Pyridine-ion-containing liquid, preparation method and application thereof
An ionic liquid and pyrrolidine technology is applied in the field of preparation of pyrrolidine-containing ionic liquids, which can solve the problem of high melting point of ionic liquids, and achieve the effects of improving complexing ability, being suitable for industrial production and being environmentally friendly.
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[0024] see figure 1 , figure 1 Show the flow chart of the preparation method of the pyrrolidine-containing ionic liquid according to the embodiment of the present invention, including the following steps:
[0025] Step S01, preparing N-methoxyethoxymethyl-N-methylpyrrolidine halide
[0026] Under anhydrous and oxygen-free conditions, mix N-methylpyrrolidine and haloalkane in a molar ratio of 1:1.05-1:1.2, stir and react at a temperature of 60-80°C for 48-72 hours, and wash to obtain the structural formula (III) Represented N-methoxyethoxymethyl-N-methylpyrrolidine halide, wherein the alkyl halide is selected from methoxyethoxymethyl chloride, methoxyethoxybromethane or methoxyethoxy A kind of in methyl iodide, structural formula (III) is:
[0027]
[0028] Step S02, preparing an ionic liquid containing pyrrolidine
[0029] The N-methoxyethoxymethyl-N-methylpyrrolidine halide represented by the structural formula (III) and the inorganic salt are dissolved in water, stirr...
Embodiment 1
[0042] The embodiment of the present invention contains pyrrole ionic liquid with the following structural formula:
[0043]
[0044] The preparation method of the pyrrole-containing ionic liquid in the embodiment of the present invention comprises the following steps:
[0045] Step 1, preparation of chlorinated N-methoxyethoxymethyl-N-methylpyrrolidine
[0046] in N 2 (or Ar 2 ) under the protection of atmosphere, N-methylpyrrolidine (85g, 1mol) and methoxyethoxymethane chloride (136.4g, 1.1mol) were added to the reactor, the temperature was adjusted to 60°C, and the reaction was stirred for 48 hours ; Standing to cool, then the reaction product was washed three times with ethyl acetate, and dried in vacuum at 80°C to obtain a light yellow solid with a yield of 83%;
[0047] Step 2, preparation of N-methoxyethoxymethyl-N-methylpyrrolidine tetrafluoroborate
[0048] The chloride N-methoxyethoxymethyl-N-methylpyrrolidine (104.5g, 0.5mol), NaBF 4 (55g, 0.5mol), and 100mL...
Embodiment 2
[0051] The embodiment of the present invention contains pyrrole ionic liquid with the following structural formula:
[0052]
[0053] The preparation method of the pyrrole-containing ionic liquid in the embodiment of the present invention comprises the following steps:
[0054] Step 1, preparation of brominated N-methoxyethoxymethyl-N-methylpyrrolidine
[0055] in N 2 (or Ar2 ) Under the protection of the atmosphere, N-methylpyrrolidine (79g, 1mol) and methoxyethoxymethyl bromide (184.8g, 1.1mol) were added to the reactor, the temperature was adjusted to 70°C, and the reaction was stirred for 60 hours; Set to cool, then the reaction product was washed three times with ethyl acetate, and dried under vacuum at 80°C to obtain a pale yellow solid with a yield of 87%;
[0056] Step 2, preparation of N-methoxyethoxymethyl-N-methylpyrrolidine tetrafluoroborate
[0057] The brominated N-methoxyethoxymethyl-N-methylpyrrolidine (0.5mol), NaBF 4 (55g, 0.5mol), and 125mL deionized...
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