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Method for separating N-ethylpiperazine-ethanolamine azeotropic mixture by azeotropic rectifying intermittent operation

A technology of azeotropic mixture and ethylpiperazine, which is applied in the field of separation of N-ethylpiperazine-ethanolamine, can solve problems that have not been seen yet, and achieve the effect of less equipment investment and flexible operation

Inactive Publication Date: 2008-05-14
TIANJIN UNIV
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  • Method for separating N-ethylpiperazine-ethanolamine azeotropic mixture by azeotropic rectifying intermittent operation

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Embodiment 1

[0010] The intermittent azeotropic distillation device is adopted, the diameter of the azeotropic distillation column is φ25mm, and the internal packing of φ2.5×2.5θ mesh ring is installed, and the height of the packing layer is 1.1m. Put 500ml of N-ethylpiperazine-ethanolamine mixture (wherein N-ethylpiperazine 88%, 12%, both are mass percentages) in heating kettle, then add cyclohexane 250ml. Turn on the heat source of the heating kettle and the cold source of the condenser, and the azeotropic distillation column starts to operate, and the liquid condensed by the condenser connected to the azeotropic distillation column enters the phase separator for phase separation, the light phase is refluxed, and the heavy phase is extracted; when the phase is separated When the liquid in the device is basically not separated into phases, the phase separator is isolated, and part of the condensed liquid is directly refluxed into the azeotropic distillation column, and part of it is extrac...

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Abstract

The invention relates to a method using discontinuous azeotropic rectifying operation to separate the N-ethylpiperazine-ethanolamine azeotropic mixture, which adopts the rectifying device and discontinuous operation to add the cyclohexane entrainer and the raw material into the heating kettle. Under the atmospheric pressure condition, when the temperature of the azeotropic rectifying tower head is between 79 and 81 DEG C, the condensate enters into the phase splitter for splitting the phase; the cyclohexane reflows to the azeotropic rectifying tower; the ethanolamine is adopted; when the temperature of the azeotropic rectifying tower head is between 82 and 154 DEG C, the transition fraction with the reflux ratio of 3:1 to 6:1 is adopted and is circulated for use to rectify the next batch of material; and when the temperature of the azeotropic rectifying tower head is between 155 and 157 DEG C, the N-ethylpiperazine with the reflux ratio of 1:2 to 1:1 is extracted. The invention has the advantages that: the entrainer and the ethanolamine form the lowest heterogeneous azeotrope to destroy the N-ethylpiperazine-ethanolamine azeotropic system and the separated N-ethylpiperazine product purity can reach 99%.

Description

technical field [0001] The invention relates to a method for separating N-ethylpiperazine-ethanolamine azeotropic mixture by intermittent operation of azeotropic rectification, which belongs to the separation technology of N-ethylpiperazine-ethanolamine. Background technique [0002] N-ethylpiperazine (NEP) has important applications in pharmaceutical and organic synthesis as pharmaceutical intermediates and fine chemicals. The main purpose is to synthesize anthrafloxacin, synthetic dyes and raw materials for plant protection agents. In the process of synthesizing piperazine and co-producing N-ethylpiperazine, there will be impurity ethanolamine. Since N-ethylpiperazine and ethanolamine will form an azeotrope that is difficult to separate, it needs to be separated by special rectification technology. The present invention The azeotropic mixture of N-ethylpiperazine-ethanolamine was separated by azeotropic distillation. There are no reports about this technology yet. Cont...

Claims

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Application Information

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IPC IPC(8): C07D295/03C07D295/023
Inventor 崔现宝冯天扬张缨杨志才孙国秀
Owner TIANJIN UNIV
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