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A pollution-free purification method for high-purity piperidine

A purification method and a technology of high-purity piperidine, which is applied in the field of pollution-free purification of high-purity piperidine, can solve the problems of piperidine influence, clean separation of raw material pyridine, etc., and achieve the effect of low pyridine content and high purity

Active Publication Date: 2020-07-21
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Piperidine is generally reduced from pyridine, because piperidine and pyridine are basic compounds with similar molecular weight and boiling point, it is difficult to separate the raw material pyridine by the usual rectification method; so the content of pure piperidine in the chemical standard is ≥98.0 %, while pyridine is ≤1.0%, so it will affect the use of piperidine in some applications

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  • A pollution-free purification method for high-purity piperidine

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Embodiment 1

[0018] Example 1: This example specifically relates to a pollution-free purification method of high-purity piperidine, which uses melt crystallization to remove pyridine with similar molecular weight and similar properties in the piperidine solution to obtain high-purity, low-pyridine content of piperidine.

[0019] The physical and chemical properties of material piperidine and pyridine are introduced as follows:

[0020] Piperidine is a colorless liquid with a pepper-like smell and soapy feel. It is hygroscopic and volatilizes with water vapor. It is strongly alkaline and sensitive to carbon dioxide. It is miscible with water and soluble in ethanol, ether, benzene and Chloroform; relative density (d204) 0.8622, melting point -7°C, boiling point 106°C, refractive index (n20D) 1.4534, flash point 16°C; flammable; low toxicity, median lethal dose (rat, oral) 0.52ml / kg , irritating.

[0021] Pyridine is a colorless liquid with foul smell and strong irritating taste; it is hygr...

Embodiment 2

[0029] Embodiment 2: This embodiment specifically relates to a pollution-free purification method of high-purity piperidine, which specifically includes the following steps:

[0030] (1) In order to avoid quality degradation caused by moisture absorption, under the protection of nitrogen, using industrial products as raw materials, put 800g of chemically pure piperidine (content 97.4%, pyridine 1.5%) in a place equipped with stirring, low-temperature cooling bath, temperature display, In the 1 liter reaction bottle of condenser, obtain initial piperidine mother liquor;

[0031] (2) First-stage crystallization: Slowly cool the piperidine mother liquor to -6.8°C and keep it warm, add seed crystals to it to crystallize under continuous stirring, keep warm and crystallize for 45 minutes, and then remove the piperidine in the reaction bottle The mother liquor is subjected to centrifugal solid-liquid separation operation, so that the piperidine crystals are separated from the piperi...

Embodiment 3

[0035] Embodiment 3: This embodiment specifically relates to a pollution-free purification method of high-purity piperidine, which specifically includes the following steps:

[0036] (1) In order to avoid quality degradation caused by moisture absorption, under the protection of nitrogen, put 800g of raw material chemically pure piperidine (content 98.2%, pyridine 0.9%) in a 1-liter reactor equipped with stirring, low-temperature cooling bath, temperature display, and condenser In the bottle, obtain initial piperidine mother liquor;

[0037] (2) First-stage crystallization: Slowly cool the piperidine mother liquor to -6°C and keep it warm, add seed crystals to it to crystallize under continuous stirring, keep warm and crystallize for 60 minutes, and then remove the piperidine in the reaction bottle The mother liquor is subjected to centrifugal solid-liquid separation operation, so that the piperidine crystals are separated from the piperidine mother liquor; the isolated crysta...

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Abstract

The present invention discloses a pollution-free purification method of high-purity piperidine. The purification method comprises: under the protection of nitrogen, placing piperidine in a reaction container to carry out multi-stage melting crystallization to remove the pyridine having the similar molecular weight and the similar property so as to prepare the high-purity and low-pyridine content piperidine in a high-selectivity and high-yield manner. According to the present invention, the purification method has the following advantages that the solvent is not used, the high energy consumption rectification way is not used, the piperidine main body multi-stage melting crystallization green process is used, the high-purity and low-pyridine content piperidine is prepared by controlling the temperature and the stirring time in the convenient and efficient purification manner, and the three waste are not generated.

Description

technical field [0001] The invention belongs to the technical field of chemical purification, and in particular relates to a pollution-free purification method of high-purity piperidine. Background technique [0002] Piperidine is a colorless liquid and is an important domestic organic chemical product. It has a wide range of applications. It can be used as an analytical reagent, a common amine curing agent for epoxy resins, and a rubber vulcanization accelerator. It can also be used as an analgesic, It can be used as a raw material for fungicides, wetting agents, and local anesthetics. It can also be used as a solvent for spinning polyacrylonitrile, a solvent for organic synthesis, a catalyst for the reaction between active methylene and aldehyde, a catalyst for olefin polymerization, and a preservative for steam equipment. And stabilizers of diazo amino compounds for synthetic fiber dyeing. [0003] Piperidine is generally reduced from pyridine, because piperidine and pyr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/023C07D295/027
Inventor 郭建国顾小焱曹丽丽柯德宏
Owner SINOPHARM CHEM REAGENT
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