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A kind of method of directly synthesizing methyl phenylcarbamate by aniline and urea

A technology of methyl phenylcarbamate and urea, which is applied in the field of synthesis of methyl phenylcarbamate, can solve the problems of low degree of automation, high energy consumption, high cost, etc., achieve simplified operation process, overcome product yield, and be conducive to industrialization The effect of promotion

Active Publication Date: 2019-05-10
陕西煤业化工技术开发中心有限责任公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] Therefore, the technical problem to be solved in the present invention is to overcome the low degree of automation of the synthesis process of methyl phenylcarbamate in the prior art, high energy consumption, and high defects such as high cost, thereby providing a benzene with simple operation process and continuous production. The synthetic method of methyl carbamate

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  • A kind of method of directly synthesizing methyl phenylcarbamate by aniline and urea

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Experimental program
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Effect test

Embodiment 1

[0026] 42.4g of urea and 157.6g of aniline were added to a 1L high-pressure reaction separation device for reaction. After the reaction, 138.7g of reaction product A was collected. The reaction product A was analyzed by HPLC to obtain the mass percentage of each component. Phenylurea is 22.7%, diphenylurea is 71.8%, aniline is 5.1%, aniline oxide and ammonium carbonate are less than 0.1%; 90g methanol is weighed into the above reaction product A and mixed uniformly, and then 300g chlorobenzene is added , The reaction device was sealed, and nitrogen gas with a flow rate of 200 ml / min was introduced into it, and the pressure of the reaction device was controlled to 2.3 MPa and heated to 175°C. Stay at 175°C for 40 minutes, stop heating, and cool down naturally to room temperature. Finally, open the device and collect 268.5g of reaction product B. Perform high performance liquid phase analysis on reaction product B. The content of each component in the product is monophenylurea. U...

Embodiment 2

[0029] 60.0g of urea and 204.6g of aniline were added to the 1L high-pressure reaction separation device for reaction. After the reaction, 189.5g of reaction product A was collected. The reaction product A was analyzed by high performance liquid phase, and the mass percentage of monophenylurea was 28.7% , The mass percentage of diphenylurea is 66.8%, and the mass percentage of aniline is 4.3%. Weigh 63.8g of methanol and add it to the above reaction product A and mix evenly, then add 300g of o-dichlorobenzene, seal the reaction device, pass nitrogen gas at a flow rate of 10ml / min into it, and control the pressure of the reaction device to 2.5MPa, And heated to 175°C. Stay at 175°C for 40 minutes, stop heating, and naturally cool to room temperature. Finally, open the device and collect 548.3g of reaction product B. The reaction product B is analyzed by HPLC. Among them, monophenylurea and diphenylurea are undetectable. Urea accounted for 0.21%, methyl phenylcarbamate accounted...

Embodiment 3

[0032] 50.0 g of urea and 186.0 g of aniline were added to a 1L high-pressure reaction separation device for reaction. After the reaction, 174.2 g of reaction product A was collected, and the reaction product A was analyzed by high performance liquid phase to obtain the mass percentage of each component. Weigh 40.0g of methanol and add it to the above reaction product A and mix well, then add 200g of diethyl phthalate, seal the reaction device, and pass nitrogen gas with a flow rate of 600ml / min into it, and control the pressure of the reaction device It is 4MPa and heated to 200°C. Stay at 200°C for 20 minutes, stop heating, and cool down naturally to room temperature. Finally, open the device and collect 408.9g of reaction product B. Perform high-performance liquid phase analysis on reaction product B to obtain the content of each component in the product, including monophenylurea Undetectable, diphenylurea accounts for 0.23%, methyl phenylcarbamate accounts for 29.21%, anili...

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Abstract

The invention provides a method for directly synthesizing phenyl carbamate with aniline and urea. The method includes: 1), mixing a product generated from reaction of the urea and the aniline with methyl alcohol to form a reaction mixture; 2), mixing the reaction mixture with an organic solvent to form a reaction system; 3), under protection of inert gases, controlling pressure to be MPa, heating the reaction system to be 120-210DEG C and sustaining for 10-300 minutes to obtain a crude product of the phenyl carbamate; 4), performing separation on the crude product of the phenyl carbamate to obtain the phenyl carbamate. With the method, synthesizing process can be performed continuously, uninterrupted production is realized, and industrialized promotion is facilitated.

Description

Technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing methyl phenylcarbamate. Background technique [0002] Isocyanates are important intermediates in organic synthesis. For example, monoisocyanates can be made into a series of carbamate insecticides, fungicides, herbicides, etc., and polyisocyanates with difunctional groups and above can be used to synthesize a series of polyurethane foams with excellent properties Plastics, rubber, elastic fibers, coatings, adhesives, synthetic leather, artificial wood, etc., among which aromatic polyisocyanates are particularly important, and have been widely used in synthetic leather, fibers, coatings and plastics. In recent years, with the domestic automobile, With the development of leather and construction industries, the market demand for related accessories has increased, making the demand for aromatic polyisocyanates rapidly expanding. [0003] Polyisocyanate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C269/04C07C271/28
CPCC07C269/04C07C271/28
Inventor 李会泉王利国陈家强贺鹏贾中宝龙世良曹妍
Owner 陕西煤业化工技术开发中心有限责任公司
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