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N-methyl diisopropanolamine preparation method

A technology of methyldiisopropanolamine and diisopropanolamine, applied in the field of preparation of N-methyldiisopropanolamine, can solve the problem of low conversion rate and low purity of N-methyldiisopropanolamine and other problems, to achieve the effect of high conversion rate, avoiding deamination reaction, and high yield

Active Publication Date: 2016-01-13
NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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Problems solved by technology

[0007] The present invention overcomes the problems of low conversion rate in the preparation of N-methyldiisopropanolamine and low purity of the prepared N-methyldiisopropanolamine in the prior art, and provides a synthesis reaction raw material with high conversion rate , obtain the preparation method of the N-methyl diisopropanolamine of high-purity N-methyl diisopropanolamine

Method used

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  • N-methyl diisopropanolamine preparation method

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Effect test

Embodiment 1

[0024] (1) Add 266g of diisopropanolamine and 60g of paraformaldehyde (polymerization degree: 200) into a four-necked flask equipped with a mechanical stirrer and a thermometer, stir evenly, heat, control the reaction temperature at 60°C, and evacuate to The vacuum degree in the reactor is -0.090~-0.099MPa. After stirring and reacting for 2 hours, an intermediate product is obtained, which is a colorless transparent liquid. Sampling is carried out for gas chromatography analysis, and the yield of the intermediate product is 95.1%;

[0025] (2) Cool 50g of the intermediate product obtained in step (1) to room temperature, add 100g of methanol for dilution to obtain the diluted product; (3) add the diluted product to the reaction kettle, and then add 2.5g of Raney nickel , 4g triethylamine, replace the air in the reactor with 1.5Mpa hydrogen for 3-4 times, fill the reactor with hydrogen to 2Mpa, stir the reaction, and control the reaction temperature at about 45°C through circula...

Embodiment 2

[0027] (1) Add 266g of diisopropanolamine and 60g of paraformaldehyde (polymerization degree: 200) into a four-necked flask equipped with a mechanical stirrer and a thermometer, stir evenly, heat, control the reaction temperature at 70°C, and evacuate to The vacuum degree in the reactor is -0.090~-0.099MPa. After stirring and reacting for 2 hours, the intermediate product is obtained as a colorless transparent liquid. Samples are taken and analyzed by gas chromatography. The yield of the intermediate product is 96.3%;

[0028] (2) Cool 50g of the intermediate product obtained in step (1) to room temperature, add 150g of isopropanol for dilution, and obtain the diluted product;

[0029] (3) Add the diluted product to the reactor, then add 2.5g of copper chromite and 4g of trimethylamine, replace the air in the reactor with 1.5Mpa hydrogen for 3-4 times, then fill the reactor with hydrogen to 2Mpa, stir the reaction, and control the reaction temperature at about 45°C by circulat...

Embodiment 3

[0031] (1) Add 266g of diisopropanolamine and 63g of paraformaldehyde (polymerization degree: 200) into a four-necked flask equipped with a mechanical stirrer and a thermometer, stir evenly, heat, control the reaction temperature at 70°C, and evacuate to The vacuum degree in the reactor is -0.090~-0.099MPa. After stirring and reacting for 3 hours, an intermediate product is obtained, which is a colorless transparent liquid. Samples are taken and analyzed by gas chromatography. The yield of the intermediate product is 99.5%;

[0032] (2) Cool 50g of the intermediate product obtained in step (1) to room temperature, add 150g of isopropanol for dilution, and obtain the diluted product;

[0033] (3) Add the diluted product to the reactor, then add 2.5g of copper chromite and 4g of trimethylamine, replace the air in the reactor with 1.5Mpa hydrogen for 3-4 times, then fill the reactor with hydrogen to 2Mpa, stir the reaction, and control the reaction temperature at about 45°C by ci...

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Abstract

The invention relates to a N-methyl diisopropanolamine preparation method, which comprises: (1) adding diisopropanolamine and paraformaldehyde to a reactor, heating, vacuumizing, and carrying out a stirring reaction to obtain an intermediate product; (2) cooling the intermediate product to a room temperature, and adding a solvent to dilute so as to obtain a diluted product; and (3) adding the diluted product to the reaction kettle, adding a catalyst and a tertiary amine inhibitor, replacing the air in the reaction kettle with hydrogen, heating, carrying out a stirring reaction, and filtering to obtain the N-methyl diisopropanolamine product. According to the present invention, diisopropanolamine and paraformaldehyde are adopted as raw materials, and diisopropanolamine is adopted as the paraformaldehyde depolymerization agent to reduce the side reaction at the intermediate product synthesis stage so as to produce the high purity intermediate product; and the tertiary amines inhibitor is added at the hydrogenation reduction reaction stage, such that the possible amine removing reaction during the reaction process is avoided, and the yield of the synthesis reaction is improved.

Description

Technical field [0001] The present invention involves the preparation method of N-methyl glycopyleine. Background technique [0002] MDIPA, as a tri-chain alkanol product, can be applied in the fields of desulfurization, soft agent, textile industry and coating auxiliary. In the field of desulfurization, due to the presence of N-methyl groups in its molecular structure, the alkaline of MDIPA aquatic solution is reduced.Good for H 2 The selective absorption of S gas reduces the energy consumption of understanding the absorption phase; MDIPA and its polyether -type substances synthesized with epoxyxane and ethylene oxide are also used in the field of soft agents and textile industry auxiliary. The main purpose is to increase natural naturally naturallyFiber and artificial fiber are soft; in terms of coatings, there are reports that MDIPA is mainly used for surface treatment additives for semiconductor electronic components.MDIPA -related applied research has reported many patent ...

Claims

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Application Information

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IPC IPC(8): C07C215/12C07C213/00
Inventor 汪少平杭建荣胡艳张书
Owner NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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