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Method for separating mixture of diisopropylamine and ethanol through azeotropic distillation

A diisopropylamine, azeotropic distillation technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve problems such as inability to separate, low relative volatility, difficult recovery of diisopropylamine raw materials, etc. Achieve the effect of convenient recycling, reduce secondary investment, and reduce energy consumption

Active Publication Date: 2021-03-05
QUZHOU RES INST OF ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Diisopropylamine (boiling point 84°C) and ethanol (boiling point 78.5°C) do not azeotrope under normal pressure, but due to the close boiling point of the two and the formation of hydrogen bonds, the relative volatility is low. separation of the two
As a result, it is difficult to recycle some diisopropylamine raw materials, which undoubtedly increases the operating cost of the enterprise
At present, there is no report on the separation of diisopropylamine and ethanol

Method used

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  • Method for separating mixture of diisopropylamine and ethanol through azeotropic distillation
  • Method for separating mixture of diisopropylamine and ethanol through azeotropic distillation
  • Method for separating mixture of diisopropylamine and ethanol through azeotropic distillation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-1

[0060] Example 1-1, a method for separating diisopropylamine and ethanol by azeotropic distillation, for the mixed solution I after water removal, the batch rectification process is adopted in the first case,

[0061] Device 1 is used, the shut-off valve 21 and the shut-off valve 28 are both closed, that is, the toluene tank 4 and the extraction tower 10 are not used in the embodiment 1-1.

[0062] details as follows:

[0063] After 360g of water-removed mixed solution I was mixed with 100g of toluene as an entrainer, they were added together to the bottom of the batch rectification tank 1, and the total reflux until the temperature at the top of the tower was stable (that is, the displayed temperature at the temperature measuring point 3 on the top of the tower was 66~67℃), then start to extract the distillate, and then go to the azeotrope collection tank 6 after being condensed by the condenser 5. The volume ratio of collection tank 6=5:1); When the ethanol concentration dr...

Embodiment 1-2

[0071] Embodiment 1-2, the fraction collected in the excess fraction tank 7 and the next batch of mixed solution I after water removal are combined and rectified, as follows:

[0072] Mix the fraction 103g and 248g of the fraction collected in the transition fraction collection tank 7 obtained in Example 1-1 and 248g of the mixed solution I after water removal, and then add 109g of the bottom liquid of the batch distillation still 1 obtained in Example 1-1 to mix; The method described in above-mentioned embodiment 1-1 is carried out, and gained result is as follows table 2:

[0073] Table 2

[0074]

Embodiment 2

[0075] Example 2. The amount of toluene was changed from 100 g to 144 g, that is, the mass ratio of entrainer: mixed solution I after water removal = 0.4:1; the rest was the same as in Example 1-1. The final result is: about 120 g of 99% diisopropylamine is obtained, and the secondary recovery rate reaches 88.1%.

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Abstract

The invention discloses a method for separating a mixture of diisopropylamine and ethanol by azeotropic distillation. According to the method, the mixture of diisopropylamine and ethanol taken as a raw material is a mixed solution mainly composed of diisopropylamine and ethanol and containing a small amount of water, firstly dehydration treatment is conducted on the mixed solution until a dewatered mixed solution with the water content of less than 1% is obtained; and a azeotropic agent and the dewatered mixed solution are rectified in an azeotropic rectification tower by adopting a batch rectification method or a three-tower continuous rectification method, and ethanol in the dewatered mixed solution is entrained out by the azeotropic agent, so that the aim of separating diisopropylamineand ethanol is fulfilled, wherein the azeotropic agent is toluene. According to the invention, water is used as an extractant to recover toluene, so addition of additional third components for separation and recovery of toluene is avoided, and energy consumption is reduced.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a method for separating diisopropylamine and ethanol through azeotropic distillation. Background technique [0002] Diisopropylamine, a colorless liquid at room temperature, with a boiling point of 84°C, has a stimulating ammonia smell, is miscible with water, and can be dissolved in most organic solvents; it is an important raw material for the production of fine chemicals such as pesticides, medicines, dyes, and emulsifiers. , especially one of the important raw materials for the production of non-nucleophilic amine base N,N-diisopropylethylamine. Ethanol, a colorless transparent liquid at room temperature, with a boiling point of 78.5°C, is the most widely used alcohol, and is an important organic synthesis raw material and organic solvent. [0003] During the industrial production of DIPEA (N,N-diisopropylethylamine, referred to as diisopropylethylamine), a mixed solution conta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/86C07C211/06C07C29/82C07C31/08
CPCC07C209/86C07C29/82C07C211/06C07C31/08
Inventor 钱超洪增阮建成周少东陈新志
Owner QUZHOU RES INST OF ZHEJIANG UNIV
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