CN115321525A - Preparation method of graphene nano-net with macroporous structure - Google Patents
Preparation method of graphene nano-net with macroporous structure Download PDFInfo
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- CN115321525A CN115321525A CN202210996426.1A CN202210996426A CN115321525A CN 115321525 A CN115321525 A CN 115321525A CN 202210996426 A CN202210996426 A CN 202210996426A CN 115321525 A CN115321525 A CN 115321525A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 26
- 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
- 238000003763 carbonization Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 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 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000002106 nanomesh Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 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
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 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
- 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
- 239000013067 intermediate product Substances 0.000 claims description 5
- 229910052799 carbon Inorganic materials 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
- 239000002135 nanosheet Substances 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
- 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 4
- 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 11
- 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
- 238000003917 TEM image Methods 0.000 description 3
- 238000004321 preservation Methods 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
- 230000004913 activation Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012217 deletion Methods 0.000 description 1
- 230000037430 deletion Effects 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
- 239000004088 foaming agent Substances 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
- 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
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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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
Abstract
The invention discloses a preparation method of a graphene nano-net with a macroporous structure, which comprises the steps of uniformly mixing alkali metal organic salt and 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 for carbonization, cooling to room temperature, washing and drying to obtain the graphene nano-net with the macroporous structure. The method is green and environment-friendly, simple to operate, low in cost and convenient for large-scale production, and the prepared graphene nano-mesh has the characteristics of rich pore channels, large specific surface area, high chemical activity and the like, and has great application potential in 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 net with a macroporous structure.
Background
The nano carbon material is widely applied and researched due to the characteristics of abundant structural form, 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, supercapacitors, secondary batteries, solar cells, biosensors, gas adsorption and separation and the like. Currently, the most commonly used means for preparing porous nanocarbons are a template method and a chemical activation method. The template method is to adopt inert substances such as molecular sieves, silicon oxide, sodium chloride and the like as pore-foaming agents to prepare the porous nano carbon. However, these methods not only increase the cost, but also result in the deletion of the active site of the product due to the chemical inertness of the template; reagents such as hydrofluoric acid with high toxicity and high corrosivity are also needed for removing the template, the operation is complex, and the yield is relatively low; and the pore structure of the product is easy to damage when the template is removed. The chemical activation method is to activate a carbon material with strong acid or strong base to obtain a porous structure. However, the method has the disadvantages of serious loss of carbon quality, low yield, difficult control of the pore channel structure of the product and the like.
Recently, the inorganic molten salt method for preparing the porous nanocarbon material attracts people's attention. Inorganic molten salts (e.g. ZnCl) 2 LiCl, naCl, a mixture thereof, etc.) with biomass, polymerizable organic molecules, ionic liquids, etc., followed by high temperature carbonization, desalting (salt can be recycled) and cleaning, to obtain the porous nanocarbon material. In the high-temperature carbonization process, the molten inorganic salt is not only used as a solvent, but also the free salt ions and the cluster thereof can be used as a pore-forming agent, so that the prepared porous nano carbon material usually has a micropore or mesopore structure. It is reported that the LiCl/KCl mixed molten salt medium can also dissolve intermediate products in the process of carbonizing sugar molecules such as glucose and induce the formation of two-dimensional graphene (Small, 2014, 10. In addition, the MOF material Zn-ZIF-L added into the LiCl/KCl mixed molten salt medium can also form a graphene nano-net (Angew. Chem. Int. Ed.,2019, 58: 13354-13359) with rich defects and the grid size of less than 5 nm. However, these inorganic molten salt method prepared porous nanocarbon materials generally lack macroporous channels (i.e., macroporous channels are commonly absent)>50 nm) are disadvantageousThe increase of active sites and the transmission of related substances limit the wider application of the nano carbon material to a certain extent.
Disclosure of Invention
The invention provides a preparation method of a graphene nano net with a macroporous structure, aiming at the problem that macroporous pore canals are difficult to construct in the preparation of a porous nano carbon material by using an inorganic molten salt method in the prior art.
The invention adopts the following technical scheme for solving the technical problems, and the preparation method of the graphene nano-net with the macroporous structure is characterized by comprising the following specific steps: uniformly mixing alkali metal organic salt and 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 the heating rate of 5-10 ℃/min under the inert atmosphere, preserving the temperature for 2-6h for carbonization, 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 nanosheet, cooling to room temperature, washing and drying to obtain the graphene nanoweb with the macroporous structure.
Further defined, the potassium chloride and the lithium chloride in the inorganic molten salt are ground and mixed uniformly in a molar ratio of 1.
Further limiting, the mass ratio of the alkali metal organic salt to the inorganic molten salt is 1.
Further defined, the inert atmosphere is a nitrogen atmosphere or an argon atmosphere.
