CN115321525B - Preparation method of graphene nano-network with macroporous structure - Google Patents
Preparation method of graphene nano-network with macroporous structure Download PDFInfo
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- CN115321525B CN115321525B CN202210996426.1A CN202210996426A CN115321525B CN 115321525 B CN115321525 B CN 115321525B CN 202210996426 A CN202210996426 A CN 202210996426A CN 115321525 B CN115321525 B CN 115321525B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 28
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 20
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 18
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 13
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000001103 potassium chloride Substances 0.000 claims abstract description 9
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 239000001509 sodium citrate Substances 0.000 claims abstract description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 5
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229940039790 sodium oxalate Drugs 0.000 claims abstract description 4
- 238000010000 carbonizing Methods 0.000 claims abstract description 3
- PXEDJBXQKAGXNJ-QTNFYWBSSA-L disodium L-glutamate Chemical compound [Na+].[Na+].[O-]C(=O)[C@@H](N)CCC([O-])=O PXEDJBXQKAGXNJ-QTNFYWBSSA-L 0.000 claims abstract description 3
- 235000013923 monosodium glutamate Nutrition 0.000 claims abstract description 3
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 claims abstract description 3
- 239000001508 potassium citrate Substances 0.000 claims abstract description 3
- 229960002635 potassium citrate Drugs 0.000 claims abstract description 3
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims abstract description 3
- 235000011082 potassium citrates Nutrition 0.000 claims abstract description 3
- 239000001472 potassium tartrate Substances 0.000 claims abstract description 3
- 229940111695 potassium tartrate Drugs 0.000 claims abstract description 3
- 235000011005 potassium tartrates Nutrition 0.000 claims abstract description 3
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 claims abstract description 3
- 229960001790 sodium citrate Drugs 0.000 claims abstract description 3
- 229940073490 sodium glutamate Drugs 0.000 claims abstract description 3
- 239000001433 sodium tartrate Substances 0.000 claims abstract description 3
- 229960002167 sodium tartrate Drugs 0.000 claims abstract description 3
- 235000011004 sodium tartrates Nutrition 0.000 claims abstract description 3
- 238000003763 carbonization Methods 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000013067 intermediate product Substances 0.000 claims description 4
- 239000002135 nanosheet Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 2
- 230000001939 inductive effect Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 7
- 239000011148 porous material Substances 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 12
- 229910021392 nanocarbon Inorganic materials 0.000 description 10
- 239000003575 carbonaceous material Substances 0.000 description 7
- 229910017053 inorganic salt Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- -1 salt ions Chemical class 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
Abstract
The invention discloses a preparation method of a graphene nano-network with a macroporous structure, which comprises the steps of uniformly mixing an alkali metal organic salt and an inorganic molten salt at room temperature, wherein the alkali metal organic salt is at least one of sodium citrate, sodium oxalate, sodium glutamate, sodium tartrate, potassium citrate or potassium tartrate, the inorganic molten salt is a mixture of potassium chloride and lithium chloride, heating the mixture to 600-900 ℃ at a heating rate of 5-10 ℃/min under an inert atmosphere, preserving heat for 2-6h, carbonizing the mixture, cooling to room temperature, washing and drying to obtain the graphene nano-network with the macroporous structure. The method is environment-friendly, simple to operate, low in cost and convenient for large-scale production, and the prepared graphene nano-net has the characteristics of rich pore channels, large specific surface area, high chemical activity and the like, and has huge application potential in the related fields of gas adsorption and separation, electrochemical energy conversion and storage and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of porous carbon materials, and particularly relates to a preparation method of a graphene nano-network with a macroporous structure.
Background
The nano carbon material is widely applied and researched due to the characteristics of abundant structural forms, excellent physical and chemical properties, low material cost and the like. The porous nano carbon material also has the characteristics of high specific surface area, high conductivity, high stability, low density and the like, and has a huge application prospect in the fields of fuel cells, super capacitors, secondary batteries, solar cells, biosensors, gas adsorption and separation and the like. Currently, the most commonly used means for preparing porous nanocarbons are the template method and the chemical activation method. The template method is to prepare the porous nano carbon by adopting inert substances such as molecular sieve, silicon oxide, sodium chloride and the like as pore-forming agents. However, these methods not only add to the cost, but also result in the active site of the product being deleted due to the chemical inertness of the template; the template is removed by using reagents such as hydrofluoric acid with high toxicity and high corrosiveness, the operation is complex, and the yield is relatively low; and the pore canal structure of the product is easy to be damaged when the template is removed. The chemical activation method is to obtain a porous structure by activating and treating a carbon material with a strong acid or a strong alkali. However, the method has the defects of serious carbon mass loss, low yield, difficult control of the pore channel structure of the product and the like.
