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The synthetic method of n, n-dimethyl diglycolamine

A technology of dimethyl diglycolamine and diglycolamine, which is applied in the preparation of amino hydroxyl compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problem of high equipment requirements, achieve simple equipment requirements, and reduce costs , the effect of high purity

Active Publication Date: 2018-05-29
Z RIVER GRP LTD
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Problems solved by technology

There are defects such as very high requirements for the use of hydrogen and high equipment requirements

Method used

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  • The synthetic method of n, n-dimethyl diglycolamine
  • The synthetic method of n, n-dimethyl diglycolamine
  • The synthetic method of n, n-dimethyl diglycolamine

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Embodiment 1

[0043] Embodiment 1, a kind of DMAEE synthetic method, take diglycolamine, paraformaldehyde and formic acid as starting raw material, carry out following steps successively:

[0044] 1), synthesis:

[0045] Add 63.1g diglycolamine (0.6mol) and 34.5g paraformaldehyde (1.2mol) into a 250ml three-necked flask, stir for 30 minutes, add 63g formic acid (1.2mol, 88%) dropwise at a temperature of 100-110°C, about After 1 hour of dropwise addition, continue to control the temperature at 100-110° C. to react for 1 hour. 30 g of water was distilled off under reduced pressure (vacuum degree -0.094 MPa, kettle temperature 80° C.). After distilling water, gas chromatographic analysis was carried out, and the product content was 90.0%, and the impurity (S-2) content was 9.8%.

[0046] 2), transesterification

[0047] Add 100 g of n-butanol to the three-necked flask in step 1), heat up to reflux (about 120° C.) for 4 hours, analyze by gas chromatography, the impurity (S-2) content is 0.02...

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Abstract

The invention discloses a synthesizing method of N, N-dimethyl diglycolamine. The method comprises the following steps: adding diglycolamine and paraformaldehyde to a vessel, and dropwise adding formic acid in stirring, wherein the molar ratio of diglycolamine to paraformaldehyde to formic acid is 1: (2-3): (2-3), and the reaction is carried out for 1-2 hours at the temperature of 50 to 110 DEG C; performing pressure-reduction steaming to obtain water generated in the reaction after the reaction is finished, so as to obtain the reacting liquid; adding alcohols substances to the obtained reacting liquid to perform an ester exchange reaction so as to obtain the purified reacting liquid; and performing pressure-reduction distilling on the obtained purified reacting liquid so as to separate out the alcohols substances and N, N-dimethyl diglycolamine, wherein the alcohols substances can be recycled.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, namely the synthesis of N,N-dimethyl diglycolamine and the method for removing impurities. Background technique [0002] N,N-Dimethyl diglycolamine (abbreviation: DMAEE), whose structural formula is shown in S-1, is an important organic chemical intermediate, and a foaming catalyst for polyurethane foam synthesis, suitable for Polyurethane rigid foam, semi-rigid foam, etc., are mainly used in packaging foam. [0003] [0004] N,N-dimethyl diglycolamine formate as an impurity is the formate of S-1, and its structural formula is shown in S-2. [0005] [0006] According to comprehensive literature reports, the preparation of N,N-dimethyl diglycolamine mainly adopts the following methods at present: [0007] 1), ethylene oxide method: [0008] It has been reported in the literature that DMAEE is generated by the reaction of dimethylamine and ethylene oxide; DMAEE is generated b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/08C07C213/02C07C213/10
CPCC07C213/02C07C213/10C07C217/08
Inventor 叶小明张超张琪张华陈新志
Owner Z RIVER GRP LTD
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