Preparation method of dibenzylamine

A technology of dibenzylamine and benzyl chloride, which is applied in the field of preparation of dibenzylamine, can solve the problems of high production raw material cost and difficult disposal of three wastes, and achieve the effects of reducing process safety hazards, less pollution, and high product yield

Active Publication Date: 2021-01-05
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The three wastes caused by the catalyst and solvent water (ethanol or methanol) used in this process are difficult to deal with, and the price of benzaldehyde as a raw material is much higher than that of benzyl chloride. The cost of raw materials is high under the same yield

Method used

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  • Preparation method of dibenzylamine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1. Make sure that there is no water in the autoclave, and then use the Roots vacuum pump to pump the autoclave to the maximum vacuum (-0.1MPa).

[0030] 2. Pump 100g of liquid ammonia into the reaction kettle through a high-pressure pump, then raise the temperature to 55°C and keep it warm.

[0031] 3. Quantitatively beat 297g of benzyl chloride into the reaction kettle through a high-pressure pump, set the finishing time to 35 minutes, control the temperature at 50-60°C throughout the process, and stop feeding when the pressure is close to 2.5MPa, and cool down to 50-55°C .

[0032] 4. After the benzyl chloride has been fed, continue to keep warm and stir for 20 minutes, then release the pressure to release the excess liquid ammonia in the reaction kettle, and then seal the reaction kettle.

[0033] 5. Vacuumize to a slight negative pressure, put 302g of liquid caustic soda (32% sodium hydroxide solution) into the reaction kettle, continue stirring at 50-60°C for 20 m...

Embodiment 2

[0037] 1. Make sure that there is no water in the autoclave, and then use the Roots vacuum pump to pump the autoclave to the maximum vacuum (-0.1MPa).

[0038] 2. Pump 100g of liquid ammonia into the reaction kettle through a high-pressure pump, then raise the temperature to 50°C and keep it warm.

[0039] 3. Quantitatively beat 297g of benzyl chloride into the reaction kettle through a high-pressure pump, set the finishing time to 35 minutes, control the temperature at 50-60°C throughout the process, and stop feeding when the pressure is close to 2.5MPa, and cool down to 50-55°C .

[0040] 4. After the benzyl chloride has been fed, continue to keep warm and stir for 20 minutes, then release the pressure to release the excess liquid ammonia in the reaction kettle, and then seal the reaction kettle.

[0041] 5. Vacuumize to a slight negative pressure, put 302g of liquid caustic soda (32% sodium hydroxide solution) into the reaction kettle, continue stirring at 50-60°C for 20 m...

Embodiment 3

[0045] 1. Make sure that there is no water in the autoclave, and then use the Roots vacuum pump to pump the autoclave to the maximum vacuum (-0.1MPa).

[0046] 2. Pump 100g of liquid ammonia into the reaction kettle through a high-pressure pump, then raise the temperature to 58°C and keep it warm.

[0047] 3. Quantitatively beat 297g of benzyl chloride into the reaction kettle through a high-pressure pump, set the finishing time to 35 minutes, control the temperature at 50-60°C throughout the process, and stop feeding when the pressure is close to 2.5MPa, and cool down to 50-55°C .

[0048] 4. After the benzyl chloride has been fed, continue to keep warm and stir for 20 minutes, then release the pressure to release the excess liquid ammonia in the reaction kettle, and then seal the reaction kettle.

[0049] 5. Vacuumize to a slight negative pressure, put 302g of liquid caustic soda (32% sodium hydroxide solution) into the reaction kettle, continue to stir at 50-60°C for 20 mi...

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PUM

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Abstract

The invention discloses a preparation method of dibenzylamine, which comprises the following steps: vacuumizing a reaction kettle until the reaction kettle is completely dewatered, then conveying liquid ammonia into the reaction kettle, heating, adding benzyl chloride into the reaction kettle, and reacting to obtain dibenzylamine; and after the reaction is finished, separating excessive liquid ammonia, adding liquid caustic soda into the reaction kettle for replacement reaction, separating out ammonia gas generated after replacement, separating liquid from the remaining material, and carryingout rectification to purify the dibenzylamine. In the invention, the low-cost raw material benzyl chloride is used for production and no catalyst or other solvent is used, so that the production costis greatly reduced, pollution is small, energy conservation and environmental protection are achieved, and the policy requirements of national green chemical engineering are met.

Description

technical field [0001] The invention relates to a preparation method of dibenzylamine, in particular to a preparation method of dibenzylamine with low cost, less time consumption, high degree of automation and simple operation, belonging to the technical field of fine chemicals. [0002] technical background [0003] Dibenzylamine, also known as benzhydrylamine and N-benzylbenzylamine, is an important intermediate in organic synthesis. Since dibenzylamine does not derive any carcinogenic nitrosamines, it is widely used in the synthesis of penicillin, linezolid and other drugs. At the same time, dibenzylamine can be used to produce highly efficient and non-toxic vulcanization accelerator dibenzyl Zinc dithiocarbamate (ZBEC) and tetrabenzylthiuram disulfide (TBzTD), and can be used for the determination of cobalt, iron, cyanate, etc. [0004] At present, the production methods of dibenzylamine mainly include benzyl chloride method and benzaldehyde method. The former is a trad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/08C07C211/27
CPCC07C209/08C07C211/27
Inventor 徐思明孟祥克王克军黄存影左秀娟李庆朝董玉标郭本凯
Owner SHANDONG YANGGU HUATAI CHEM
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