CN107189493A - A kind of preparation method of ion liquid modified graphene - Google Patents
A kind of preparation method of ion liquid modified graphene Download PDFInfo
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- CN107189493A CN107189493A CN201710227322.3A CN201710227322A CN107189493A CN 107189493 A CN107189493 A CN 107189493A CN 201710227322 A CN201710227322 A CN 201710227322A CN 107189493 A CN107189493 A CN 107189493A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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Abstract
The invention discloses a kind of preparation method of ion liquid modified graphene.After graphene oxide solution is uniformly mixed with ionic liquid, deionized water is added, is well mixed.Then under nitrogen protection; in the autoclave of polytetrafluoroethylliner liner; 6 ~ 14h is reacted at 120 ~ 200 DEG C; ion liquid modified graphene solution is made; with deionized water centrifuge washing 3 ~ 5 times; suction filtration is carried out, much filtrate is dried in vacuo 6 ~ 12h at 70 ~ 120 DEG C, that is, ion liquid modified graphene is made.The ion liquid modified graphene that the inventive method is simple to operate, cost is low and obtained has higher water solubility, is graphene with opening new approach.
Description
Technical field
The invention belongs to graphene new material technical field, more particularly to a kind of preparation side of ion liquid modified graphene
Method.
Background technology
Preferable graphene-structured is plane hexagonal lattice, can be seen as one stripped down from three-dimensional graphite
Layer molecular layer, each carbon atom is SP2Hydridization, contributes the electronics shape on a remaining track on the direction vertical with plane
Into big pi bond, pi-electron can be moved freely, and assign the good electric conductivity of graphene in graphene, each carbon atom passes through very strong
σ keys（Chemical bond most strong in nature）It is connected with other 3 carbon atoms, these very strong carbon-carbon bonds cause graphene
Lamella is with extremely excellent mechanical property and structural rigidity, and its Young's modulus is about 1TPa, and intensity is about 130 ~ 180GPa.By
There are above-mentioned excellent properties in graphene so that it can be used for the ultracapacitor system in the fields such as automobile, machinery, electronics, military affairs
Make, and can be with various metals, the conductive material of the compound composition excellent combination property of nonmetallic and high polymer material, high-strength composite
Material, shielding material and stealth material etc..
But it is due to the nano-grade size of graphene, big specific surface area, while Van der Waals stronger between graphene molecules
Power is acted on so that graphene easily occurs with reunion shape form, and it is difficult to be distributed in various solvents thus to cause graphene, seriously
The practical application of graphene is have impact on, how effectively dispersed graphite alkene has great importance.
It is to improve its dispersed important method that graphenic surface, which is modified,.Generally strong acid pretreatment is carried out using to graphene
Afterwards, make its surface with functional groups such as carboxyls, the scion graftings such as phthalein amination, esterification reaction is then carried out again, so as to improve graphene
Dispersiveness.But use strong acid or nitration mixture processing that there is certain destruction to graphene, and often need higher temperature and
Long period, while easily producing the gas of contaminative during processing.
Therefore, by experimental study, using the ion liquid modified graphene of one-step method, it can make what graphene uniform disperseed
Simultaneously, moreover it is possible to streamline operation, reduction synthesis cost.
The content of the invention
It is an object of the invention to provide a kind of preparation method of ion liquid modified graphene.
Concretely comprise the following steps：
(1) raw material is weighed according to following parts by weight：The graphene oxide solution that 20 ~ 40 parts of concentration are 10 ~ 25mg/ml, 5 ~ 20
Part ionic liquid, 40 ~ 80 parts of deionized waters, the parts by weight sum of above-mentioned raw materials is 100.
(2) graphene oxide and ionic liquid weighed step (1) is put into beaker, is added after 20 ~ 80min of ultrasound
The deionized water uniform stirring that step (1) is weighed, is made mixed liquor.
(3) under nitrogen protection, mixed liquor made from step (2) is poured into the autoclave of polytetrafluoroethylliner liner,
6 ~ 14h is reacted at 120 ~ 200 DEG C, gained ion liquid modified graphene solution deionized water centrifuge washing 3 ~ 5 times is carried out
Suction filtration, much filtrate is dried in vacuo 6 ~ 12h at 70 ~ 120 DEG C, that is, ion liquid modified graphene is made.
