CN115838166A - Preparation method of nano onion carbon - Google Patents
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- CN115838166A CN115838166A CN202211376260.XA CN202211376260A CN115838166A CN 115838166 A CN115838166 A CN 115838166A CN 202211376260 A CN202211376260 A CN 202211376260A CN 115838166 A CN115838166 A CN 115838166A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 56
- 241000234282 Allium Species 0.000 title claims abstract description 50
- 235000002732 Allium cepa var. cepa Nutrition 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229920002678 cellulose Polymers 0.000 claims abstract description 91
- 239000001913 cellulose Substances 0.000 claims abstract description 91
- 230000008929 regeneration Effects 0.000 claims abstract description 28
- 238000011069 regeneration method Methods 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 23
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 21
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000004202 carbamide Substances 0.000 claims description 9
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims description 7
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- VEPTXBCIDSFGBF-UHFFFAOYSA-M tetrabutylazanium;fluoride;trihydrate Chemical compound O.O.O.[F-].CCCC[N+](CCCC)(CCCC)CCCC VEPTXBCIDSFGBF-UHFFFAOYSA-M 0.000 claims description 4
- 239000012296 anti-solvent Substances 0.000 claims description 3
- PBIDWHVVZCGMAR-UHFFFAOYSA-N 1-methyl-3-prop-2-enyl-2h-imidazole Chemical compound CN1CN(CC=C)C=C1 PBIDWHVVZCGMAR-UHFFFAOYSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229920000875 Dissolving pulp Polymers 0.000 claims 1
- 230000006798 recombination Effects 0.000 abstract description 2
- 238000005215 recombination Methods 0.000 abstract description 2
- 230000001172 regenerating effect Effects 0.000 abstract description 2
- 239000004627 regenerated cellulose Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000002077 nanosphere Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 5
- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- FPGGTKZVZWFYPV-UHFFFAOYSA-M tetrabutylammonium fluoride Chemical compound [F-].CCCC[N+](CCCC)(CCCC)CCCC FPGGTKZVZWFYPV-UHFFFAOYSA-M 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000007233 catalytic pyrolysis Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229940075579 propyl gallate Drugs 0.000 description 2
- 235000010388 propyl gallate Nutrition 0.000 description 2
- 239000000473 propyl gallate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of nano onion carbon, which comprises the following steps: under the condition of cellulose regeneration temperature, adding a regeneration solvent into the cellulose solution, uniformly mixing, and obtaining a suspension after cellulose regeneration; and then washing the suspension by using a regenerated solvent, reserving regenerated cellulose, and finally drying to obtain the nano onion carbon. The invention takes the most abundant renewable resource cellulose on the earth as a carbon source, regulates and controls the recombination behavior of cellulose molecules in the process of regenerating cellulose solution into cellulose, and successfully prepares nano onion carbon with the diameter of 10 nm-100 nm, which can be called cellulose nano onion. The preparation method is extremely simple, and the nano onion carbon can be prepared at normal temperature by only adding a proper amount of regenerated solvent into the cellulose solution and uniformly mixing.
Description
Technical Field
The invention belongs to the technical field of carbon materials, and particularly relates to a preparation method of nano onion carbon.
Background
The nano onion carbon is an onion-shaped nanosphere material formed by nesting a plurality of concentric spherical carbon-containing material shells, and has a special onion-shaped spherical microstructure and excellent physicochemical properties, so that the nano onion carbon is widely researched in the fields of energy storage, photoelectricity, biomedicine, catalysis, lubrication and the like, and is considered to be a novel carbon material with great potential after carbon nanotubes and graphene.
