Method for synthesizing N,N-diethyl ethanolamine

Abstract

The invention discloses a method for synthesizing N,N-diethyl ethanolamine, which is to synthesize N,N-diethyl ethanolamine in one step in the presence of a catalyst by using diethylamine and ethylene oxide as raw materials, wherein the molar ratio of diethylamine to ethylene oxide in the reaction is (1-15):1, the synthesis reaction temperature is controlled to be 10 to 180 DEG C, the catalyst is added continuously at a speed of 5 to 10g / h, and the added amount is 0.1 to 2.0 percent based on the total mass of the catalyst and the two materials. The method has the following advantages that: 1) pure diethylamine instead of aqueous solution of diethylamine is used as the reaction raw material, so the energy consumption is low and the equipment efficiency is high; and 2) a tubular reactor with a jacket is adopted to transfer heat conveniently, which is favorable continuous operation.

Description

technical field

[0001] The invention relates to the field of pharmaceutical intermediates, in particular to a method for synthesizing N,N-diethylethanolamine. Background technique

[0002] N,N-diethylethanolamine can be used as a pharmaceutical intermediate to prepare procaine hydrochloride, kebetidine, and kemephen, etc.; it can also be used as a solvent to remove acidic gases in natural gas and refinery gas Such as hydrogen sulfide and carbon dioxide, in addition, it can also be used to prepare derivatives of fatty acids, fiber softeners, antirust agents, emulsifiers, vulcanization catalysts for polyurethane foam, etc.

[0003] There are many ways to synthesize N, N-diethylethanolamine. Most of them in China use the aqueous solution of diethylamine to react with ethylene oxide. This process obviously has the disadvantages of low reaction efficiency and many side reactions.

[0004] In addition, as in U.S. Patent No. 4,745,190, diethylamine and ethylene glycol are used as ...

Examples

Embodiment 1

[0022] In a Φ30mm metal tubular reactor with a total length of 2m, 731.4g / h (10mol / h) of diethylamine, 88.1g / h (2.0mol / h) of ethylene oxide, and Catalyst zinc chloride 7g / h was added continuously, cooling water at 25°C was passed into the jacket of the reactor, and the flow rate of cooling water was adjusted to keep the reaction temperature basically constant at 50±5°C. The composition of the final analysis reaction liquid is: DEA70.9%, catalyst 0.8%, DEEA28.1%, high boiler 0.2%.

Embodiment 2

[0024] In a Φ30mm metal tubular reactor with a total length of 2m, 731.4g / h (10mol / h) of diethylamine, 176.2g / h (4.0mol / h) of ethylene oxide, and Catalyst zinc chloride 7g / h was added continuously, cooling water at 25°C was passed into the jacket of the reactor, and the flow rate of cooling water was adjusted to keep the reaction temperature basically constant at 50±5°C. The composition of the final analysis reaction liquid is: DEA48.6%, catalyst 0.7%, DEEA49.2%, high boiling substances 1.5%.

Embodiment 3

[0026] In a Φ30mm metal tubular reactor with a total length of 2m, 731.4g / h (10mol / h) of diethylamine, 88.1g / h (2.0mol / h) of ethylene oxide, and Catalyst ferric chloride 7g / h was added continuously, cooling water at 25°C was passed into the jacket of the reactor, and the flow rate of cooling water was adjusted to keep the reaction temperature basically constant at 50±5°C. The composition of the final analysis reaction liquid is: DEA71.1%, ethylene oxide 0.1%, catalyst 0.8%, DEEA27.8%, high boiler 0.2%.

technical field

[0001] The invention relates to the field of pharmaceutical intermediates, in particular to a method for synthesizing N,N-diethylethanolamine. Background technique

[0002] N,N-diethylethanolamine can be used as a pharmaceutical intermediate to prepare procaine hydrochloride, kebetidine, and kemephen, etc.; it can also be used as a solvent to remove acidic gases in natural gas and refinery gas Such as hydrogen sulfide and carbon dioxide, in addition, it can also be used to prepare derivatives of fatty acids, fiber softeners, antirust agents, emulsifiers, vulcanization catalysts for polyurethane foam, etc.

[0003] There are many ways to synthesize N, N-diethylethanolamine. Most of them in China use the aqueous solution of diethylamine to react with ethylene oxide. This process obviously has the disadvantages of low reaction efficiency and many side reactions.

[0004] In addition, as in U.S. Patent No. 4,745,190, diethylamine and ethylene glycol are used as ...

Examples

Embodiment 1

[0022] In a Φ30mm metal tubular reactor with a total length of 2m, 731.4g / h (10mol / h) of diethylamine, 88.1g / h (2.0mol / h) of ethylene oxide, and Catalyst zinc chloride 7g / h was added continuously, cooling water at 25°C was passed into the jacket of the reactor, and the flow rate of cooling water was adjusted to keep the reaction temperature basically constant at 50±5°C. The composition of the final analysis reaction liquid is: DEA70.9%, catalyst 0.8%, DEEA28.1%, high boiler 0.2%.

Embodiment 2

[0024] In a Φ30mm metal tubular reactor with a total length of 2m, 731.4g / h (10mol / h) of diethylamine, 176.2g / h (4.0mol / h) of ethylene oxide, and Catalyst zinc chloride 7g / h was added continuously, cooling water at 25°C was passed into the jacket of the reactor, and the flow rate of cooling water was adjusted to keep the reaction temperature basically constant at 50±5°C. The composition of the final analysis reaction liquid is: DEA48.6%, catalyst 0.7%, DEEA49.2%, high boiling substances 1.5%.

Embodiment 3

[0026] In a Φ30mm metal tubular reactor with a total length of 2m, 731.4g / h (10mol / h) of diethylamine, 88.1g / h (2.0mol / h) of ethylene oxide, and Catalyst ferric chloride 7g / h was added continuously, cooling water at 25°C was passed into the jacket of the reactor, and the flow rate of cooling water was adjusted to keep the reaction temperature basically constant at 50±5°C. The composition of the final analysis reaction liquid is: DEA71.1%, ethylene oxide 0.1%, catalyst 0.8%, DEEA27.8%, high boiler 0.2%.

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