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Method for synthesizing 2, 2-dimorpholinyl diethyl ether by taking high-boiling morpholine as raw material

A technology of morpholino diethyl ether and high boiler, which is applied in 2 fields and achieves the effects of high separation efficiency, small investment scale and simple device

Active Publication Date: 2011-02-16
ANHUI HYEA AROMAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report yet in the current literature to synthesize 2,2-dimorpholino diethyl ether as a raw material with morpholine high boilers, and then separate and purify the method

Method used

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  • Method for synthesizing 2, 2-dimorpholinyl diethyl ether by taking high-boiling morpholine as raw material

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Embodiment Construction

[0016] (1), the raw material morpholine high boiler is detected, and the results are as follows:

[0017] Component name Composition (wt%)

[0018] water 3.0

[0019] Morpholine 6.0

[0020] Diethylene glycol 17.5

[0021] Monomorpholino diethyl ether 40

[0022] 2,2-Dimorpholino diethyl ether 29

[0023] Other 4.5

[0024] (2), the synthesis of 2,2-dimorpholino diethyl ether: in 1000L stainless steel autoclave, add the morpholine high boiler 300kg that contains 2,2-dimorpholino diethyl ether 29% , add 15 kg of 80-mesh catalyst; use nitrogen replacement three times to get rid of the air in the reaction system; hydrogen and ammonia are continuously fed into the reactor with a volume ratio of 1:6, and the temperature is raised while stirring until the temperature reaches 225 ° C. The reaction time is 6 hours ; Reaction ends, stop feeding hydrogen and ammonia, cool down, filter and separate the catalyst reactants. The reactant was detected by gas chromatography, containing...

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Abstract

The invention discloses a method for synthesizing 2, 2-dimorpholinyl diethyl ether by taking high-boiling morpholine as a raw material. The method comprises the following steps of: importing hydrogen and nitrogen with a volume ratio of 1 / 6 continuously into a reaction kettle in the presence of a catalyst and at reaction temperature of 180-280 DEG C and pressure of 0.25-9.8Mpa, reacting for 4-10h,and then filtering to separate the catalyst to obtain a reactant, transferring the reactant to a kettle type rectifying tower which is filled with a cy700 stainless steel ripple packing, heating the kettle to 120-160 DEG C at normal pressure, and collecting the components such as water, morpholine and the like at the tower top; controlling the temperature of the kettle at 140 DEG C, and collecting the light components at the tower top under the pressure of 20mmHg; and collecting the 2, 2-dimorpholinyl diethyl ether at the tower top at the kettle temperature of 165 DEG C under the pressure of 0.1mmHg with a reflux ratio of 1 / 5-1 / 10. The quality of the obtained product meets the requirement of the polyurethane catalyst. In addition, the invention has the advantages of small investment scale, simple device, high separation efficiency and the product yield reaching 86%.

Description

1. Technical field [0001] The invention relates to a method for synthesizing 2,2-dimorpholino diethyl ether, in particular to a method for synthesizing 2,2-dimorpholino diethyl ether with morpholine high boilers as raw materials. 2. Background technology [0002] 2,2-dimorpholino diethyl ether is a catalyst for the synthesis of polyurethane, and many foreign patents describe its synthesis method. The representative ones are: [0003] U.S. Patent US 6111100 describes a synthetic method, that is, ammonia and diethylene glycol react with hydrogen to prepare 2,2-dimorpholino diethyl ether under high temperature and high pressure in the presence of a hydrogenation catalyst; the involved The device investment is huge. [0004] European patent EP0716084A1 describes a synthetic method, in the presence of cobalt, copper metal catalysts and hydrogen, morpholine and diethylene glycol react at high temperature and pressure to generate 2,2-dimorpholino diethyl ether, while producing a ...

Claims

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Application Information

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IPC IPC(8): C07D295/088
Inventor 范一义
Owner ANHUI HYEA AROMAS
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