The basic principle of nano onion carbon preparation can be summarized as the assembly of carbon-containing basic units into onion-shaped nanospheres through a special process. The existing preparation method of the nano onion carbon mainly comprises the methods of arc discharge, ion implantation, vapor deposition, heat treatment and electron beam irradiation. For example, the publication No. CN 114381324B discloses a method for preparing a functionalized onion carbon material nano additive, which specifically discloses: collecting candle ash at the flame position in the candle flame, and carrying out heat treatment on the candle ash at the temperature of 300-1100 ℃ for 6-24 h to obtain nano onion carbon; publication No. CN 111634904A discloses a method for preparing carbon nano-onions by lignin blending catalytic pyrolysis, and specifically discloses: mixing lignin containing transition metal with a blending agent at 700-900 ℃ for catalytic pyrolysis to obtain nano onion carbon; publication No. CN 114348993A discloses a graphene array surface in-situ growth carbon nano onion, a preparation method and application thereof, and specifically discloses: spin-coating a catalyst solution containing metal on the surface of graphene, drying at 40-80 ℃, calcining at 250-400 ℃, introducing inert gas, heating to 650-950 ℃, and growing nano onion carbon on the surface of the graphene array in situ by chemical vapor deposition. The disclosed method for synthesizing nano onion carbon generally requires higher energy and complex processes, such as higher current, higher temperature and the like, which results in high production cost, and has certain dangerousness, which severely limits the research and utilization of nano onion carbon, a material with great potential.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing nano onion carbon, aiming at the defects of the prior art, the method takes cellulose which is the most abundant renewable resource on the earth as a carbon source, regulates and controls the recombination behavior of cellulose molecules in the process of regenerating cellulose solution into cellulose, and successfully prepares nano onion carbon with the diameter of 10 nm-100 nm, which can be called cellulose nano onion. The preparation method is extremely simple, and the nano onion carbon can be prepared at normal temperature only by adding a proper amount of regeneration solvent into the cellulose solution.
The technical scheme of the invention is as follows: a preparation method of nano onion carbon is characterized by comprising the following steps: the preparation method comprises the following steps: under the condition of cellulose regeneration temperature, adding a regeneration solvent into the cellulose solution and uniformly mixing, and obtaining a suspension after cellulose regeneration; and then washing the suspension with a regenerated solvent until the solvent for dissolving the cellulose is completely removed, and drying to obtain the nano onion carbon.
In the preparation method of the present invention, the cellulose can be partially or completely regenerated, and the nano onion carbon can be obtained after washing and drying. When the cellulose is partially regenerated, the cellulose can be continuously regenerated after being washed by the regeneration solvent.
Preferably, the regeneration solvent is an anti-solvent that is insoluble but soluble in the cellulose solvent, e.g. the regeneration solvent may be deionized water or ethanol, but other anti-solvents capable of being insoluble but soluble in the cellulose solvent are not excluded.
Preferably, the cellulose regeneration temperature is-10 ℃ to 100 ℃.
Preferably, the cellulose solution is tetrabutylammonium fluoride trihydrate/dimethyl sulfoxide cellulose solution (TBAF 3H) 2 O/DMSO cellulose solution), 1-allyl-3-methylimidazole cellulose chloride solution (AmimCl cellulose solution), znCl 2 Cellulose solutions, N-methylmorpholine-N-oxide cellulose solutions (NMMO cellulose solutions), naOH/urea cellulose solutions or NaOH/thiourea/urea cellulose solutions and other cellulose solutions.
Preferably, the temperature of drying does not exceed 200 ℃.
Compared with the prior art, the invention has the following effects:
1. the invention overcomes the problems of generally higher energy and complex process in the existing synthesis of nano onion carbon, and provides a brand new synthesis method for preparing the nano onion carbon, and the preparation process is simple and low in cost.
2. The traditional raw materials for preparing the nano onion carbon are mostly selected from diamond, graphite, carbon-containing gas and other carbon-containing materials, but the invention firstly takes cellulose as a carbon source, adds a regeneration solvent into a cellulose solution, regulates and controls the cellulose regeneration process, and leads cellulose molecules to recombine to prepare the nano onion carbon. Cellulose is a recyclable carbon source, is considered as the most abundant renewable resource on the earth, has the excellent properties of being renewable, widely distributed, low in price and the like, is an environment-friendly and economic raw material, and is more beneficial to reducing the production cost.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
Fig. 1 is a TEM photograph and a corresponding element scanning mapping photograph of nano onion carbon prepared in example 1 of the present invention.
