CN102899677A - Method for electrochemically synthesizing ionic liquid/carbon dot gel in one step - Google Patents
Method for electrochemically synthesizing ionic liquid/carbon dot gel in one step Download PDFInfo
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Abstract
The invention provides a method for electrochemically synthesizing an ionic liquid/carbon dot gel in one step. Room temperature ionic liquid is taken as an electrolyte and a high-purity carbon rod is taken as a carbon dot resource. The cleaned high-purity carbon rod is placed into a mixed solution of the room temperature ionic liquid and water; the carbon rod is oxidized in a position of positive potential by adopting a constant potential electrolytic process; and cleaning and drying are performed, so that the ionic liquid/carbon dot gel is obtained. According to the method provided by the invention, the room temperature ionic liquid/water is directly taken as the electrolyte and the high-purity carbon rod is taken as the carbon dot resource, and an anode carbon rod is oxidized in the position of the positive potential in the electrolyte solution, so that the prepared ionic liquid/carbon dot gel is uniform and excellent in reproducibility. The method provided by the invention is simple and is easy to implement; the speed is high; the material resource is wide and low-cost; the preparation process is pollution-free; the method can be finished in a common chemical laboratory; the method can be applied to large-scale industrial production; the ionic liquid/carbon dot gel prepared according to the method can be used for preparing the material with high conductivity; and the ionic liquid/carbon dot gel can be served as the solar battery electrolyte and can be used for constructing a chemical and biological sensor.
Description
Technical field
The invention belongs to chemistry and material science, relate to the method for a class electrochemical synthesis ionic liquid/carbon point gel.
Background technology
Ionic liquid at room temperature (being low temperature molten salt) is at room temperature for liquid, consisted of by ion fully, have higher ionic conductivity, extremely low volatility, higher thermostability (reaching approximately 400 ℃), the advantages such as wider electrochemical window (about 4 V).By changing the structure of ionic liquid positively charged ion or negatively charged ion, also can in a big way, change the character of ionic liquid.Therefore, ionic liquid as the determine safety problem of liquid battery of the electrolysis mass-energy efficient solution of electrical condenser and battery etc., had very tempting application prospect.At present, its application form is mainly: directly as ionogen; Or solidify ionic liquid with polymkeric substance, small molecules gelifying agent and inorganic nano-particle and form gel electrolyte, this gellike ionogen does not contain any volatilizable composition, good stability, and specific conductivity is high.Particularly solidify the formed gel electrolyte of ionic liquid with inorganic nano-particle and have very tempting prospect, reason is that the one nanoparticle has high specific surface area, orderly pore passage structure, therefore can be used as the solidifying agent of ionic liquid; The ion diffusion that the structure of its two nanoparticle can be in the ionogen provides passage, can obviously improve its ionic conductivity.
At present, prepare ionic liquid/used method of nanoparticle gel and mostly be direct mixing, ultrasonic or in grinding alms bowl, directly mill.Yet nano particle diameter is little, specific surface greatly, is very easily reunited, and surface polarity is large, and is poor with the common solvent consistency, adopts general blending technology to be difficult to obtain Uniform Dispersion on the nanoscale; And being mixed to get inhomogeneous meeting so that existing interface modification technology is difficult to eliminate fully the interfacial tension between filler and ionic liquid matrix, the bonding interface that is difficult to realize ideal does not reach the purpose of the nano-filled curing of particle.And different batches preparation ionic liquid/nanoparticle gelling properties difference is very large, be difficult to realize batch production.Therefore, prepare that to have well distributed ionic liquid/nanoparticle gel be research and the prerequisite used.
Since Iijima found carbon nanotube, nanosecond science and technology had obtained develop rapidly.Take the nano material of carbon as the basis, comprise carbon nanotube, Nano diamond, soccerballene, Nano carbon fibers peacekeeping carbon quantum dot etc.Carbon point also arouses great concern as a kind of new carbon nanomaterial.Carbon nano-particles is as a kind of new quantum dot, compares with traditional quantum dot to have obvious superiority: its good water solubility; Toxicity is little.With the research phase of carbon nanotube, Nano diamond and traditional quantum dot, carbon point there is no more fully research so far because its preparation method and isolation technique are deficient, and relevant report is also less.The patent documentation that synthesizes for carbon point at present has " a kind of preparation method of low-toxicity fluorescent carbon point " (Chinese patent application number 200810197695.1), this patent is to be to carry out electrochemical oxidation in the oxysalt aqueous solution of pH value between 2-11 to process with carbon dioxide process carbon electrode at electrolyte solution, has made hypotoxic fluorescent carbon point.With the ionic liquid of the present invention preparation/carbon point gel, owing to ionic liquid and carbon point all have good electroconductibility, can prepare the material with high conduction performance; Because ionic liquid/carbon point gel does not have volatility, can transmit well electronics again, can be used as solar cell electrolytic solution and make up chemistry and biosensor.
