Preparation method of N-methyl diethanolamine

A technology of methyldiethanolamine and monomethylamine, which is applied in the preparation of organic compounds, preparation of aminohydroxyl compounds, chemical instruments and methods, etc. It can solve problems such as low vacuum degree, insufficient mixing of raw materials, excessive side reactions, etc. , to achieve the effect of reducing excessive consumption, reducing unit consumption of raw materials, and avoiding environmental pollution

Active Publication Date: 2013-05-01
NINGBO ZHETIE JIANGNING CHEM +1
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0003] At present, the preparation methods for producing N-methyldiethanolamine include the ring-opening reaction of ethylene oxide and methylamine, the methylation reaction of ethanolamine and methanol, the catalytic hydrogenation reaction of ethanolamine and formaldehyde, the substitution reaction of chloroethanol and methylamine, etc. There are many methods, but there are many problems in the production process, such as many reaction side reactions, low conversion rate, high unit consumption ratio, high temperature, low yield, etc.
[0004] For example: Chinese invention patent applications (publication numbers: CN101265195A, CN101506144A) all directly mix raw materials at normal temperature and pressure, and since the raw material methylamine is gaseous at normal temperature and ethylene oxide is liquid

Method used

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  • Preparation method of N-methyl diethanolamine
  • Preparation method of N-methyl diethanolamine

Examples

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Embodiment 1

[0031] combine figure 1 The inventive method is described, figure 1 The scheme shown is a preferred embodiment of the process of the present invention.

[0032] (1) The raw materials of ethylene oxide and monomethylamine are respectively passed through the metering pump ethylene oxide pump 4 and monomethylamine pump 3, and adjusted according to the material ratio of monomethylamine and ethylene oxide as 1.5:1 The flow rate is respectively introduced into two heat exchangers 5 for cooling. 5 is a U-shaped shell-and-tube heat exchanger, with a single shell and two tubes, and liquid ammonia is used for cooling. The pressure in the tube is 0.1~0.3MPa, the pressure in the tube is 0.4~0.5MPa, the raw material is cooled to 2°C, and the cooled raw material is passed into the primary mixer 7-1 and the secondary mixer 7-2 to fully mix. The pressure of the primary mixer and the secondary mixer is 0.4~0.5MPa to obtain mixed raw materials.

[0033] (2) Put the mixed raw materials into t...

Embodiment 2

[0044] Each technical condition is the same as embodiment 1, and difference is:

[0045] In step (5), the temperature at the top of the primary distillation column is 110°C, and the vacuum inside the column is -0.06MPa.

[0046] The top temperature of the secondary rectification tower is 88°C, and the vacuum degree in the tower is -0.95MPa.

[0047] The yield of the obtained N-methyldiethanolamine product is 90.4%, the selectivity is 94.1%, and the color purity of the product is very good.

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Abstract

The invention relates to a manufacturing technology of organic amine, in particular to a preparation technological method of N-methyl diethanolamine. The preparation method comprises the following steps: respectively injecting ethylene epoxide and monomethylamine into heat exchangers for being cooled, and then injecting ethylene epoxide and monomethylamine into a mixer for being premixed; injecting the mixed raw material into a reaction kettle for reaction when the reaction pressure is kept at 4.5-5 MPa and the reaction temperature is kept at 120-135 DEG C; injection reaction liquid into a pressure-relief device to remove excess methylamine; injecting amine-removed substrate into a flash vaporization absorption tower for being processed so as to remove moisture and light component impurities; and finally utilizing a tertiary distillation and rectification column to separate N-methyl diethanolamine product. The preparation method solves the problems of overlong reaction time, low conversion rate, excessive side reaction and the like, which are caused by insufficient premixing in a conventional process, increases the MDEA (methyl diethanolamine) content from 70-80 percent in the original process to more than 90 percent, improves the reaction yield, lowers the unit consumption of raw materials, reduces energy consumption and also avoids environmental pollution.

Description

technical field [0001] The invention relates to the technical field of preparation of organic amine products, in particular to a preparation process of N-methyldiethanolamine. Background technique [0002] N-Methyldiethanolamine, commonly known as MDEA, is a colorless or yellowish viscous liquid with an ammonia smell, flammable and miscible with water and alcohol, slightly soluble in ether. MDEA is widely used in desulfurization and purification of oilfield gas and coal gas, natural gas, emulsifier and acid gas absorbent, acid-base control agent, polyurethane foam catalyst. CO2 and H2S produced in ammonia synthesis can be removed with the participation of activators. In addition, it can also be used as semi-finished products of insecticides, emulsifiers, fabric auxiliaries, intermediates of antitumor drug nitrogen mustard hydrochloride, catalysts for urethane coatings, fiber auxiliaries, etc. dry agent. [0003] At present, the preparation methods for producing N-methyldi...

Claims

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Application Information

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IPC IPC(8): C07C215/12C07C213/04C07C213/10
Inventor 饶金土肖晓辉陈爱民胡军毛正余
Owner NINGBO ZHETIE JIANGNING CHEM
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