The ionic liquid is 1- alkyl -3- methyl imidazolium tetrafluoroborates, 1- alkyl -3- methylimidazole hexafluorophosphoric acids
Salt, N- alkyl pyridines tetrafluoroborate, 1- butyl methyl tetrafluoroborate chlorination 1- pi-allyl -3- methylimidazoles, bromination
One kind in 1- pi-allyl -3- methylimidazoles and iodate 1- pi-allyl -3- methylimidazoles.
The ion liquid modified graphene that the inventive method is simple to operate, cost is low and obtained has higher water-soluble
Property.
Brief description of the drawings
Fig. 1 is that the embodiment of the present invention 1 prepares ion liquid modified graphene dispersed photo in deionized water.
Embodiment
Embodiment 1：
(1) raw material is weighed according to following parts by weight：The graphene oxide solution that 20 parts of concentration are 25mg/ml, 5 parts of ionic liquids
Body, 75 parts of deionized waters.
(2) graphene oxide and ionic liquid weighed step (1) is put into beaker, and step is added after ultrasonic 20min
Suddenly the deionized water uniform stirring that (1) is weighed, is made mixed liquor.
(3) under nitrogen protection, mixed liquor made from step (2) is poured into the autoclave of polytetrafluoroethylliner liner,
React 8h at 200 DEG C, gained ion liquid modified graphene solution deionized water centrifuge washing 4 times carries out suction filtration, filtered out
Thing is dried in vacuo 7h at 80 DEG C, that is, ion liquid modified graphene is made.
The ionic liquid is 1- alkyl -3- methyl imidazolium tetrafluoroborates.
Embodiment 2：
(1) raw material is weighed according to following parts by weight：The graphene oxide solution that 25 parts of concentration are 20mg/ml, 10 parts of ionic liquids
Body, 65 parts of deionized waters.
(2) graphene oxide and ionic liquid weighed step (1) is put into beaker, and step is added after ultrasonic 30min
Suddenly the deionized water uniform stirring that (1) is weighed, is made mixed liquor.
(3) under nitrogen protection, mixed liquor made from step (2) is poured into the autoclave of polytetrafluoroethylliner liner,
React 10h at 180 DEG C, gained ion liquid modified graphene solution deionized water centrifuge washing 4 times carries out suction filtration, filter
Go out thing and 8h is dried in vacuo at 80 DEG C, that is, ion liquid modified graphene is made.
The ionic liquid is 1- alkyl -3- methyl imidazolium tetrafluoroborates.
Embodiment 3：
(1) raw material is weighed according to following parts by weight：The graphene oxide solution that 30 parts of concentration are 17.5mg/ml, 10 parts of ions
Liquid, 60 parts of deionized waters.
(2) graphene oxide and ionic liquid weighed step (1) is put into beaker, and step is added after ultrasonic 30min
Suddenly the deionized water uniform stirring that (1) is weighed, is made mixed liquor.
(3) under nitrogen protection, mixed liquor made from step (2) is poured into the autoclave of polytetrafluoroethylliner liner,
React 14h at 140 DEG C, gained ion liquid modified graphene solution deionized water centrifuge washing 4 times carries out suction filtration, filter
Go out thing and 8h is dried in vacuo at 80 DEG C, that is, ion liquid modified graphene is made.
The ionic liquid is 1- alkyl -3- methylimidazole hexafluorophosphates.
Embodiment 4：
(1) raw material is weighed according to following parts by weight：The graphene oxide solution that 40 parts of concentration are 10mg/ml, 15 parts of ionic liquids
Body, 55 parts of deionized waters.
(2) graphene oxide and ionic liquid weighed step (1) is put into beaker, and step is added after ultrasonic 40min
Suddenly the deionized water uniform stirring that (1) is weighed, is made mixed liquor.
(3) under nitrogen protection, mixed liquor made from step (2) is poured into the autoclave of polytetrafluoroethylliner liner,
React 10h at 160 DEG C, gained ion liquid modified graphene solution deionized water centrifuge washing 4 times carries out suction filtration, filter
Go out thing and 8h is dried in vacuo at 80 DEG C, that is, ion liquid modified graphene is made.
