Method for producing beta-hydroxyethyl ethylenediamine

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

Active Publication Date: 2014-06-04
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] Two Series II digital pumps (Chrom Tech, Inc.) are used to control the output of ethylenediamine liquid and ethylene oxide liquid respectively. The ethylene oxide liquid enters the microchannel vaporizer after passing through the back pressure valve and back pressure of 0.3MPa After gasification, it is synchronously and continuously input into the microreactor to react with the ethylenediamine liquid after gasification.

[0024] Microreactor: CNC precision machining preparation

[0025] The pore diameter is 0.3mm, the number is 5, the vertical spacing is 4.5mm

[0026] Micron-level mixing channel is 0.4mm wide and 0.4mm deep

[0027] Effective volume 230μl

[0028] Process conditions: micro-reactor temperature control 100℃

[0029] Environment temperature 12℃

[0030] Reaction pressure

[0031] Digital pump flow rate of ethylenediamine 4.00ml / min

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

[0033] Feed ethylenediamine and ethylene oxide molecular ratio 9...

Embodiment 2

[0045] The process is the same as in Example 1.

[0046] Micro reactor: same as example 1

[0047] Process conditions: micro-reactor temperature control 100℃

[0048] Environment temperature 12℃

[0049] Reaction pressure

[0050] Digital pump flow rate of ethylenediamine 3.30ml / min

[0051] EO flow setting is 0.50ml / min, 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℃, 2, 5, 10, 20min

[0055] Analysis condition: same as example 1

[0056] Implementation results: (If there is no description, it is the mass concentration, other implementations are the same) The conversion rate of ethylene oxide at the outlet of the microreactor is 25.3%, the main product hydroxylamine is 5%, high boiling point 0; 65-75℃, maturation 2, 5, 10, After 20 minutes, the ethylene oxide conversion was 58.1%, 76.1%, 93.0%, 98.6%, β-hydroxyethylethylenediamine 10.6, ...

Embodiment 3

[0058] The process is the same as in Example 1.

[0059] Microreactor: same as example 1

[0060] Process conditions: micro-reactor temperature control 100℃

[0061] Environment temperature 12℃

[0062] Reaction pressure

[0063] Digital pump flow rate of ethylenediamine 6.60ml / min

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

[0065] The molecular ratio of feed ethylenediamine to ethylene oxide is 13.2:1

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

[0067] Curing temperature and time: 90-100℃, 2, 5, 10min

[0068] Analysis condition: same as example 1

[0069] Implementation results: (mass concentration if not specified, other implementations are the same) The conversion rate of ethylene oxide at the outlet of the microreactor is 16.6%, the main product hydroxylamine is 2%, high boiling point 0; 90-100℃, after maturing for 2, 5, and 10 minutes The conversion of ethylene oxide was 47.3%, 87.9%, 96.5%, β-hydroxyethyl ethylenediamine 5.55, 10.88, 12.37%, high ...

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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-hydroxyethyl ethylenediamine by ethoxylation of ethylenediamine, in particular to a method for carrying out the process using microreactor technology. Background technique: [0002] The organic amine ethoxylation reaction is a typical gas-liquid contact reaction. The side reaction rate in series is very high. The reactor requires no backmixing and a large gas-liquid contact area. At present, the more advanced ethoxylation reactor has a BUSS loop. Reactor and Press circulating spray reactor, as well as tubular reactor, the former two have high mass transfer efficiency, no backmixing, and the consumption rate of ethylene oxide per cubic meter of reactor reaches 1200-1500kg·h -1 , The tubular reactor is close to the plug flow, the reaction speed is fast, the residence time is short, and the EO consumption reaches 5000-10000kg·h -1 ·M -3 . Ethylenediamine ethoxylation synthesis of β-hydroxylamine mostly uses re...

Claims

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Application Information

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Patent Type & Authority Patents(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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