Recently, an inorganic molten salt growth method has attracted attention for porous nanocarbon materials. Inorganic fused salts (e.g. ZnCl) 2 LiCl, naCl, mixtures thereof, etc.) and biomass, polymerizable organic molecules or ionic liquids, etc., through high-temperature carbonization, desalting (salt can be recycled) and cleaning, the porous nanocarbon material can be obtained. In the high-temperature carbonization process, the molten inorganic salt not only serves as a solvent, but also serves as a pore-forming agent for free salt ions and clusters thereof, so that the prepared porous nano carbon material generally has a microporous or mesoporous structure. LiCl/KCl mixed molten salt medium is reported to dissolve intermediate products of carbonization process of saccharide molecules such as glucose, and two-dimensional graphene is induced to be formed (Small, 2014, 10:193-200). In addition, the MOF material Zn-ZIF-L is added into the LiCl/KCl mixed molten salt medium to form a graphene nano-network (Angew. Chem. Int. Ed.,2019, 58:13354-13359) with rich defects and a grid size smaller than 5 nm. However, these inorganic molten salt methods are widely used for preparing porous nanocarbon materials that lack large pore channels (i.e.>50 nm), which is unfavorable for the increase of active sites and the transmission of related substances, and limits the wider application of the nano carbon material to a certain extent.
Disclosure of Invention
Aiming at the problem that macroporous pore canals of a porous nano carbon material are difficult to construct by using an inorganic molten salt method in the prior art, the invention provides a preparation method of a graphene nano net with a macroporous structure.
The invention adopts the following technical scheme to solve the technical problems, and is characterized by comprising the following specific steps: uniformly mixing an alkali metal organic salt and an inorganic molten salt at room temperature, wherein the alkali metal organic salt is at least one of sodium citrate, sodium oxalate, sodium glutamate, sodium tartrate, potassium citrate or potassium tartrate, the inorganic molten salt is a mixture of potassium chloride and lithium chloride, heating the mixture to 600-900 ℃ at a heating rate of 5-10 ℃/min under inert atmosphere, preserving heat for 2-6 hours for carbonization treatment, taking the alkali metal organic salt as a carbon source in the carbonization process, decomposing a macroporous template in situ, dissolving a carbonized intermediate product in an inorganic molten salt medium, inducing to form a two-dimensional nano sheet, cooling to room temperature, washing and drying to obtain the graphene nano net with the macroporous structure.
Further defined, the potassium chloride and the lithium chloride in the inorganic molten salt are ground and uniformly mixed in a molar ratio of 1:1-1:4.
Further limited, the mass ratio of the alkali metal organic salt to the inorganic molten salt is 1:3-1:5, and the alkali metal organic salt and the inorganic molten salt are uniformly mixed in a grinding or ball milling mixing mode.
Further defined, the inert atmosphere is a nitrogen atmosphere or an argon atmosphere.
Further limited, deionized water, dilute hydrochloric acid and absolute ethyl alcohol are repeatedly washed in the washing and drying process, and the drying temperature is 60-105 ℃.
Compared with the prior art, the invention takes the alkali metal organic salt as a carbon source in the inorganic molten salt medium, and the macroporous template is decomposed in situ while the inorganic molten salt medium is carbonized, the inorganic molten salt medium dissolves the carbonized intermediate product and induces the formation of the two-dimensional nano-sheets, and finally the formation of the graphene nano-network with the macroporous structure is realized. The invention has the following advantages: 1. the process is simple and convenient to operate. The graphene nano-network with the macroporous structure can be directly obtained by carbonizing the mixture of the inorganic molten salt and the alkali metal organic salt in one step. 2. No pollution and environmental protection. The invention uses an inorganic fused salt medium which is green and environment-friendly, has low vapor pressure and wide operating temperature range, and is a green technology. 3. The graphene nano-network prepared by the method has macroporous grids larger than 50nm, micro/mesoporous channels, large specific surface area and more active sites, is favorable for the transmission of reactants/products, can further expand the application field of graphene, and has huge application potential in the related fields of gas adsorption and separation, electrochemical energy conversion and storage and the like.
Drawings
Fig. 1 is a TEM image of graphene nanonets with a macroporous structure prepared in example 1.
Detailed Description
The above-described matters of the present invention will be described in further detail by way of examples, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples, and all techniques realized based on the above-described matters of the present invention are within the scope of the present invention.
