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Method for producing beta-hydroxyethyl ethylenediamine

A technology of hydroxyethylethylenediamine and ethylenediamine, which is applied in the field of using microreactor technology to carry out the process, can solve the problems of high energy consumption, high feed ratio, large liquid reflux and the like

Active Publication Date: 2012-11-21
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problems of high feed ratio of ethoxylation reactor, large liquid return flow and high energy consumption, and provide a micro-reactor technology for ethoxylation, especially for the micro-reactor of β-hydroxyethylethylenediamine. Reaction Technology Synthesis

Method used

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  • Method for producing beta-hydroxyethyl ethylenediamine
  • Method for producing beta-hydroxyethyl ethylenediamine
  • Method for producing beta-hydroxyethyl ethylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Use two Series II digital pumps (Chrom Tech, Inc.) to control the output of ethylenediamine liquid and ethylene oxide liquid respectively, and the ethylene oxide liquid enters the microchannel steam vaporizer after passing through the back pressure valve with a back pressure of 0.3MPa Gasification, after gasification, it is synchronously and continuously input into the microreactor for reaction with ethylenediamine liquid.

[0024] Microreactor: CNC precision machining preparation

[0025] Micropore diameter 0.3mm, quantity 5, vertical spacing 4.5mm

[0026] Micron mixing channel 0.4mm wide and 0.4mm deep

[0027] Effective volume 230μl

[0028] Process conditions: Microreactor temperature control 100°C

[0029] Ambient temperature 12°C

[0030] reaction pressure normal pressure

[0031] Ethylenediamine digital pump flow rate 4.00ml / min

[0032] EO flow setting is 0.50ml / min, the actual output is 0.33ml / min

[0033] The molecular ratio of feed ethylenediamine to ...

Embodiment 2

[0045] The process is the same as example 1.

[0046] Microreactor: same as example 1

[0047] Process conditions: Microreactor temperature control 100°C

[0048] Ambient temperature 12°C

[0049] reaction pressure normal pressure

[0050] Ethylenediamine digital pump flow rate 3.30ml / min

[0051] EO flow setting is 0.50ml / min, the actual output is 0.33ml / min

[0052] The molecular ratio of feed ethylenediamine to ethylene oxide is 7.5:1

[0053] EO consumption rate 75,000 kg·h -1 m -3

[0054] Curing temperature and time: 65-75°C, 2, 5, 10, 20 minutes

[0055] Analysis conditions: same as example 1

[0056] Implementation result: (if no description is mass concentration, other implementations are the same) microreactor outlet ethylene oxide conversion rate 25.3%, main product hydroxylamine 5%, high boiling 0; 65-75 ℃, aging 2, 5, 10, After 20 minutes, the conversions of ethylene oxide were 58.1%, 76.1%, 93.0%, 98.6%, β-hydroxyethylethylenediamine 10.6, 14.7, 20.2, 2...

Embodiment 3

[0058] The process is the same as example 1.

[0059] Microreactor: same as example 1

[0060] Process conditions: Microreactor temperature control 100°C

[0061] Ambient temperature 12°C

[0062] reaction pressure normal pressure

[0063] Ethylenediamine digital pump flow rate 6.60ml / min

[0064] EO flow setting is 0.50ml / min, actual output is 0.38ml / min

[0065] Feed ethylenediamine and ethylene oxide molecular ratio 13.2:1

[0066] EO consumption rate 86,000 kg·h -1 m -3

[0067] Curing temperature and time: 90-100°C, 2, 5, 10 minutes

[0068] Analysis conditions: same as example 1

[0069] Implementation results: (if no description is mass concentration, other implementations are the same) microreactor outlet ethylene oxide conversion rate 16.6%, main product hydroxylamine 2%, high boiling 0; 90-100 ° C, after aging for 2, 5, and 10 minutes , The conversion of ethylene oxide was 47.3%, 87.9%, 96.5%, respectively, β-hydroxyethylethylenediamine was 5.55, 10.88, 12....

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Abstract

The invention relates to a method for producing beta-hydroxyethyl ethylenediamine. The method comprises the following steps that an ethylenediamine liquid and ethylene oxide gas are continuously and synchronously input into a microreactor and undergo a reaction; and an effluent from the microreactor is subjected to heat preservation at a temperature of 50 to 140 DEG C for 2 to 30min, wherein a reaction temperature in the microreactor is in a range of 10 to 115 DEG C; a mole ratio of ethylenediamine to ethylene oxide is (5 to 15): 1; and an ethylene oxide airspeed is 4 to 400000kg.h<-1>.m<-3>. Under the optimal conditions, ethylene oxide is fully transformed; beta-hydroxyethyl ethylenediamin discharged from the microreactor has a concentration of 5 to 20%; and the content of beta-hydroxyethyl ethylenediamin in products obtained by ethanediamine separation is above 95%. Compared with the prior art, the method has the advantages that a ratio of ethanediamine to ethylene oxide is lower; a production capacity is improved; a reaction period is short; and by-products are reduced.

Description

Technical field: [0001] The invention relates to a method for producing β-hydroxyethylethylenediamine by ethoxylation of ethylenediamine, in particular to a method for carrying out the process by adopting micro-reactor technology. Background technique: [0002] The ethoxylation reaction of organic amines is a typical gas-liquid phase contact reaction, and the rate of side reactions in series is very high, requiring no back-mixing in the reactor and a large gas-liquid contact area. At present, more advanced ethoxylation reactors have BUSS loops Reactor and Press circulation spray reactor, as well as tubular reactor, the first two have high mass transfer efficiency, no back mixing, and the consumption rate of ethylene oxide per cubic meter of reactor reaches 1200-1500kg·h -1 , the tubular reactor is close to plug flow, the reaction speed is fast, the residence time is short, and the EO consumption reaches 5000-10000kg h -1 m -3 . The ethoxylation of ethylenediamine to synth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/14C07C213/04
Inventor 陈光文陈毅征焦凤军
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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