The ionic liquid is 1- alkyl -3- methylimidazole hexafluorophosphates.
Embodiment 5：
(1) raw material is weighed according to following parts by weight：The graphene oxide solution that 30 parts of concentration are 17.5mg/ml, 15 parts of ions
Liquid, 55 parts of deionized waters.
(2) graphene oxide and ionic liquid weighed step (1) is put into beaker, and step is added after ultrasonic 50min
Suddenly the deionized water uniform stirring that (1) is weighed, is made mixed liquor.
(3) under nitrogen protection, mixed liquor made from step (2) is poured into the autoclave of polytetrafluoroethylliner liner,
React 12h at 160 DEG C, gained ion liquid modified graphene solution deionized water centrifuge washing 4 times carries out suction filtration, filter
Go out thing and 8h is dried in vacuo at 80 DEG C, that is, ion liquid modified graphene is made.
The ionic liquid is N- alkyl pyridine tetrafluoroborates.
Embodiment 6：
(1) raw material is weighed according to following parts by weight：The graphene oxide solution that 35 parts of concentration are 10mg/ml, 15 parts of ionic liquids
Body, 50 parts of deionized waters.
(2) graphene oxide and ionic liquid weighed step (1) is put into beaker, and step is added after ultrasonic 50min
Suddenly the deionized water uniform stirring that (1) is weighed, is made mixed liquor.
(3) under nitrogen protection, mixed liquor made from step (2) is poured into the autoclave of polytetrafluoroethylliner liner,
React 12h at 140 DEG C, gained ion liquid modified graphene solution deionized water centrifuge washing 4 times carries out suction filtration, filter
Go out thing and 8h is dried in vacuo at 80 DEG C, that is, ion liquid modified graphene is made.
The ionic liquid is 1- butyl methyl tetrafluoroborate chlorination 1- pi-allyl -3- methylimidazoles.
Embodiment 7：
(1) raw material is weighed according to following parts by weight：The graphene oxide solution that 40 parts of concentration are 10mg/ml, 15 parts of ionic liquids
Body, 45 parts of deionized waters.
(2) graphene oxide and ionic liquid weighed step (1) is put into beaker, and step is added after ultrasonic 30min
Suddenly the deionized water uniform stirring that (1) is weighed, is made mixed liquor.
(3) under nitrogen protection, mixed liquor made from step (2) is poured into the autoclave of polytetrafluoroethylliner liner,
React 12h at 160 DEG C, gained ion liquid modified graphene solution deionized water centrifuge washing 4 times carries out suction filtration, filter
Go out thing and 8h is dried in vacuo at 80 DEG C, that is, ion liquid modified graphene is made.
The ionic liquid is 1- butyl methyl tetrafluoroborate chlorination 1- pi-allyl -3- methylimidazoles.
Claims (1)
1. a kind of preparation method of ion liquid modified graphene, it is characterised in that concretely comprise the following steps：
(1) raw material is weighed according to following parts by weight：The graphene oxide solution that 20 ~ 40 parts of concentration are 10 ~ 25mg/ml, 5 ~ 20
Part ionic liquid, 40 ~ 80 parts of deionized waters, the parts by weight sum of above-mentioned raw materials is 100；
(2) graphene oxide and ionic liquid weighed step (1) is put into beaker, and step is added after 20 ~ 80min of ultrasound
(1) the deionized water uniform stirring weighed, is made mixed liquor；
(3) under nitrogen protection, mixed liquor made from step (2) is poured into the autoclave of polytetrafluoroethylliner liner, 120
6 ~ 14h is reacted at ~ 200 DEG C, gained ion liquid modified graphene solution deionized water centrifuge washing 3 ~ 5 times carries out suction filtration,
Much filtrate is dried in vacuo 6 ~ 12h at 70 ~ 120 DEG C, that is, ion liquid modified graphene is made；
The ionic liquid is 1- alkyl -3- methyl imidazolium tetrafluoroborates, 1- alkyl -3- methylimidazoles hexafluorophosphate, N-