Fig. 2 is a TEM photograph of nano onion carbon prepared in example 2 of the present invention.
Fig. 3 is a TEM photograph of nano onion carbon prepared in example 3 of the present invention.
Fig. 4 is a TEM photograph of nano onion carbon prepared in example 4 of the present invention.
Fig. 5 is a TEM photograph of nano onion carbon prepared in example 5 of the present invention.
Detailed Description
Example 1
The preparation method of the nano onion carbon comprises the following steps:
1wt% of cellulose was dispersed in 60mL of DMSO and 6.6g of TBAF.3H 2 Mechanically stirring the O mixed solution at room temperature (25 ℃) at the rotating speed of 1000rpm/min for 15min, and then stirring the O mixed solution at 60 ℃ for 1H until cellulose is completely dissolved to obtain TBAF & 3H 2 O/DMSO cellulose solution. Then, at a regeneration temperature of 60 ℃, dropwise adding deionized water serving as a regeneration solvent into the cellulose solution at a speed of 1mL/min, wherein the adding mass of the deionized water is 3 times of that of the cellulose solution, and stirring at a speed of 500rpm/min to uniformly mix the cellulose solution and the deionized water until the cellulose is completely regenerated to obtain a suspension. Washing the suspension with deionized water until TBAF and DMSO are completely removed, drying at 60 deg.C to obtain product, testing the product with TEM, and preparing the product shown in FIG. 1The onion-shaped nanospheres are formed by arranging a circle of carbon layers together, have the particle size of about 35nm and are of a typical nano onion carbon structure.
Example 2
The preparation method of the nano onion carbon comprises the following steps:
1wt% cellulose was dispersed in AmimCl and mechanically stirred at 100 ℃ for 1h at 1000rpm/min until the cellulose was completely dissolved to give a cellulose solution of AmimCl. And then, dropwise adding a regeneration solvent deionized water into the cellulose solution at the regeneration temperature of 100 ℃ at the speed of 10mL/min, wherein the adding mass of the deionized water is 2 times of the mass of the cellulose solution, and stirring at 300rpm/min simultaneously to uniformly mix the cellulose solution and the deionized water until the cellulose is completely regenerated to obtain a suspension. The suspension is washed by deionized water until AmimCl is completely removed, and after drying at 25 ℃ and room temperature, a product is obtained, the product is tested by a TEM (transmission electron microscope) test, and as shown in figure 2, the prepared product is arranged by a circle of carbon layers to form onion-shaped nanospheres, the particle size of which is about 42nm, and the onion-shaped nanospheres are of a typical nano onion carbon structure.
Example 3
The preparation method of the nano onion carbon comprises the following steps:
2% by weight of cellulose were dispersed in ZnCl at a concentration of 71.6% 2 Mechanically stirring the solution at 80 ℃ for 1h at 1000rpm/min until the cellulose is completely dissolved to obtain ZnCl 2 A cellulose solution. Then adding a regeneration solvent ethanol into the cellulose solution at a speed of 100mL/min at a regeneration temperature of 25 ℃ and room temperature, wherein the addition mass of the ethanol is 5 times of the mass of the cellulose solution, and stirring at 100rpm/min simultaneously to uniformly mix the cellulose solution and the ethanol until the cellulose is completely regenerated to obtain a suspension. The suspension is washed with ethanol until complete removal of ZnCl 2 Drying at 60 deg.C to obtain product, and testing with TEM, as shown in FIG. 3, to obtain Bulbus Allii Cepae nanospheres with particle size of about 52nm and typical nanometer carbon structure.
