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Method for preparing ethylene glycol monoethyl ether

A technology of ethylene glycol monoethyl ether and catalyst, which is applied in the fields of ether preparation, dehydration of hydroxyl-containing compounds to prepare ether, organic chemistry, etc., can solve the problems of back mixing, no ethylene glycol monoethyl ether catalyst, and low selectivity coefficient. , to achieve the effect of high selectivity, easy industrialization and simple preparation process

Inactive Publication Date: 2008-03-12
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process method has the following disadvantages: on the one hand, there is back-mixing of the materials in the reaction system in the tank reactor, and the ethoxylated product cannot leave the reaction system
And in continuous production " preparation method (CN1081176A) of ethylene glycol ether (class) " patent document, the selectivity of the catalyst ethylene glycol ether (class) material involved is the highest only 54%, selectivity coefficient is lower
Within the scope of the applicant's search, there is no report on the process of preparing ethylene glycol monoethyl ether using an atmospheric pressure membrane reactor, nor is there any report on the preparation of an ethylene glycol monoethyl ether catalyst suitable for an atmospheric pressure membrane reactor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 46.0gMg(NO 3 ) 2 ·6H 2 O, 13.1gCo(NO 3 ) 2 ·6H 2 O was dissolved in 100ml distilled water, and then 1.4gLa(NO 3 ) 3 .6H 2 0, to obtain a salt solution, the resulting solution is mixed with 25% by weight of concentrated ammonia water in a co-current and dropwise manner, and the pH of the mixed solution is adjusted to be 9, reacted at normal pressure and 40°C for 1h, then cooled to room temperature, and then Aging for 20 hours, conventional suction filtration, washing, drying, and roasting at 500°C for 4 hours to obtain a block catalyst, which was crushed to 40-60 mesh to obtain the desired catalyst, marked as GM1.

[0018] The prepared catalyst GM1 was placed in a tubular membrane in a continuous membrane reactor, and nitrogen was purged outside the membrane; The ethanol was first vaporized in a 90°C preheater, the temperature of the membrane reactor was kept at 100°C, and the gas space velocity was 1.5×10 3 ml·g -1 h -1 , to produce ethylene glycol monoethyl ...

Embodiment 2

[0020] 34.6gMg(NO 3 ) 2 ·6H 2 O, 13.1gCo(NO 3 ) 2 ·6H 2 O was dissolved in 100ml distilled water, and then 1.05g Ce(NO 3 ) 2 ·6H 2 0, to obtain a salt solution, the gained solution is mixed with the concentrated ammonia water of 25% by weight in a parallel dripping manner, and the pH of the mixed solution is adjusted to be 10, reacted at normal pressure and 50°C for 1.5h, then cooled to room temperature, Aging for another 18 hours, conventional suction filtration, washing, drying, and roasting at 400°C for 6 hours to obtain a block catalyst, which was crushed to 40-60 mesh to obtain the desired catalyst, marked as GM2.

[0021] The prepared catalyst GM2 is placed in a tubular membrane in a continuous membrane reactor, and nitrogen is purged outside the membrane; The ethanol is first vaporized in a preheater at 100°C, the temperature of the membrane reactor is maintained at 115°C, and the gas space velocity is 2×10 3 ml·g -1 h -1 , to produce ethylene glycol monoethy...

Embodiment 3

[0023] 34.6gMg(NO 3 ) 2 ·6H 2 O, 13.1gCo(NO 3 ) 2 ·6H 2 O was dissolved in 100ml of distilled water, and then 6.6g of Al(NO 3 ) 3 9H 20, to obtain a salt solution, the resulting solution was mixed with 25% by weight of concentrated ammonia water in a co-current and dropwise manner, and the pH of the mixed solution was adjusted to be 9, reacted at normal pressure and 60°C for 1h, then cooled to room temperature, and then Aging for 24 hours, conventional suction filtration, washing, drying, and roasting at 600°C for 5 hours to obtain a block catalyst, which was crushed to 40-60 mesh to obtain the desired catalyst, marked as GM3.

[0024] The prepared catalyst GM3 is placed in a tubular membrane in a continuous membrane reactor, and nitrogen is purged outside the membrane; under normal pressure conditions, the gas phase ethoxylation of ethanol and ethylene oxide with a molar ratio of 3:1 For the reaction, ethanol was first vaporized in a 100°C preheater, the temperature o...

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Abstract

The present invention relates to a preparation method of the glycol monoethyl ether. The preparation method uses the continuous membrane reactor and the following process: 1. the catalyst consisting of the active ingredient and the carrier with the quality ratio being 0.1 to between 20 and 100 is prepared; the carrier is the MgO / CoO complex with the atomic number ratio that the ratio between the Mg and Co is between 3 and 5 to 1; the active ingredient is one or a plurality of the oxides of the La, Ce, Al, Ni or Cu; 2. the glycol monoethyl ether is to be synthesized; the catalyst prepared in the first step is arranged in the tubular membrane of the continuous membrane reactor; the nitrogen is used to blow and sweep outside the membrane; the ethanol and ethylene oxide with the molar ratio being between 3 and 4 to 1 are used as the raw materials; at first, the ethanol is preheated and gasified at the temperature between 90 and 100 Celsius system; the gas-phase ethoxylated reaction is done at the room pressure and the temperature between 100 and 140 Celsius system; the air speed of the reactive gas is (1-3) multiplied by the 103ml question mark g-1question mark h-1; thus, the glycol monoethyl ether can be made.

Description

technical field [0001] The invention relates to a preparation technology of chemical products, specifically a preparation method of ethylene glycol monoethyl ether, and the international patent classification number is proposed to be Int.Cl.C07C 43 / 00 (2006.01). Background technique [0002] Ethylene glycol monoethyl ether is a general purpose solvent. Because its structure contains two groups of ether bond and hydroxyl group, it has excellent properties such as low freezing point, excellent mutual solubility, fast permeability, strong diffusion force, good solubility and dilution, and is often used as nitrocellulose, synthetic resin or Solvents for paints, for example, in the leather industry for colorants, emulsion stabilizers, ink solvents, vitamin B12 refining solvents, etc.; in the paint industry for the preparation of paint thinners, paint removers and raw materials for spray paint; in the textile industry It is used as a dyeing agent in the manufacture of fibers; it ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/10C07C41/09
Inventor 刘秀军潘兵
Owner TIANJIN POLYTECHNIC UNIV
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