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A kind of method for preparing 2-methoxyethylamine by direct catalytic amination of ethylene glycol monomethyl ether

A technology of ethylene glycol monomethyl ether and methoxyethylamine, applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxyl compounds, etc., can solve problems such as complex control process, large amount of waste residue, environmental pollution, etc. Achieve the effects of simple reaction process, less by-products and simple preparation

Active Publication Date: 2021-12-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these two methods are non-atomic and economical reactions, and the phthalic acid or its salts produced will produce a large amount of waste residue and cause great pollution to the environment.
[0008] Patent CN103936599 describes a preparation method of 2-methoxyethylamine, which uses ethanolamine as raw material, undergoes azeotropic dehydration with benzaldehyde to form aldimine, and then methylates under alkaline conditions, deprotects and alkalizes The final product 2-methoxyethylamine can be obtained by rectification, and its yield is 56%-84%. However, a large amount of salt will be produced in the reaction, which is troublesome to handle and complicated to control.

Method used

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  • A kind of method for preparing 2-methoxyethylamine by direct catalytic amination of ethylene glycol monomethyl ether
  • A kind of method for preparing 2-methoxyethylamine by direct catalytic amination of ethylene glycol monomethyl ether

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Effect test

Embodiment 1

[0020] Preparation of Catalyst A: Utilize equal volume impregnation method to weigh 2.5698g copper nitrate, 2.1048g nickel nitrate, 0.6482g cerium nitrate, 3.7850g chromium nitrate and 0.0745g silver nitrate according to the percentage content of each element, be mixed with 10ml salt solution and The salt solution was impregnated on 10g of γ-alumina carrier, impregnated at room temperature for 12h, dried at 100°C for 12h, calcined in a muffle furnace at 500°C for 3h, and the required oxidized catalyst was obtained after cooling, and catalyst A (Cu-Cr- Ni-Ce-Ag / Al 2 o 3 ). Based on the mass fraction of elements, the prepared catalyst contains 7.8wt% Cu, 6.7wt% Cr, 5.13wt% Ni, 2.5wt% Ce, 0.5wt% Ag, and the rest is carrier γ-alumina.

Embodiment 2

[0022] Preparation of Catalyst B: Weigh 3.7965g of copper nitrate and 4.8658g of nickel nitrate according to the percentage content of each element by equal-volume impregnation method, prepare 10ml of salt solution and impregnate the salt solution on 10g of γ-alumina carrier, after immersion at room temperature for 12 hours Dry at 100°C for 12h, bake in a muffle furnace at 500°C for 3h, and after cooling, the desired catalyst B (Cu-Ni / Al 2 o 3 ), the prepared catalyst is based on the element mass fraction, the content of Cu is 10wt%, the content of Ni is 10wt%, and the rest is carrier gamma-alumina.

Embodiment 3

[0024] Preparation of Catalyst C: Weigh 5.3590g copper nitrate, 4.8642g nickel nitrate and 0.0765g silver nitrate according to the percentage content of each element by equal volume impregnation method, prepare 10ml salt solution and impregnate 10g gamma-alumina carrier with the salt solution After immersing at room temperature for 12 hours, drying at 100°C for 12 hours, calcination at 500°C in a muffle furnace for 3 hours, and after cooling, the required catalyst C(Cu-Ni-Ag / Al 2 o 3 ), the prepared catalyst is based on the mass fraction of elements, wherein the content of Cu is 15wt%, the content of Ni is 10wt%, the content of Ag is 0.5wt%, and the rest is carrier gamma-alumina.

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Abstract

The invention discloses a method for preparing 2-methoxyethylamine by direct catalytic amination of ethylene glycol monomethyl ether. The raw materials ethylene glycol monomethyl ether, ammonia and hydrogen are continuously input into a tubular fixed bed filled with catalyst. Amination reaction is directly carried out in the reactor to prepare 2-methoxyethylamine. The catalyst is based on γ-alumina as a carrier, and the supported active metal component is one or any mixture of copper, cobalt, nickel, chromium, cerium, silver or ruthenium elements, and the active group The theoretical loading amount of the minute is 15%-35% of the mass of the catalyst. The method of the invention has the advantages of simple process, mild reaction conditions, high yield of 2-methoxyethylamine, and low cost.

Description

Technical field: [0001] The invention relates to the production field of organic amines, in particular to a method for preparing 2-methoxyethylamine by catalytic amination of ethylene glycol methyl ether and ammonia as raw materials in the presence of a solid catalyst. [0002] technical background: [0003] Organic aliphatic amines are derivatives in which some or all of the hydrogen atoms in the ammonia molecule are replaced by alkyl groups. According to the number of hydrogen atoms in the ammonia molecule replaced by alkyl groups, it can be divided into primary amines, secondary amines and tertiary amines, and can also be called mono-, di- and tri-alkyl amines. According to the number of carbon atoms in the substituted alkyl group, it can be divided into lower aliphatic amines and higher aliphatic amines; lower aliphatic amines are generally generated by substituting hydrogen on amines with alkyls with less than 6 carbons, and higher aliphatic amines are generally formed b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/08C07C213/02B01J23/89B01J23/755
CPCC07C213/02B01J23/002B01J23/755B01J23/8926B01J23/8993B01J2523/00C07C217/08B01J2523/17B01J2523/18B01J2523/31B01J2523/3712B01J2523/67B01J2523/847B01J2523/845B01J2523/821
Inventor 张泽凯周贤机刘华彦卢晗锋朱秋莲
Owner ZHEJIANG UNIV OF TECH