Example 4
The preparation method of the nano onion carbon comprises the following steps:
1% by weight of propyl gallate was added to 50% aqueous NMMO solution, and the solution was distilled under reduced pressure at 120 ℃ with an oil bath until the water content was 13%. Subsequently, 1wt% cellulose was dispersed in the NMMO solution and stirred at 100 ℃ at 1000rpm/min for 2h until the cellulose was completely dissolved to give a NMMO cellulose solution. Then, at the regeneration temperature of 100 ℃, dropwise adding deionized water serving as a regeneration solvent into the cellulose solution at the speed of 10mL/min, wherein the adding mass of the deionized water is 4 times of the mass of the cellulose solution, and stirring at 300rpm/min to uniformly mix the cellulose solution and the deionized water until the cellulose is completely regenerated to obtain a suspension. The suspension is washed by deionized water until NMMO and propyl gallate are completely removed, and after drying at 60 ℃, a product is obtained, the product is tested by TEM, as shown in figure 4, and the prepared product is arranged by a circle of carbon layers to form onion-shaped nanospheres with the particle size of about 38nm, which are typical nano onion carbon structures.
Example 5
The preparation method of the nano onion carbon comprises the following steps:
pre-cooling NaOH/12wt% urea solution as calculated by 7wt% to-10 deg.C, then dispersing 2wt% cellulose into the solution, and mechanically stirring at-10 deg.C at 2000rpm/min for 30min until the cellulose is completely dissolved to obtain NaOH/urea cellulose solution. And then, at a regeneration temperature of-10 ℃, pouring deionized water serving as a regeneration solvent into the cellulose solution and uniformly mixing, wherein the mass of the deionized water is 5 times of that of the cellulose solution until the cellulose is regenerated, so as to obtain a suspension. The suspension is washed by deionized water until NaOH and urea are completely removed, and after drying at 120 ℃, a product is obtained, the product is tested by a TEM (transmission electron microscope), and as shown in figure 5, the prepared product is arranged by a circle of carbon layers to form onion-shaped nanospheres, the particle size of the onion-shaped nanospheres is about 55nm, and the onion-shaped nanospheres are of a typical nano onion carbon structure.
In this embodiment, the NaOH/thiourea/urea cellulose solution can be used to replace the NaOH/urea cellulose solution, and the nano onion carbon can still be prepared.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (4)
1. A preparation method of nano onion carbon is characterized by comprising the following steps: the preparation method comprises the following steps:
under the condition of cellulose regeneration temperature, adding a regeneration solvent into the cellulose solution, uniformly mixing, and obtaining a suspension after cellulose regeneration; and then washing the suspension with a regenerated solvent until the solvent for dissolving cellulose is completely removed, and drying to obtain the nano onion carbon.
2. The method for preparing nano onion carbon according to claim 1, wherein the method comprises the following steps: the regeneration solvent is an anti-solvent that is insoluble in cellulose but soluble in the cellulose solvent.
3. The method for preparing nano onion carbon according to claim 1, wherein the method comprises the following steps: the regeneration temperature of the cellulose is-10 ℃ to 100 ℃.
4. The method for preparing nano onion carbon according to claim 1, wherein the method comprises the following steps: the cellulose solution is tetrabutylammonium fluoride trihydrate/dimethyl sulfoxide cellulose solution, 1-allyl-3-methylimidazole chloride cellulose solution, znCl 2 Cellulose solution, N-methylmorpholine-N-oxide cellulose solution, naOH/urea cellulose solution or NaOH/thiourea/urea cellulose solution and other cellulose solutions.
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- 2022-11-04 CN CN202211376260.XA patent/CN115838166A/en active Pending
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US20100133481A1 (en) * | 2006-02-09 | 2010-06-03 | Headwaters Technology Innovation, Llc | Polymeric materials incorporating carbon nanostructures and methods of making same |
CN103935978A (en) * | 2014-03-28 | 2014-07-23 | 新乡学院 | Nano carbon material prepared by pyrolysis of wheat straw and preparation method thereof |
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