Preparation method of methamine formate ionic liquid
A technology of ionic liquid and methylamine formate, which is applied in the preparation of carboxylic acid salts, organic compounds, amino compounds, etc., can solve the problems of harsh reaction conditions, low purity, and low repeatability, so as to ensure quality and repeatability , Simplify the operation steps and shorten the reaction time
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Embodiment 1
[0039] The embodiment of the present invention provides a preparation method of methylamine formate ionic liquid, and the preparation method comprises the following steps:
[0040] Step 1, measure according to the mol ratio of formic acid and methylamine as 1:1.2, refer to figure 2 The schematic diagram of the device, the methylamine aqueous solution with a concentration of 40wt% was added to the three-necked flask 4, the formic acid was added to the syringe 1, and when the formic acid started to inject, the temperature of the ultrasonic generator 2 was set to 20 ℃, and the frequency was 25KHz , the power is 1.5KW, after the injection is completed, the reaction is performed for 15min to obtain an ionic liquid mixture, wherein the injection speed of formic acid is 6mL / min;
[0041] In step 2, the ionic liquid mixture is subjected to rotary evaporation under reduced pressure for 2 hours at a temperature of 60° C. and a vacuum degree of -0.1 MPa to obtain methylamine formate ion...
Embodiment 2
[0046] The embodiment of the present invention provides a preparation method of methylamine formate ionic liquid, and the preparation method comprises the following steps:
[0047] Step 1, measure according to the mol ratio of formic acid and methylamine to be 1:1, refer to figure 2 The schematic diagram of the device, the methylamine methanol solution with a concentration of 33wt% was added to the three-necked flask 4, the formic acid was added to the syringe 1, and when the formic acid started to inject, the temperature of the ultrasonic generator 2 was set to 25 ℃, and the frequency was 20KHz, the power is 2KW, after the injection is completed, the reaction is performed for 30min to obtain an ionic liquid mixture, wherein the injection speed of formic acid is 9mL / min;
[0048] In step 2, the ionic liquid mixture is subjected to vacuum rotary evaporation for 2 hours under the conditions of a temperature of 65° C. and a vacuum degree of -0.095 MPa to obtain methylamine forma...
Embodiment 3
[0051] The embodiment of the present invention provides a preparation method of methylamine formate ionic liquid, and the preparation method comprises the following steps:
[0052] Step 1, measure according to the mol ratio of formic acid and methylamine as 1:1.1, refer to figure 2 The schematic diagram of the device, the methylamine methanol solution with a concentration of 35wt% was added to the three-necked flask 4, the formic acid was added to the syringe 1, and when the formic acid started to inject, the temperature of the ultrasonic generator 2 was set to 30 ° C, and the frequency was 25KHz, the power is 3KW, after the injection is completed, the reaction is performed for 20min to obtain an ionic liquid mixture, wherein the injection speed of formic acid is 3mL / min;
[0053] In step 2, the ionic liquid mixture is subjected to rotary evaporation under reduced pressure at a temperature of 70° C. and a vacuum degree of -0.09 MPa for 1 hour to obtain methylamine formate ionic...
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