Summary of the invention
The objective of the invention is for above-mentioned present situation, aim to provide that a kind of raw materials cost cheaply is easy to get, operation is simple, the gel that makes evenly, favorable reproducibility, preparation process is pollution-free, can carry out the method an of the one-step electrochemistry synthetic ionic liquid of large-scale industrial production/carbon point gel.
The implementation of the object of the invention is, an one-step electrochemistry synthesizes the method for ionic liquid/carbon point gel, and concrete steps are as follows:
(1) the high-purity carbon-point with two long 6-7cm carries out ultrasonic cleaning;
(2) two cleaned carbon-points are placed in parallel in 2mL ionic liquid at room temperature/water mixed system, are used separately as anode and negative electrode, between two electrodes, apply 4-10V constant potential, electrolysis 0.3-10h;
Used ionic liquid is 1-butyl-3-Methylimidazole Tetrafluoroboric acid, 1-butyl-3-Methylimidazole phosphofluoric acid, 1-ethyl-3-methylimidazole Tetrafluoroboric acid, 1-ethyl-3-methylimidazole phosphofluoric acid, 1-be base-3-Methylimidazole Tetrafluoroboric acid or 1-base-3-Methylimidazole phosphofluoric acid;
The ionic liquid at room temperature of used ionic liquid at room temperature/water mixed solution: the volume ratio of water is 9:1,8:2,7:3,6:4,5:5 or 4:6;
(3) electrolyte solution after the collection electrolysis; Clean 5-6 time with 0.5-2mL dehydrated alcohol;
(4) electrolyte solution after will cleaning is placed in 80 ℃ the baking oven and dries 2h, namely gets ionic liquid/carbon point gel.
The present invention with ionic liquid at room temperature/water mixed solution directly as ionogen, with high-purity carbon-point as the carbon point source, in carrying out oxidation than positive potential place antianode carbon-point, it is even, favorable reproducibility to prepare the gel that ionic liquid/carbon point gel makes in the electrolyte solution.The present invention is simple, fast; Material source is extensively cheap, and preparation process is pollution-free; Can finish at general chemical laboratory, and can carry out large-scale industrial production.
Description of drawings
Fig. 1 is the TEM phenogram of the example 1 1-butyl synthetic take 1-butyl-3-Methylimidazole phosphofluoric acid as ionogen-3-Methylimidazole phosphofluoric acid/carbon point,
Fig. 2 is the TEM phenogram of the example 2 1-butyl synthetic take 1-butyl-3-Methylimidazole Tetrafluoroboric acid as ionogen-3-Methylimidazole Tetrafluoroboric acid/carbon point,
Fig. 3 is the photo of the example 1 1-butyl synthetic take 1-butyl-3-Methylimidazole phosphofluoric acid as ionogen-3-Methylimidazole phosphofluoric acid/carbon point,
Fig. 4 is the photo of the example 2 1-butyl synthetic take 1-butyl-3-Methylimidazole Tetrafluoroboric acid as ionogen-3-Methylimidazole Tetrafluoroboric acid/carbon point.
Embodiment
The present invention, originates as carbon point with high-purity carbon-point as ionogen with ionic liquid at room temperature.Place ionic liquid at room temperature in potentiostatic electrolysis carbon-point being carried out oxidation than the positive potential place cleaned high-purity carbon-point, electrolytic solution is cleaned, make ionic liquid/carbon point gel after the drying.
Used ionic liquid is 1-butyl-3-Methylimidazole Tetrafluoroboric acid, 1-butyl-3-Methylimidazole phosphofluoric acid, 1-ethyl-3-methylimidazole Tetrafluoroboric acid, 1-ethyl-3-methylimidazole phosphofluoric acid, 1-be base-3-Methylimidazole Tetrafluoroboric acid or 1-base-3-Methylimidazole phosphofluoric acid.The ionic liquid at room temperature of used ionic liquid at room temperature/water mixed solution: the volume ratio of water is 9:1,8:2,7:3,6:4,5:5 or 4:6.The synthetic required condition of electrooxidation is: used constant potential is between 4-10V, and electrolysis time is between 0.3-10h.
