Process for synthesizing N-ethyl piperazidine

A synthesis method, the technology of ethylpiperazine, is applied in the field of synthesis of N-ethylpiperazine, which can solve the problems of process control, three wastes treatment difficulty, many by-products, and many reaction steps, and achieve three wastes treatment difficulty, demanding effects

Active Publication Date: 2007-05-16
ZHEJIANG XINHUA CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the reaction temperature is high, resulting in high equipment requirements; there are many reaction steps and equipment and instruments, resulting in great difficulty in process control and three waste treatment; poor catalyst selectivity, low conversion rate, and many by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Embodiment 1: adjust the high-speed stirrer of 5L stainless steel autoclave, measure (control) temperature system, pressure gauge, safety valve etc., with nitrogen the autoclave is replaced to 0 2 ≤0.5%, add 260 grams of anhydrous piperazine (purity 99.5%), 4.5 grams of 1# catalyst, and 46 grams of absolute alcohol at one time, wherein the composition of 1# catalyst (wt%): Cu: 1.0%, Co: 1.0 %, Mo: 2.5%, Ni: 1.0%, Mn: 0.5%, Mg: 0.1%, Cr: 0.05%, and the rest is Al 2 o 3 . After passing the replacement with hydrogen, use hydrogen to raise the pressure in the kettle to 3.0MP a , close the hydrogenation valve. Turn on stirring and heating up, the temperature is controlled at 190-210°C, and the ammonia pressure is controlled at 6.0MP a Inside. During the reaction, the temperature will rise obviously, and the heat generated by the reaction should be removed in time. React for 3 hours, lower the temperature, release the pressure, take out the reactant, and filter to obtai...

Embodiment 2

[0011] Embodiment 2: add 85 grams of anhydrous piperazine, other are with embodiment 1.

Embodiment 3

[0012] Embodiment 3: add 420 grams of anhydrous piperazine, react for 2 hours, other is the same as embodiment 1.

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PUM

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Abstract

The invention discloses a synthesizing method of N-ethyl piperazine, which comprises the following steps: adopting Cu-Co-M0 / Al2O3 as catalyst with 1-70% Cu, 1-90% Co,1-30% Mo, 0.1-10% Ni, 0.05-10% Mn, 0.01-5.0% Mg, 0.01-5.0% Cr and Al2O3; setting the pressure of liquid phase at 0.1-10.0Mpa under 80-350 Deg C in the interval course with surplus piperazidine; making the molar rate of piperazidine and alcohol at 0.5-10.0 with 0.1-5.0% catalytic cracking quantity.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a synthesis method of N-ethylpiperazine using ethanol and piperazine as raw materials. Background technique [0002] N-Ethylpiperazine is one of piperazine series products. It is an important fine chemical and an intermediate in synthetic medicine and synthetic pesticide. It is mainly used in the synthesis of ethyl ciprofloxacin antibacterial drugs. It is used as a synthetic raw material for dyes and plant protection agents, and is also widely used in fungicides and surfactants. The product is still in the development stage in China, and its consumption mainly depends on imports. There are mainly two kinds of synthetic methods recorded in the known literature: [0003] Method 1: Synthesis from piperazine: piperazine reacts with acetonitrile, acetaldehyde or ethyl bromide. The method of synthesizing N-ethylpiperazine by reacting piperazine and bromoe...

Claims

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Application Information

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IPC IPC(8): C07D295/03B01J23/885
Inventor 陈国建谢自强刘训军
Owner ZHEJIANG XINHUA CHEM
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