Method for producing N,N-dimethyl diglycolamine and co-producing N,N-dimethyl ethanolamine

A technology of dimethyl diglycolamine and dimethylethanolamine, which is applied in chemical instruments and methods, preparation of amino hydroxyl compounds, preparation of organic compounds, etc., can solve problems such as not being widely used and side reactions, and achieve atomic High economy, high total yield, resource saving effect

Inactive Publication Date: 2017-08-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This reaction is prone to side reactions, so it is necessary to develop a highly selective catalyst, which has not been widely used in industry at present

Method used

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  • Method for producing N,N-dimethyl diglycolamine and co-producing N,N-dimethyl ethanolamine
  • Method for producing N,N-dimethyl diglycolamine and co-producing N,N-dimethyl ethanolamine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1, a kind of technique of producing DMAEE and coproducing DMAE. With ethylene oxide (EO), 33% dimethylamine (DMA) aqueous solution as starting material, carry out following steps successively:

[0038] (1) Synthesis:

[0039] Add 68g of dimethylamine aqueous solution (0.5mol) into a 250ml autoclave, replace the reactor with nitrogen three times, fill with 44g (1mol) of ethylene oxide, then fill with nitrogen to 1.2MPa, heat up to 80°C for reaction, The reaction time is 4h. 112 g of the resulting reaction solution was collected.

[0040] (2) Separation:

[0041] The reaction solution in step (1) was distilled under reduced pressure (20mmHg). Separately collect 40~70℃, 90~95℃ fractions. The obtained light component is 48.7g of DMAE aqueous solution; the obtained heavy component is 61.5g of DMAEE. DMA conversion was 100%. Based on amino groups, the yield of DMAE was 7.8%, and the yield of DMAEE was 91.6%.

[0042] (3) Loop:

[0043] Measure (2) step DMA...

Embodiment 2

[0046] Embodiment 2, a kind of technique of producing DMAEE and coproducing DMAE. Taking EO and 33% DMA aqueous solution as starting materials, the following steps are carried out in sequence:

[0047] (1) Synthesis:

[0048] Add 68g of dimethylamine aqueous solution (0.5mol) into a 250ml autoclave, replace the reactor with nitrogen 3 times, fill it with 44g (1mol) of ethylene oxide, keep the reactor at normal pressure, raise the temperature to 80°C for reaction, and the reaction time for 2h. The resulting reaction solution was collected.

[0049] (2) Separation:

[0050] The reaction solution in step (1) was distilled under reduced pressure (20mmHg). Separately collect 40~70℃, 90~95℃ fractions. The obtained light component is 81.5 g of DMAE aqueous solution; the obtained heavy component is 12.1 g of DMAEE. DMA conversion was 100%. EO conversion was 59.3%. Based on the amino group, the yield of DMAE was 82.1%, and the yield of DMAEE was 18.3%.

[0051] (3) Loop:

[0...

Embodiment 3

[0055] Embodiment 3, a kind of technique of producing DMAEE and coproducing DMAE. Taking EO and 33% DMA aqueous solution as starting materials, the following steps are carried out in sequence:

[0056] (1) Synthesis:

[0057] Add 68g of dimethylamine aqueous solution (0.5mol) to a 250ml autoclave, replace the reactor with nitrogen 3 times, then fill in 22g (0.5mol) of ethylene oxide, the reactor is at normal pressure, and heat up to 40°C for reaction. The time is 2h. 88.6 g of the resulting reaction solution was collected.

[0058] (2) Separation:

[0059] The reaction solution in step (1) was distilled under reduced pressure (20mmHg). Collect 40~70℃, 90~95℃ fractions. The light component obtained was 87.2 g of DMAE aqueous solution; the heavy component obtained at the bottom of the kettle was 1.2 g of DMAEE. DMA conversion was 100%. EO conversion rate 95%. Based on amino groups, the yield of DMAE was 95.0%, and the yield of DMAEE was 4.7%.

[0060] (3) Loop:

[0061...

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Abstract

The invention discloses a method for producing N,N-dimethyl diglycolamine and co-producing N,N-dimethyl ethanolamine. The method comprises the following steps: 1) heating dimethylamine aqueous solution and ethylene oxide as reaction raw materials at a temperature of 40-140 DEG C and a pressure of 0-1.5MPa for 2-6 hours according to the molar ratio of dimethylamine to ethylene oxide of 1:1-2.5, and introducing nitrogen during reaction to keep pressure; and (2) distilling the reacting product in the step (1) at reduced pressure after the reaction is finished so as to obtain N,N-dimethyl diglycolamine aqueous solution serving as a light component and N,N-dimethyl ethanolamine serving as a heavy component.

Description

technical field [0001] The invention relates to a co-production preparation of organic compounds N,N-dimethyl diglycolamine (N,N-Dimethylaminoethoxyethanol, DMAEE) and N,N-dimethylethanolamine (N,N-Dimethyl ethanolamine, DMAE) method. Background technique [0002] The main product is DMAEE, the molecular formula is C6H15O2N; co-production DMAE, the molecular formula is C4H11ON. Its structural formula is as follows: [0003] [0004] DMAEE is a new type of catalyst, which is often used to catalyze the synthesis of low-odor polyurethane foam materials. It is widely used in the production of automotive interiors, home decorations, household appliances, building materials, and thermal insulation materials. [0005] Comprehensive literature reports, the preparation of DMAEE mainly adopts the following methods at present: [0006] Method 1: DMAE reacts with ethylene oxide (Ethylene oxide, EO) in one step. Zhao Bin et al. (Molecular Catalysis, 2008, 22 (6), 487-490.) used an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/04C07C217/08C07C215/08C07C213/06
CPCC07C213/04C07C213/06C07C217/08C07C215/08
Inventor 陈新志史雅静钱超
Owner ZHEJIANG UNIV
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