Below in conjunction with embodiment in detail the present invention is described in detail.
Embodiment 1
(1) the high-purity carbon-point with two long 6cm carries out ultrasonic cleaning;
(2) two cleaned carbon-points are placed in parallel among the electrolysis Xiao Chi that fills 2mL1-butyl-3-Methylimidazole phosphofluoric acid/water (V:V=5:5), two carbon-points are used separately as anode and negative electrode.Between two electrodes, apply constant potential 4V, electrolysis 3h;
(3) electrolyte solution after the collection electrolysis; Clean 5 times with the 0.5mL dehydrated alcohol;
(4) electrolyte solution after will cleaning is placed on 2h in 80 ℃ the baking oven, and oven dry makes ionic liquid shown in Figure 1/carbon point gel.
As seen from Figure 1, prepared carbon point is evenly distributed in 1-butyl-3-Methylimidazole phosphofluoric acid, forms carbon point/ionic liquid gel.Fig. 3 shows that formed gel has certain bonding strength, tackyness.
Embodiment 2
(1) the high-purity carbon-point with two long 6.5cm carries out ultrasonic cleaning;
(2) two cleaned carbon-points are placed in parallel among the electrolysis Xiao Chi that fills 2mL1-butyl-3-Methylimidazole Tetrafluoroboric acid/water (V:V=6:4), two carbon-points are used separately as anode and negative electrode.Between two electrodes, apply constant potential 6V, electrolysis 2h;
(3) electrolyte solution after the collection electrolysis; Clean 6 times with the 1mL dehydrated alcohol;
(4) electrolyte solution after will cleaning is placed on 2h in 80 ℃ the baking oven, and oven dry makes ionic liquid shown in Figure 2/carbon point gel.
As seen from Figure 2, prepared carbon point is evenly distributed in 1-butyl-3-Methylimidazole Tetrafluoroboric acid, forms carbon point/ionic liquid gel.Fig. 4 shows that formed gel has certain bonding strength, tackyness.
Embodiment 3
(1) the high-purity carbon-point with two long 6.7cm carries out ultrasonic cleaning;
(2) two cleaned carbon-points are placed in parallel among the electrolysis Xiao Chi that fills 2mL1-ethyl-3-methylimidazole Tetrafluoroboric acid/water (V:V=9:1), two carbon-points are used separately as anode and negative electrode.Between two electrodes, apply constant potential 8V, electrolysis 1h;
(3) electrolyte solution after the collection electrolysis; Clean 6 times with 1 mL dehydrated alcohol;
(4) electrolyte solution after will cleaning is placed on 2h in 80 ℃ the baking oven, and oven dry makes ionic liquid/carbon point gel.
Embodiment 4
(1) the high-purity carbon-point with two long 6.6cm carries out ultrasonic cleaning;
(2) two cleaned carbon-points are placed in parallel among the electrolysis Xiao Chi that fills 2mL1-ethyl-3-methylimidazole phosphofluoric acid/water (V:V=9:1), two carbon-points are used separately as anode and negative electrode.Between two electrodes, apply constant potential 10V, electrolysis 5h;
(3) electrolyte solution after the collection electrolysis; Clean 6 times with the 2mL dehydrated alcohol;
(4) electrolyte solution after will cleaning is placed on 2h in 80 ℃ the baking oven, and oven dry makes ionic liquid/carbon point gel.
Embodiment 5
(1) the high-purity carbon-point with two long 7cm carries out ultrasonic cleaning;
(2) two cleaned carbon-points are placed in parallel in fill 2mL1-among the electrolysis Xiao Chi of base-3-Methylimidazole Tetrafluoroboric acid/water (V:V=8:2), two carbon-points are used separately as anode and negative electrode.Between two electrodes, apply constant potential 9V, electrolysis 1h;
(3) electrolyte solution after the collection electrolysis; Clean 6 times with the 1mL dehydrated alcohol;
(4) electrolyte solution after will cleaning is placed on 2h in 80 ℃ the baking oven, and oven dry makes ionic liquid/carbon point gel.
Embodiment 6
(1) the high-purity carbon-point with two long 6.9cm carries out ultrasonic cleaning;
(2) two cleaned carbon-points are placed in parallel in fill 2mL1-among the electrolysis Xiao Chi of base-3-Methylimidazole phosphofluoric acid/water (V:V=7:3), two carbon-points are used separately as anode and negative electrode.Between two electrodes, apply constant potential 7V, electrolysis 2h;
(3) electrolyte solution after the collection electrolysis; Clean 5 times with the 1mL dehydrated alcohol;
(4) electrolyte solution after will cleaning is placed on 2h in 80 ℃ the baking oven, and oven dry makes ionic liquid/carbon point gel.
