered mesoporous carbon prepared in example 1;
FIG. 2 is a thermogravimetric diagram of the ordered mesoporous carbon prepared in example 1;
FIG. 3 is a scanning electron micrograph of the ordered mesoporous carbon prepared in example 1;
FIG. 4 is a transmission electron microscope image of the ordered mesoporous carbon prepared in example 1;
FIG. 5 is N of ordered mesoporous carbon prepared in example 1 2 Adsorption and desorption curves and pore size distribution diagrams;
FIG. 6 is a Raman diagram of the ordered mesoporous carbon prepared in example 1;
FIG. 7 is a dispersion spectrum of the ordered mesoporous carbon prepared in example 1;
Detailed Description
Example 1:
step one: taking Al-MCM-41 (Si/Al=25) molecular sieve as template agent, taking 80mg of the template agent, putting into a CVD horizontal furnace, and introducing N 2 And (5) discharging air impurities after 10 min. Heating to 500 ℃ at the speed of 10 ℃/min, introducing 30% acetylene gas with the volume fraction for heat preservation for 2h, continuously heating to 850 ℃ at the speed of 10 ℃/min after the reaction is finished, preserving heat for 3h to improve the graphitization degree, naturally cooling, taking out, and introducing N in the whole process 2 。
Step two: 400ml of mixed solution of 1.5% HCl and 2.5% HF is prepared, the mixed solution is stirred and etched for 2 times at constant speed by a plastic bottle at normal temperature, each time for 2 hours, suction filtration is carried out after the etching is finished, distilled water is used for washing for a plurality of times in the suction filtration process to ensure that the mixed solution is removed completely, and the mixed solution is dried in a vacuum box at 70 ℃ for 12 hours, so that a product is finally obtained.
Example 2:
step one: taking Al-MCM-41 (Si/Al=25) molecular sieve as template agent, taking 90mg of the template agent, putting into a CVD horizontal furnace, and introducing N 2 And (5) discharging air impurities after 10 min. Heating to 400 ℃ at a speed of 5 ℃/min, introducing 20% acetylene gas for 3h, continuously heating to 850 ℃ at a speed of 5 ℃/min after the reaction is finished, preserving heat for 4h to improve graphitization degree, naturally cooling, taking out, and introducing N in the whole process 2 。
Step two: preparing 500ml of mixed solution of 2% HCl and 3% HF by mass fraction, stirring and etching for 2 times at constant speed by using a plastic bottle at normal temperature for 2 hours each time, carrying out suction filtration after etching is finished, washing for a plurality of times by using distilled water in the suction filtration process to ensure that the mixed solution is removed completely, and drying in a vacuum box at 60 ℃ for 12 hours to finally obtain the product.
Example 3:
step one: taking 100mg of Al-MCM-41 (Si/Al=25) template agent, putting into a CVD horizontal furnace, and introducing N 2 And (5) discharging air impurities after 10 min. Heating to 420 ℃ at a speed of 5 ℃/min, introducing acetylene gas with a volume fraction of 20% for 3h, continuously heating to 900 ℃ at a speed of 5 ℃/min after the reaction is finished, preserving heat for 5h to improve the graphitization degree, naturally cooling, taking out, and introducing N in the whole process 2 。
Step two: 400ml of mixed solution of 1.5% HCl and 2.5% HF is prepared, the mixed solution is stirred and etched for 2 times at constant speed by a plastic bottle at normal temperature, each time for 2 hours, suction filtration is carried out after the etching is finished, distilled water is used for washing for a plurality of times in the suction filtration process to ensure that the mixed solution is removed completely, and the mixed solution is dried in a vacuum box at 70 ℃ for 12 hours, so that a product is finally obtained.
Example 4:
step one: 80mg of Al-MCM-41 (Si/Al=25) template agent is taken and put into a CVD horizontal furnace, and N is introduced 2 And (5) discharging air impurities after 10 min. Heating to 440 ℃ at the speed of 10 ℃/min, and introducing 30% of ethylene by volumeThe alkyne gas is heated to 800 ℃ at the speed of 10 ℃/min after the reaction is finished for 3 hours, the temperature is kept for 6 hours to improve the graphitization degree, the alkyne gas is taken out after natural cooling, and N is introduced in the whole process 2 。
Step two: preparing 500ml of mixed solution of 2% HCl and 3% HF by mass fraction, stirring and etching for 2 times at constant speed by using a plastic bottle at normal temperature for 2 hours each time, carrying out suction filtration after etching is finished, washing for a plurality of times by using distilled water in the suction filtration process to ensure that the mixed solution is removed completely, and drying in a vacuum box at 70 ℃ for 12 hours to finally obtain the product.
The foregoing description is only of the preferred embodiments of the invention. And are not intended to limit the invention in any way; those skilled in the art can readily practice the present invention as illustrated in the drawings and described above; however, those skilled in the art will appreciate that many modifications, adaptations, and variations of the present invention are possible in light of the above teachings without departing from the scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the implementation techniques of the present invention are all within the scope of the present invention.
Claims (4)
1. A preparation method for synthesizing ordered mesoporous carbon in one step is realized by controlling conditions. The preparation method is characterized in that the preparation process can be completed by one step of acidification, carbonization and carbon deposition.
The preparation method of the ordered mesoporous carbon is characterized by comprising the following specific steps of:
step one: the Al-MCM-41 molecular sieve is used as a template agent, acetylene is used as a carbon source, and OMCs are synthesized. Taking 80-100mg of template agent, placing into a CVD horizontal furnace, introducing N 2 And (5) discharging air impurities after 10 min. Heating to a certain interval range at a speed of 5-10deg.C/min, introducing acetylene gas for 2-3 hr, continuously heating to 800-900deg.C at a speed of 5-10deg.C/min after the reaction is completed, maintaining the temperature for 3-6 hr to improve graphitization degree, naturally cooling, taking out, and introducing N in the whole process 2 。
Step two: 400-500ml of mixed solution of 1.5-2% HCl and 2.5-3% HF is prepared, the mixed solution is stirred and etched for 2 times at constant speed by a plastic bottle at normal temperature, each time for 2 hours, suction filtration is carried out after the etching is finished, distilled water is used for washing for a plurality of times in the suction filtration process, so as to ensure that the mixed solution is removed cleanly, and the mixed solution is dried in a vacuum box at 60-70 ℃ for 12 hours, so that the product is finally obtained.
2. The method according to claim 1, wherein the Al-MCM-41 molecular sieve in the first step has a silica-alumina ratio of 25.
3. The method according to claim 1, wherein the reaction temperature after the temperature rise in the first step is 400 to 500 ℃.
4. The method according to claim 1, wherein the acetylene gas is present in the amount of 20 to 30% by volume in the first step.
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2023
- 2023-03-08 CN CN202310215739.3A patent/CN116062733A/en active Pending
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