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Preparation method of methylamine acetate ionic liquid

A technology of ionic liquid and methylamine acetate, which is applied in the field of preparation of methylamine acetate ionic liquid, can solve the problems of easy gasification of methylamine and low yield of methylamine acetate ionic liquid, and achieve avoidance of by-products, stable temperature and stable reaction fast speed effect

Pending Publication Date: 2022-07-01
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems that existing methylamine is easy to vaporize under microwave conditions and the yield of methylamine acetate ionic liquid is low, the invention provides a method for preparing methylamine acetate ionic liquid

Method used

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  • Preparation method of methylamine acetate ionic liquid
  • Preparation method of methylamine acetate ionic liquid

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Embodiment 1

[0032] The embodiment of the present invention provides a preparation method of methylamine acetate ionic liquid, and the preparation method comprises the following steps:

[0033] Step 1. Under the stirring condition of the rotating speed of 200rpm, acetic acid is added dropwise to the methylamine aqueous solution with a concentration of 20wt% at a speed of 0.6mL / min, and the temperature is 8°C, the power is 150W, and the microwave condition is 2450MHz The batch reaction is carried out 6 times to obtain an ionic liquid mixture. The conditions of the batch reaction are as follows: the microwave irradiation time is 2 min, the first intermittent time is 2.5 min, and the n+1 intermittent time is longer than the nth intermittent time by 30s , 1≤n≤5; the molar ratio of the above formic acid and methylamine is 1:1.1;

[0034] Step 2: The ionic liquid mixture is subjected to vacuum rotary evaporation for 1.5 h at a temperature of 80° C. and a vacuum degree of -0.15 MPa to obtain meth...

Embodiment 2

[0039] The embodiment of the present invention provides a preparation method of methylamine acetate ionic liquid, and the preparation method comprises the following steps:

[0040] Step 1. Under the stirring condition of the rotating speed of 300rpm, acetic acid was added dropwise to the methylamine methanol solution with a concentration of 15wt% at a speed of 0.8mL / min. The ionic liquid mixture is obtained by intermittently reacting 5 times under the conditions, wherein the conditions of the intermittent reaction are as follows: the microwave irradiation time is 1.5min, the first intermittent time is 2, and the intermittent time of the n+1th time is longer than that of the nth time. 40s, 1≤n≤4; the molar ratio of the above formic acid to methylamine is 1:1.2;

[0041] In step 2, the ionic liquid mixture is subjected to vacuum rotary evaporation for 2 hours under the conditions of temperature of 85° C. and vacuum degree of -0.12 MPa to obtain methylamine acetate ionic liquid M...

Embodiment 3

[0044] The embodiment of the present invention provides a preparation method of methylamine acetate ionic liquid, and the preparation method comprises the following steps:

[0045]Step 1. Under the stirring condition of the rotating speed of 100rpm, acetic acid was added dropwise to the methylamine aqueous solution with a concentration of 15wt% at a speed of 0.5mL / min. The temperature was 5°C, the power was 200W, and the frequency was 2450MHz under microwave conditions The batch reaction is carried out for 6 times to obtain an ionic liquid mixture, wherein the conditions of the batch reaction are: the microwave irradiation time is 2.5min, the first batch time is 3, and the interval time of the n+1th time is 20s longer than that of the nth time. , 1≤n≤5; the molar ratio of the above formic acid and methylamine is 1:1.1;

[0046] In step 2, the ionic liquid mixture is subjected to reduced pressure rotary evaporation for 1 hour under the conditions of a temperature of 75° C. and ...

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Abstract

The invention relates to the technical field of organic synthesis, and particularly discloses a preparation method of methylamine acetate ionic liquid. The preparation method comprises the following steps that acetic acid is added into a methylamine solution, intermittent reaction is conducted 5-6 times under the microwave conditions that the temperature ranges from 5 DEG C to 10 DEG C, the power ranges from 100 W to 200 W, the frequency is 2450 MHz, an ionic liquid mixture is obtained, and the intermittent reaction conditions are that the microwave radiation time ranges from 1.5 min to 2.5 min, the first intermittent time ranges from 2 min to 3 min, the (n + 1) th intermittent time is 20 s to 40 s longer than the nth intermittent time, and n is larger than or equal to 1 and smaller than or equal to 5; and carrying out reduced pressure rotary evaporation on the ionic liquid mixture to obtain the methylamine acetate ionic liquid. The intermittent microwave reaction method is adopted to prepare the ionic liquid, no organic solvent is added, the reaction yield is remarkably improved, the impurity removal step is reduced, the reaction rate is high, and the method has important significance on wide application of the acetic acid methylamine ionic liquid.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of methylamine acetate ionic liquid. Background technique [0002] Ionic liquids are a class of green organic solvents whose structure and function can be designed. Due to its special properties such as wide liquid temperature range, non-volatile, wide electrochemical window, high thermal stability and high oxidation resistance, it has replaced the use of volatile and toxic organic solvents in many chemical reaction processes. It is used in the fields of catalytic reaction, organic synthesis, extraction separation and electrochemistry. [0003] There are many kinds of ionic liquids, and amine-type ionic liquids have the value of development and application due to the advantages of low cost. The amine-type ionic liquids currently studied mainly include amide-type ionic liquids with N,N-dimethylformamide and formamide as cations, and alcoholamine-ty...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C53/10C07C209/00C07C211/04
CPCC07C51/412C07C209/00C07C53/10C07C211/04
Inventor 吴海霞李跃龙李征
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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