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Method for synthesizing N-methyl carbamate

A technology of methyl carbamate and methanol, which is applied in the preparation of carbamic acid derivatives, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of environmental protection treatment of invalid catalysts, increase production costs, and affect product purity, etc. problems, achieve good commercial value, reduce the trouble of separation process, and improve the effect of production safety

Pending Publication Date: 2021-02-26
安徽长华化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the above methods, the raw material 1,3-dimethylurea used is not easy to obtain, and a catalyst needs to be used in the reaction. The invalid catalyst should be treated as solid waste according to the current environmental protection laws and regulations, which has a certain impact on environmental protection.
In addition to increasing production costs, filtration and separation are required for subsequent treatment. Poor separation will also affect product purity, and environmental protection treatment of spent catalysts is difficult.

Method used

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  • Method for synthesizing N-methyl carbamate

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Add 60g (1mol) urea and 300g methanol to a 1L high-pressure reactor with an alcohol ammonia separator, seal the reactor, fill the reactor with nitrogen to 0.6MPa, discharge to 0.1MPa, replace 4 times continuously, and keep the last time 0.1 MPa nitrogen residual pressure.

[0017] After checking that the valves of the reaction kettle and the alcohol and ammonia separator are in the correct position, turn on the agitator (100-200 rpm), turn on the electric heating system, and raise the temperature of the material to 220°C at a heating rate of 3-4°C / min , the equilibrium pressure at this temperature is 5.92MPa. After maintaining the temperature for 15 minutes, methanol, ammonia, and carbon dioxide are separated by the alcohol ammonia separator, and the methanol is returned to the reactor. The ammonia and carbon dioxide generated by the reaction are continuously discharged from the reaction system and introduced into the absorption device.

[0018] When the temperature of...

Embodiment 2

[0021] Other processing conditions are with embodiment 1, and the raw material that adds and temperature of reaction are as follows:

[0022] Add 60 g of urea and 300 g of methanol, and the reaction temperature is 240° C. to obtain 61.9 g of the product.

Embodiment 3

[0024] Other processing conditions are with embodiment 1, and the raw material that adds and temperature of reaction are as follows:

[0025] Add 60 g of urea and 390 g of methanol, and the reaction temperature is 220° C. to obtain 58.5 g of the product.

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Abstract

The invention discloses a method for synthesizing N-methyl carbamate, and relates to the technical field of chemical synthesis of fine chemical products. The method comprises the following steps: in an atmosphere with nitrogen in a reaction kettle, mixing urea and excessive methanol to react, after the reaction is finished, performing cooling, relieving pressure, removing reactants, recovering methanol, performing distilling, collecting a distillation section at 167-168 DEG C, and obtaining the Nmethyl carbamate. The method has the advantages of high conversion rate, accessible raw materials,simple flow, high raw material conversion rate, favorable product selectivity and favorable commercial value of byproducts, and does not use any catalyst in the preparation process, thereby reducing the trouble of the subsequent separation procedure and enhancing the production safety.

Description

technical field [0001] The invention relates to the technical field of synthesis of methyl N-methyl carbamate. Background technique [0002] N-Methyl carbamate is an important fine chemical product. In the pesticide industry, it can be used as a raw material for the production of a variety of high-efficiency and low-toxicity carbamate pesticides; in medicine, it can be used as a raw material for the synthesis of the antithrombotic drug riociguat; it can be used in the lithium battery industry to develop liquid electrolytes and gel electrolytes; It is also widely used in chemical industry and paint industry. [0003] At present, the product is still in the development stage in China, and the synthesis methods recorded in the published literature mainly include: [0004] Method 1: Chinese Invention Patent Application Publication No. CN103524381A, using dimethyl carbonate and 1,3-dimethylurea as raw materials, mixing them at a molar ratio of 15 to 1:1, and using dibutyltin ox...

Claims

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Application Information

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IPC IPC(8): C07C269/00C07C269/08C07C271/12
CPCC07C269/00C07C269/08C07C271/12
Inventor 仲力
Owner 安徽长华化工有限公司
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