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Method for directly co-preparing glycol dimethyl ether and ethylene glycol from ethylene glycol monomethyl ether

A technology of ethylene glycol monomethyl ether and ethylene glycol dimethyl ether, which is applied in the direction of ether preparation, alcoholysis preparation, and organic part exchange to prepare ether, etc., which can solve the problem of harsh reaction conditions, high reaction temperature, inability to metabolize out of the body, etc. problems, to achieve the effect of less side reactions and simple products

Active Publication Date: 2017-04-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the above-mentioned reported method by preparing ethylene glycol dimethyl ether, or take multiple reactant as raw material, involve complicated reaction process and complicated by-product, or reaction condition is harsh such as high reaction temperature, and in these methods all There is a by-product 1,4-dioxane
However, when the by-product is dissolved in wastewater, it is difficult to remove by physical separation, and the by-product is not easy to be biodegraded in the natural environment, and can enter the human body or animal through inhalation, ingestion or absorption through the skin , which gradually accumulate in the body and cannot be metabolized out of the body, thus causing harm to the human or animal body

Method used

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  • Method for directly co-preparing glycol dimethyl ether and ethylene glycol from ethylene glycol monomethyl ether
  • Method for directly co-preparing glycol dimethyl ether and ethylene glycol from ethylene glycol monomethyl ether
  • Method for directly co-preparing glycol dimethyl ether and ethylene glycol from ethylene glycol monomethyl ether

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Experimental program
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Effect test

Embodiment 1

[0047] The H-beta molecular sieve with Si / Al=i6 was pressed into tablets under a pressure of 40 MPa, and granulated into 20-40 mesh to obtain a spare catalyst. 1 g of this catalyst was filled in a fixed-bed reactor and pretreated. Catalyst pretreatment conditions are: N 2 The flow rate is 30ml / min, rising from 25°C to 500°C over 150min, and maintaining at 500°C for 180min.

[0048] The reaction raw material ethylene glycol monomethyl ether was prepared by N 2 It is brought into the reactor at a flow rate of 30ml / min, and the reaction pressure is 0.5Mpa.

[0049] The raw material conversion rate and product selectivity change with temperature are shown in Table 1.

[0050] Table 1: Reaction activity and product selectivity of raw material ethylene glycol monomethyl ether on H-β molecular sieve catalyst under different temperature conditions

[0051]

[0052] Reaction conditions: reaction pressure 0.5Mpa, catalyst mass 1g, water bath temperature 60°C, N 2 Flow rate 30ml / ...

Embodiment 2

[0055] The H-Y molecular sieve with a silicon-aluminum ratio of 10.6 was pressed into tablets under a pressure of 40 MPa and granulated into 20-40 mesh to obtain a spare catalyst. 1 g of this catalyst was filled in a fixed-bed reactor and pretreated. The pretreatment condition is: N 2 The flow rate is 30ml / min, rising from 25°C to 500°C over 150min, and maintaining at 500°C for 180min.

[0056] The reaction raw material ethylene glycol monomethyl ether was prepared by N 2 It is brought into the reactor at a flow rate of 30ml / min, and the reaction pressure is 0.5Mpa.

[0057] The raw material conversion rate and product selectivity change with temperature are shown in Table 2.

[0058] Table 2: Reactivity and product selectivity of raw material ethylene glycol monomethyl ether on H-Y catalyst under different temperature conditions

[0059]

[0060] Reaction conditions: reaction pressure 0.5Mpa, catalyst mass 1g, water bath temperature 60°C, N 2 Flow rate 30ml / min.

[0...

Embodiment 3

[0063] Select H-β, H-Y, H-ZSM-5, H-MOR, F-FER molecular sieves with different silicon-aluminum ratios, press them into tablets under a pressure of 40Mpa, and granulate them into 20-40 meshes to obtain spare catalysts. 1g of each catalyst was selected and packed into a fixed-bed reactor for pretreatment. The pretreatment condition is: N 2 The flow rate is 30ml / min, rising from 25°C to 500°C over 150min, and maintaining at 500°C for 180min. The reaction raw material ethylene glycol monomethyl ether is prepared by N 2Bring into the reactor at a flow rate of 30ml / min. Space velocity, reaction pressure.

[0064] The conversion of raw materials and the selectivity of products ethylene glycol dimethyl ether and 1,4-dioxane as a function of temperature and pressure are shown in Table 3.

[0065] Table 3: Reactivity of ethylene glycol monomethyl ether on catalysts with different topological structures and silicon-aluminum ratios and selectivity of ethylene glycol dimethyl ether and...

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Abstract

The invention provides a method for directly co-preparing glycol dimethyl ether and ethylene glycol from ethylene glycol monomethyl ether. The method specifically comprises the following steps: enabling a raw material ethylene glycol monomethyl ether and optional inert gas which is taken as carrier gas to pass through a reactor loaded with a solid acid catalyst; reacting under conditions with a reaction temperature ranging from 40 DEG C to 150 DEG C and reaction pressure ranging from 0.1 Mpa to 15.0 Mpa to generate glycol dimethyl ether and ethylene glycol, wherein mass space velocity of the raw material ethylene glycol monomethyl ether ranges from 0.05 h<-1> to 5.0 h<-1>; and volume concentration of the raw material ethylene glycol monomethyl ether is 1-100%, and volume concentration of the carrier gas is 0-99%. Under a low-temperature condition, the method takes solid acid as a catalyst and takes ethylene glycol monomethyl ether as the raw material to prepare glycol dimethyl ether and ethylene glycol with high selectivity; and meanwhile, formation of a byproduct 1,4-dioxane which pollutes the environment or damages a human body or an animal body is basically or completely avoided.

Description

technical field [0001] The application belongs to the field of chemistry and chemical engineering, and specifically relates to a method for directly preparing ethylene glycol dimethyl ether from ethylene glycol monomethyl ether and co-producing ethylene glycol. Background technique [0002] Ethylene glycol dimethyl ether, the Chinese name is 1,2-dimethoxyethane (DME). At room temperature, ethylene glycol dimethyl ether is a colorless and transparent liquid with an ether smell. It is an aprotic polar solvent with excellent performance. Carbon (C1-C6) alcohols, ketones, esters and other organic solvents are miscible in any proportion, and have strong solubility for alkali metal compounds. Therefore, it can become an ideal solvent required in many organic synthesis reactions, and it is also widely used as a cleaning agent compound, as a textile printing and dyeing, paint and ink additives, fuel additives, and for organic compounds and pharmaceutical intermediates synthesis et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/14C07C43/10C07C29/10C07C31/20
CPCC07C29/10C07C41/14C07C43/10C07C31/202Y02P20/52B01J29/7815C07C29/128B01J29/084B01J29/18B01J29/40B01J29/65
Inventor 石磊倪友明朱文良刘勇刘红超刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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