Embodiment 7
(1) the high-purity carbon-point with two long 7cm carries out ultrasonic cleaning;
(2) two cleaned carbon-points are placed in parallel in fill 2mL1-among the electrolysis Xiao Chi of base-3-Methylimidazole phosphofluoric acid/water (V:V=4:6), two carbon-points are used separately as anode and negative electrode.Between two electrodes, apply constant potential 5V, electrolysis 0.3h;
(3) electrolyte solution after the collection electrolysis; Clean 6 times with 2 mL dehydrated alcohols;
(4) electrolyte solution after will cleaning is placed on 2h in 80 ℃ the baking oven, and oven dry makes ionic liquid/carbon point gel.
Embodiment 8
(1) the high-purity carbon-point with two long 6.8cm carries out ultrasonic cleaning;
(2) two cleaned carbon-points are placed in parallel among the electrolysis Xiao Chi that fills 2mL1-ethyl-3-methylimidazole phosphofluoric acid/water (V:V=8:2), two carbon-points are used separately as anode and negative electrode.Between two electrodes, apply constant potential 4V, electrolysis 10h;
(3) electrolyte solution after the collection electrolysis; Clean 5 times with the 1mL dehydrated alcohol;
(4) electrolyte solution after will cleaning is placed on 2h in 80 ℃ the baking oven, and oven dry makes ionic liquid/carbon point gel.
Claims (1)
1. an one-step electrochemistry synthesizes the method for ionic liquid/carbon point gel, it is characterized in that concrete steps are as follows:
(1) the high-purity carbon-point with two long 6-7cm carries out ultrasonic cleaning;
(2) two cleaned carbon-points are placed in parallel in 2mL ionic liquid at room temperature/water mixed system, are used separately as anode and negative electrode, between two electrodes, apply 4-10V constant potential, electrolysis 0.3-10h;
Used ionic liquid is 1-butyl-3-Methylimidazole Tetrafluoroboric acid, 1-butyl-3-Methylimidazole phosphofluoric acid, 1-ethyl-3-methylimidazole Tetrafluoroboric acid, 1-ethyl-3-methylimidazole phosphofluoric acid, 1-be base-3-Methylimidazole Tetrafluoroboric acid or 1-base-3-Methylimidazole phosphofluoric acid;
The ionic liquid at room temperature of used ionic liquid at room temperature/water mixed solution: the volume ratio of water is 9:1,8:2,7:3,6:4,5:5 or 4:6;
(3) electrolyte solution after the collection electrolysis; Clean 5-6 time with 0.5-2mL dehydrated alcohol;
(4) electrolyte solution after will cleaning is placed in 80 ℃ the baking oven and dries 2h, namely gets ionic liquid/carbon point gel.
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Cited By (4)
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| CN104726890A (en) * | 2015-02-09 | 2015-06-24 | 银基烯碳新材料股份有限公司 | Method for preparing nano active carbon solution based on electrolytic method |
| CN107221455A (en) * | 2017-06-24 | 2017-09-29 | 渤海大学 | A kind of preparation method of the high-performance electrolyte solution for carbon-based ionic liquid composites of adulterating |
| CN112028220A (en) * | 2020-09-07 | 2020-12-04 | 江苏开放大学（江苏城市职业学院） | Method for catalytic degradation of bisphenol A |
| CN112760688A (en) * | 2021-03-08 | 2021-05-07 | 浙江大学 | Electrolyte solution for carbon plating and preparation and use methods thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104726890A (en) * | 2015-02-09 | 2015-06-24 | 银基烯碳新材料股份有限公司 | Method for preparing nano active carbon solution based on electrolytic method |
| CN107221455A (en) * | 2017-06-24 | 2017-09-29 | 渤海大学 | A kind of preparation method of the high-performance electrolyte solution for carbon-based ionic liquid composites of adulterating |
| CN107221455B (en) * | 2017-06-24 | 2019-02-12 | 渤海大学 | A kind of preparation method for the high-performance electrolyte solution adulterating carbon-based ionic liquid composites |
| CN112028220A (en) * | 2020-09-07 | 2020-12-04 | 江苏开放大学（江苏城市职业学院） | Method for catalytic degradation of bisphenol A |
| CN112760688A (en) * | 2021-03-08 | 2021-05-07 | 浙江大学 | Electrolyte solution for carbon plating and preparation and use methods thereof |
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