Example 1
Grinding and mixing potassium chloride and lithium chloride uniformly in a molar ratio of 1:1.45; weighing 4g of the mixed inorganic salt, adding 1g of sodium citrate, and fully grinding by using a mortar; then placing the quartz tube into a tube furnace, introducing nitrogen for 2 hours, replacing oxygen in the quartz tube, heating to 700 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2 hours at 700 ℃ for carbonization treatment; cooling to room temperature along with the furnace, repeatedly cleaning with deionized water, dilute hydrochloric acid and absolute ethyl alcohol, and finally drying in a drying oven at 80 ℃ to obtain the graphene nano-net with the macroporous structure.
Fig. 1 is a TEM image of a graphene nanonet with a macroporous structure prepared, and it can be seen from the figure that the prepared sample has a two-dimensional network structure with a mesh size range of 11-143nm.
Example 2
The procedure was essentially the same as in example 1, except that sodium citrate was replaced with sodium oxalate, and the morphology and structure of the graphene material produced was similar to example 1.
Example 3
The procedure is substantially the same as in example 1, except that the molar ratio of potassium chloride to lithium chloride in the mixed inorganic salt is 1:3, and the morphology and structure of the prepared graphene material are the same as in example 1.
Example 4
The procedure was essentially the same as in example 1, except that the mass of the mixed inorganic salt was increased to 4.5g, and the morphology and structure of the resulting graphene material were the same as in example 1.
Example 5
The procedure was essentially the same as in example 1, except that the nitrogen atmosphere was changed to an argon atmosphere, and the morphology and structure of the resulting graphene material were the same as in example 1.
Example 6
The procedure was essentially the same as in example 1, except that the carbonization treatment was carried out at a soak temperature of 900 ℃, and the morphology and structure of the resulting graphene material were similar to example 1.
Example 7
The procedure is substantially the same as in example 1, except that the carbonization treatment is carried out for a holding time of 6h, and the morphology and structure of the prepared graphene material are the same as those of example 1.
Example 8
The procedure was essentially the same as in example 3, except that the carbonization treatment was carried out at a soak temperature of 900 ℃, and the morphology and structure of the resulting graphene material were similar to example 1.
While the basic principles, principal features and advantages of the present invention have been described in the foregoing examples, it will be appreciated by those skilled in the art that the present invention is not limited by the foregoing examples, but is merely illustrative of the principles of the invention, and various changes and modifications can be made without departing from the scope of the invention, which is defined by the appended claims.
Claims (3)
1. The preparation method of the graphene nano-network with the macroporous structure is characterized by comprising the following specific steps: uniformly mixing an alkali metal organic salt and an inorganic molten salt at room temperature, wherein the alkali metal organic salt is at least one of sodium citrate, sodium oxalate, sodium glutamate, sodium tartrate, potassium citrate or potassium tartrate, the inorganic molten salt is a mixture of potassium chloride and lithium chloride, the mixture is heated to 600-900 ℃ at a heating rate of 5-10 ℃/min under inert atmosphere and is subjected to carbonization treatment for 2-6 hours, the alkali metal organic salt is used as a carbon source in the carbonization process and is in-situ decomposed into a macroporous template, the inorganic molten salt medium is used for dissolving and carbonizing an intermediate product and inducing to form a two-dimensional nano sheet, then the two-dimensional nano sheet is cooled to room temperature, the graphene nano net with a macroporous structure is obtained after washing and drying, the potassium chloride and the lithium chloride in the inorganic molten salt are uniformly mixed in a molar ratio of 1:1-1:4, the alkali metal organic salt and the inorganic molten salt are uniformly mixed in a grinding or ball-milling mixing mode.
2. The method for preparing the graphene nanonet with the macroporous structure according to claim 1, wherein the method comprises the following steps: the inert atmosphere is nitrogen atmosphere or argon atmosphere.
3. The method for preparing the graphene nanonet with the macroporous structure according to claim 1, wherein the method comprises the following steps: in the washing and drying process, deionized water, dilute hydrochloric acid and absolute ethyl alcohol are used for repeated washing, and the drying temperature is 60-105 ℃.
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| CN103601177A (en) * | 2013-11-19 | 2014-02-26 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene from solid organic acid by using alkali metal salt as catalyst |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210234167A1 (en) * | 2020-01-27 | 2021-07-29 | Global Graphene Group, Inc. | Porous graphene/carbon composite balls for an alkali metal battery anode |
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