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Production method of diisopropylethylamine

A technology of diisopropylethylamine and its production method, which is applied in the preparation of amino-substituting functional groups, purification/separation of amino compounds, organic chemistry, etc., can solve the problems of high production cost, limited development, low efficiency, etc., and achieve low cost, The effect of reducing production costs and simplifying the process flow

Active Publication Date: 2017-04-26
ZHEJIANG JIANYE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low yield and intermittent operation of this process, the production cost is high and the efficiency is low, which limits its further development

Method used

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  • Production method of diisopropylethylamine
  • Production method of diisopropylethylamine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1, a kind of production method of diisopropylethylamine, carry out following steps successively:

[0045]1) In a tubular reactor with an inner diameter of 8mm and a length-to-diameter ratio of 30:1, use a metering pump to inject DIPA and Et according to the proportion 2 SO 4 , Raw material ratio n(DIPA):n(Et 2 SO 4 )=1.25:1.0, the pressure is 0.6Mpa, and the liquid space velocity of the reaction material is 0.2h -1 (At this liquid space velocity, the residence time of the reactant in the tubular reaction device is 5 hours), and the reaction temperature is 125°C.

[0046] 2) The reacted material passes through the condenser at the outlet of the tubular reactor, and the cooling water volume of the condenser is controlled to control the temperature of the material at 35°C.

[0047] 3) The condensed material enters the stratifier, and there are two feeding ports in the middle of the stratifying device. One feeding port is a mixture of the condensed material a...

Embodiment 2

[0050] Embodiment 2, a kind of production method of diisopropylethylamine, carry out following steps successively:

[0051] 1) In a tubular reaction device with an inner diameter of 8mm and a length-to-diameter ratio of 100:1, use a metering pump to inject DIPA and Et at the same time according to the ratio 2 SO 4 , Raw material ratio n(DIPA):n(Et 2 SO 4 )=1.50:1.0, the pressure is 0.55Mpa, and the liquid space velocity of the reaction material is 0.4h -1 (At this liquid space velocity, the residence time of the reactants in the tubular reaction device is 2.5 hours), and the reaction temperature is 130°C.

[0052] 2) The reacted material passes through the condenser at the outlet of the reactor, and the cooling water volume of the condenser is controlled to control the temperature of the material at 45°C.

[0053] 3) The condensed material enters the layerer, and the middle part of the layerer is provided with two feeding ports, one feeding port is a mixture of the condens...

Embodiment 3

[0056] Embodiment 3, a kind of production method of diisopropylethylamine, carry out following steps successively:

[0057] 1) In a tubular reaction device with an inner diameter of 8mm and a length-to-diameter ratio of 100:1, use a metering pump to inject DIPA and Et 2 SO 4 , Raw material ratio n(DIPA):n(Et 2 SO 4 )=1.40:1.0, the pressure is 0.40Mpa, and the liquid space velocity of the reaction material is 0.3h -1 (At this liquid space velocity, the residence time of the reactants in the tubular reaction device is 3.3 hours), and the reaction temperature is 130°C.

[0058] 2) The reacted material passes through the condenser at the outlet of the reactor, and the cooling water volume of the condenser is controlled to control the temperature of the material at 50°C.

[0059] 3) The condensed material enters the stratifier, and there are two feeding ports in the middle of the stratifying device. One feeding port is a mixture of the condensed material and a strong alkali aqu...

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Abstract

The invention discloses a production method of diisopropylethylamine. The production method comprises the steps of simultaneously injecting diisopropylamine and diethyl sulfate into a tubular reactor to be subjected to reaction; putting the material flowing out of the tubular reactor after reaction into a condenser, and lowering the temperature to 30-50 DEG C; putting the material after condensation into a demixer, wherein the upper layer obtained after layering is an organic layer and the lower layer is an inorganic layer; injecting the organic layer into a first rectifying tower with pressure being 0.2-0.8 Mpa through a pump, using isopropylamine which is collected from the top of the first rectifying tower and is not totally reacted as a raw material, and leading the raw material into the tubular reactor to be subjected to reaction again; putting the material in the column bottom of the first rectifying tower into a second rectifying tower with pressure being 0-0.6 Mpa to be subjected to purification so as to obtain a product with boiling range being 126.5-127.0 DEG C, namely, diisopropylethylamine, wherein the material in the column bottom of the second rectifying tower is petroleum ether, and the petroleum ether is put back to the mixer to be recycled and used.

Description

technical field [0001] The present invention relates to a kind of production method of diisopropylethylamine (DIPEA). Background technique [0002] Diisopropylethylamine, also known as N-ethyldiisopropylamine, is an important pharmaceutical and pesticide intermediate, such as amino acid peptide synthesis, pharmaceutical anesthetics, pesticide herbicides, etc. [0003] According to literature reports, there are mainly four synthesis methods of DIPEA: [0004] (1) Patent CN101759571A reports a kind of reaction that takes diisopropylamine (DIPA) and ethyl chloride as raw materials to generate DIPEA. This reaction requires to carry out under the pressure of 0.4~2.5MPa, and product yield is about 95% (if operate with normal pressure, product yield is lower, and reaction time is long, and utilization ratio of ethyl chloride is low), generates a large amount of salts in addition, Subsequent processing is difficult and inconvenient to operate. [0005] (2) Patent WO2007137990A1 r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/08C07C209/22C07C209/86
CPCC07C209/22C07C209/86C07C211/08
Inventor 曹伟富余婉风陆旻强林萍刘尚文谈敦玲
Owner ZHEJIANG JIANYE CHEM