Further limiting, in the washing and drying process, deionized water, dilute hydrochloric acid and absolute ethyl alcohol are adopted for washing repeatedly, and the drying temperature is 60-105 ℃.
Compared with the prior art, the method takes alkali metal organic salt as a carbon source in an inorganic molten salt medium, the alkali metal organic salt is carbonized and simultaneously decomposed into the macroporous template in situ, the inorganic molten salt medium dissolves a carbonized intermediate product and induces the carbonized intermediate product to form a two-dimensional nanosheet, and finally the graphene nano-net with the macroporous structure is formed. The invention has the following advantages: 1. the process is simple and convenient to operate. The graphene nano-net 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 the inorganic molten salt medium which is green and environment-friendly, has low steam pressure and wide operating temperature range, and is a green technology. 3. The graphene nano-net prepared by the invention has macroporous grids larger than 50nm, micro/mesoporous channels, large specific surface area and many 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 the graphene nanomesh with a macroporous structure prepared in example 1.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be understood that the scope of the subject matter of the present invention is limited to the examples below, and any technique realized based on the above contents of the present invention falls within the scope of the present invention.
Example 1
Grinding and uniformly mixing potassium chloride and lithium chloride in a molar ratio of 1.45; weighing 4g of the mixed inorganic salt, adding 1g of sodium citrate, and fully grinding by using a mortar; then putting the quartz tube into a tube furnace, introducing nitrogen for 2h to replace oxygen in the quartz tube, heating to 700 ℃ at the heating rate of 5 ℃/min, and preserving the heat at 700 ℃ for 2h to carry out carbonization treatment; and 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 the prepared graphene nano-mesh having a macroporous structure, and it can be seen from the TEM image that the prepared sample has a two-dimensional network structure and the mesh size range is 11-143nm.
Example 2
The steps are basically the same as those of the embodiment 1, except that sodium citrate is replaced by sodium oxalate, and the shape and the structure of the prepared graphene material are similar to those of the embodiment 1.
Example 3
The steps are basically the same as those in example 1, except that the molar ratio of potassium chloride to lithium chloride in the mixed inorganic salt is 1.
Example 4
The procedure is substantially the same as in example 1, except that the mass of the mixed inorganic salt is increased to 4.5g, and the morphology and structure of the prepared graphene material are similar to those of example 1.
Example 5
The steps are basically the same as those of the embodiment 1, except that the nitrogen atmosphere is changed into the argon atmosphere, and the morphology and the structure of the prepared graphene material are similar to those of the embodiment 1.
Example 6
The steps are basically the same as those of the embodiment 1, except that the carbonization treatment heat preservation temperature is 900 ℃, and the morphology and the structure of the prepared graphene material are similar to those of the embodiment 1.
Example 7
The steps are basically the same as those of the embodiment 1, except that the heat preservation time of the carbonization treatment is 6h, and the appearance and the structure of the prepared graphene material are similar to those of the embodiment 1.
Example 8
The steps are basically the same as those in the embodiment 3, except that the carbonization treatment heat preservation temperature is 900 ℃, and the morphology and the structure of the prepared graphene material are similar to those in the embodiment 1.
While the foregoing embodiments have described the general principles, features and advantages of the present invention, it will be understood by those skilled in the art that the present invention is not limited thereto, and that the foregoing embodiments and descriptions are only illustrative of the principles of the present invention, and various changes and modifications can be made without departing from the scope of the principles of the present invention, and these changes and modifications are within the scope of the present invention.
Claims (5)
1. A preparation method of a graphene nano-net with a macroporous structure is characterized by comprising the following specific steps: uniformly mixing alkali metal organic salt and 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 the heating rate of 5-10 ℃/min under an inert atmosphere, preserving heat for 2-6h for carbonization treatment, taking the alkali metal organic salt as a carbon source in the carbonization process, decomposing in situ to obtain a macroporous template, dissolving a carbonized intermediate product in an inorganic molten salt medium, inducing to form a two-dimensional nanosheet, cooling to room temperature, washing and drying to obtain the graphene nanomesh with the macroporous structure.
2. The method for preparing the graphene nano-mesh with the macroporous structure according to claim 1, wherein the method comprises the following steps: the potassium chloride and the lithium chloride in the inorganic molten salt are ground and uniformly mixed according to a molar ratio of 1.
3. The method for preparing the graphene nano-mesh with the macroporous structure according to claim 1, wherein the method comprises the following steps: the mass ratio of the alkali metal organic salt to the inorganic molten salt is 1.
4. The method for preparing the graphene nano-mesh with the macroporous structure according to claim 1, wherein the method comprises the following steps: the inert atmosphere is nitrogen atmosphere or argon atmosphere.
5. The method for preparing the graphene nano-mesh 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 adopted for washing repeatedly, and the drying temperature is 60-105 ℃.
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|---|---|---|---|---|
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