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A New Efficient and Dynamic Synthesis and Purification Technology of N-Methylimidazole

A new technology of methylimidazole and new technology, which is applied in the new field of high-efficiency dynamic N-methylimidazole purification, can solve the problems of complex process flow, high energy consumption of reaction, complex purification, etc., achieve short purification process flow and increase product yield , The effect of easy access to raw materials

Active Publication Date: 2022-03-29
郑州中科新兴产业技术研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The imidazole substitution method has high energy consumption, a large amount of sewage, and the use of expensive and toxic methyl iodide. Therefore, most of the current one-step ring methods are used to produce N-methylimidazole
However, the existing one-step ring production process also has problems such as complicated purification and serious pollution.
Both patents CN110343071A and CN103086978 use imidazole and methanol to synthesize N-methylimidazole, and use a catalyst for the reaction. The energy consumption of the reaction is high, and the production of imidazole is not conducive to the large-scale preparation of N-methylimidazole
Patent CN105348199 uses organic solvents for extraction, which does not conform to the concept of clean and green development and the process is complicated
In the patent CN105732508A, gas-phase catalytic reaction is used to prepare N-methylimidazole, which speeds up the reaction speed, but the risk of reaction also increases

Method used

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  • A New Efficient and Dynamic Synthesis and Purification Technology of N-Methylimidazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The high-efficiency dynamic N-methylimidazole purification new technology of the present embodiment, the steps are as follows:

[0024] (1) Add a certain amount of formaldehyde solution into the reaction device, turn on the circulating water bath of the reaction device, keep it at room temperature, and then add 40% methylamine solution and ammonia solution in turn, and the molar ratio of formaldehyde and 40% methylamine solution is 1:2.5 , the molar ratio of formaldehyde and ammonia water is 1:2, and stirring is started at room temperature. After stirring for 10 min, the glyoxal solution was slowly added, and the molar ratio of formaldehyde and glyoxal was 1:1.5. After the glyoxal solution was completely added, the temperature of the circulating water bath was raised to 50°C, and the reaction was carried out at this temperature for 5h;

[0025] (2) After the reaction is completed, the reaction device is connected to the vacuum condensation system, the temperature of th...

Embodiment 2

[0029] The high-efficiency dynamic N-methylimidazole purification new technology of the present embodiment, the steps are as follows:

[0030] (1) Add a certain amount of formaldehyde solution into the reaction device, turn on the circulating water bath of the reaction device, keep it at room temperature, and then add 40% methylamine solution and ammonia solution in turn, and the molar ratio of formaldehyde and 40% methylamine solution is 1:4 , the molar ratio of formaldehyde and ammonia water is 1:3, and stirring is started at room temperature. After stirring for 10 min, the glyoxal solution was slowly added, and the molar ratio of formaldehyde and glyoxal was 1:2. After the glyoxal solution was completely added, the temperature of the circulating water bath was raised to 70°C, and the reaction was carried out at this temperature for 3h;

[0031] (2) After the reaction, the reaction device was connected to the vacuum condensation system, the temperature of the circulating wa...

Embodiment 3

[0035] The high-efficiency dynamic N-methylimidazole purification new technology of the present embodiment, the steps are as follows:

[0036] (1) Add a certain amount of formaldehyde solution into the reaction device, turn on the circulating water bath of the reaction device, keep it at room temperature, and then add 40% methylamine solution and ammonia solution in turn, the molar ratio of formaldehyde and 40% methylamine solution is 1:1 , the molar ratio of formaldehyde and ammonia water is 1:1, and stirring is started at room temperature. After stirring for 10 min, the glyoxal solution was slowly added, and the molar ratio of formaldehyde and glyoxal was 1:1. After the glyoxal solution was completely added, the temperature of the circulating water bath was raised to 60°C, and the reaction was carried out at this temperature for 4h;

[0037] (2) After the reaction is completed, the reaction device is connected to the vacuum condensation system, the temperature of the circul...

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Abstract

The invention provides a new technology for the synthesis and purification of highly efficient and dynamic N-methylimidazole, adding methylamine, formaldehyde, ammonia water and glyoxal solution into a reaction kettle to react to obtain a crude product containing N-methylimidazole; into the distillation condensing system, the distilled product is condensed and recovered into the condensation collection tank; the crude product in the condensation collection tank flows into the rectification raw material tank, and the raw material tank is connected to the rectification tower for rectification, and the raw material concentration and N-methyl The concentration of the imidazole product is adjusted dynamically to adjust the operating conditions of the refining system, and the concentration of the obtained N-methylimidazole product is above 99%. The present invention improves and upgrades the traditional process, and has the characteristics of short process and simple process. Especially, in the refining system, the operating parameters are dynamically adjusted according to the product concentration, which not only reduces energy consumption, but also improves the purity of N-methylimidazole. The obtained N-methylimidazole can be used in fields such as pharmaceutical synthesis, ionic liquid synthesis, curing agent for epoxy resin and other resins.

Description

technical field [0001] The invention relates to the technical field of synthesis and purification technology, in particular to a new high-efficiency dynamic N-methylimidazole purification technology. Background technique [0002] N-Methylimidazole (scientific name: 1-Methylimidazole) Alias: 1-methyl-1H-imidazole, 1-methylimidazole, colorless to light yellow transparent liquid, mainly used for the synthesis of conventional imidazole ionic liquids, can also be used Curing agent for epoxy resins and other resins, and intermediates for organic synthesis. [0003] Ionic liquid is a new type of green and environmentally friendly solvent composed of anions and cations. It has many properties different from conventional solvents, such as non-volatile, wide liquid range, good thermal stability, strong solubility, and wide electrochemical window. In recent years, ionic liquids have been widely used in the fields of catalysis and separation, organic synthesis, material preparation, re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/58
CPCC07D233/58
Inventor 聂毅王斌琦郑双双马良玉吴文亮
Owner 郑州中科新兴产业技术研究院
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