Alkyl pyridine tetrafluoroborate, 1- butyl methyl tetrafluoroborate chlorination 1- pi-allyl -3- methylimidazoles, bromination 1- allyls
One kind in base -3- methylimidazoles and iodate 1- pi-allyl -3- methylimidazoles.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108335917A (en) * | 2018-01-26 | 2018-07-27 | 渤海大学 | A kind of preparation method of carbon nanofibers load ordered arrangement redox graphene electrode material |
| CN108950285A (en) * | 2018-08-29 | 2018-12-07 | 含山县金中环装饰材料有限公司 | A kind of ionic liquid modified graphene reinforced aluminum matrix composites |
| CN109401195A (en) * | 2018-10-15 | 2019-03-01 | 桂林理工大学 | Epoxy resin/graphite alkene/ionic liquid composite material preparation method |
| CN109954509A (en) * | 2018-12-04 | 2019-07-02 | 山东科技大学 | A kind of preparation method and application of silicon carbide-based photochemical catalyst |
| CN110963487A (en) * | 2019-12-21 | 2020-04-07 | 桂林理工大学 | Preparation method of ionic liquid modified graphene with wave absorption performance |
| CN111117106A (en) * | 2019-12-24 | 2020-05-08 | 中山圣洛迪新材料有限公司 | Wood-plastic composite floor and preparation method thereof |
| CN111154087A (en) * | 2020-01-15 | 2020-05-15 | 浙江光华科技股份有限公司 | Nitrogen-phosphorus-fluorine co-doped graphene oxide/polyester resin compound and preparation method thereof |
| CN111518524A (en) * | 2020-05-29 | 2020-08-11 | 四川路恒达机械科技有限公司 | Preparation method of special liquid for heating |
| CN111834641A (en) * | 2020-06-24 | 2020-10-27 | 中国科学院过程工程研究所 | Preparation method of carbon felt modified by graphene in ionic liquid |
| CN113072916A (en) * | 2021-03-05 | 2021-07-06 | 西安交通大学 | Modified graphene-based heat conduction enhanced ionic liquid composite phase change heat storage material and preparation method thereof |
| CN113896188A (en) * | 2021-10-22 | 2022-01-07 | 中国科学院兰州化学物理研究所 | Preparation method of boron-doped graphene heat-conducting film |
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Cited By (15)
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| CN108335917A (en) * | 2018-01-26 | 2018-07-27 | 渤海大学 | A kind of preparation method of carbon nanofibers load ordered arrangement redox graphene electrode material |
| CN108950285A (en) * | 2018-08-29 | 2018-12-07 | 含山县金中环装饰材料有限公司 | A kind of ionic liquid modified graphene reinforced aluminum matrix composites |
| CN109401195A (en) * | 2018-10-15 | 2019-03-01 | 桂林理工大学 | Epoxy resin/graphite alkene/ionic liquid composite material preparation method |
| CN109954509A (en) * | 2018-12-04 | 2019-07-02 | 山东科技大学 | A kind of preparation method and application of silicon carbide-based photochemical catalyst |
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| CN111117106A (en) * | 2019-12-24 | 2020-05-08 | 中山圣洛迪新材料有限公司 | Wood-plastic composite floor and preparation method thereof |
| CN111154087A (en) * | 2020-01-15 | 2020-05-15 | 浙江光华科技股份有限公司 | Nitrogen-phosphorus-fluorine co-doped graphene oxide/polyester resin compound and preparation method thereof |
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| CN111834641A (en) * | 2020-06-24 | 2020-10-27 | 中国科学院过程工程研究所 | Preparation method of carbon felt modified by graphene in ionic liquid |
| CN111834641B (en) * | 2020-06-24 | 2022-03-15 | 中国科学院过程工程研究所 | Preparation method of carbon felt modified by graphene in ionic liquid |
| CN113072916A (en) * | 2021-03-05 | 2021-07-06 | 西安交通大学 | Modified graphene-based heat conduction enhanced ionic liquid composite phase change heat storage material and preparation method thereof |
| CN113896188A (en) * | 2021-10-22 | 2022-01-07 | 中国科学院兰州化学物理研究所 | Preparation method of boron-doped graphene heat-conducting film |
| CN114656823A (en) * | 2022-04-06 | 2022-06-24 | 张家港市天源制漆涂装有限公司 | Water-based epoxy heavy-duty anticorrosive paint and preparation method thereof |
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