Low-viscosity ionic liquid
A technology of ionic liquids and compounds, applied in the field of preparation of low-viscosity ionic liquids
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Embodiment 1
[0026] Put N-butylimidazole (65g, 0.52mol) and chlorobutane (58.14g, 0.62mol) in the 250ml there-necked flask that has condensing reflux device, reaction mixture was reacted 72 hours at 78 ℃ of mechanical stirring, reaction mixture After cooling, it was washed with ethyl acetate for 3 to 5 times to remove unreacted raw materials, and then distilled under reduced pressure to obtain a light yellow viscous liquid, 110 g of 1-butyl-3-butyl imidazole chloride, with a yield of 90%.
[0027] Divide the product 1-butyl-3-butylimidazole chloride into four parts, and add FeCl in the mass ratio (1:1, 1:2, 1:3, 1:4) 3 ·6H 2 O, stirred at room temperature for 24 hours, centrifuged and static layered, 1:1 to take the lower liquid, 1:2, 1:3, 1:4 to take the upper liquid respectively.
[0028] The following are the physical data and detection data of four iron-based ionic liquids.
[0029] Raw material molar ratio
Embodiment 2
[0031] Put N-benzyl imidazole (80g, 0.5mol) and dodecane chloride (113.7g, 0.556mol) in the 250ml there-necked flask with condensing reflux device, the reaction mixture reacted 72 hours at 85 ℃ of mechanical stirring, After the reaction mixture is cooled, add ethyl acetate, heat to 85°C and reflux for a period of time, then cool to room temperature to separate ethyl acetate, repeat the above operation 3 to 5 times, remove unreacted raw materials, and then heat to 85°C under reduced pressure for distillation 182 g of tan solid 1-benzyl-3-dodecyl imidazole chloride was obtained with a yield of 94%.
[0032] Divide 1-benzyl-3-dodecyl imidazolium chloride into four parts, and add FeCl at a mass ratio (1:1, 1:2, 1:3, 1:4) 3 ·6H 2 O, heated to 45°C in a water bath and stirred for 24 hours, centrifuged and statically layered, the lower layer liquid was taken for 1:1, and the upper layer liquid was taken for 1:2, 1:3, and 1:4 respectively.
[0033] The following are the physical dat...
Embodiment 3
[0036] Put 433.3g of N-methylimidazole and 512.9g of chlorobutane into a 250ml three-neck flask with a condensing reflux device, and the reaction mixture was mechanically stirred at 78°C for 72 hours. After the reaction mixture was cooled, it was washed with ethyl acetate for 3 to 5 Once, the unreacted raw materials were removed, and then distilled under reduced pressure to obtain a light yellow viscous liquid, namely 852.9 g of 1-methyl-3-butyl imidazole chloride, with a yield of 90.13%.
[0037] Divide the product 1-methyl-3-butyl imidazole chloride into four parts, and add FeCl in the mass ratio (1:1, 1:1.5, 1:2, 1:2.5) 3 ·6H 2 O, stirred at room temperature for 24 hours, centrifuged and static layered, 1:1 and 1:1.5 were used to take the lower layer liquid, and 1:2 and 1:2.5 were used to take the upper layer liquid.
[0038] The physical data and detection data of the four ionic liquids are as follows:
[0039] Raw material molar ratio
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