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Method of preparing ethylene glycol monomethyl ether through continuous etherification method

A technology of ethylene glycol monomethyl ether and ethylene glycol, which is applied in the fields of ether preparation, dehydration of hydroxyl-containing compounds to prepare ether, organic chemistry, etc. It can solve the problems of pollution, difficult separation, difficult post-processing, etc., and avoid corrosion , the effect of high product selectivity

Inactive Publication Date: 2016-05-18
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

The Williamson synthesis method is a method adopted in industrial scale production, but this method is prone to produce a large amount of sodium chloride or sodium sulfate, has certain pollution, difficult post-processing, and has certain limitations to industrial production.
The ring-opening etherification of ethylene oxide is a relatively clean and economical production method. In the patent CN101190876B, niobium oxide is used as a catalyst, the conversion rate of ethylene glycol is greater than 99%, and the selectivity of ethylene glycol monoether is greater than 82%; CN101263101A HBF 4 / BF 3 And protonic acid, as a composite catalyst to catalyze the direct reaction of dimethyl ether and ethylene oxide, but the product components are complex and difficult to separate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put the silica-alumina molecular sieve into the fixed-bed reactor, take the ZSM series as an example, feed 40ml / min of nitrogen, and control the reaction pressure to maintain at about 0.5MPa. Prepare an ethylene glycol-methanol solution with a molar ratio of 1 / 8 and put it in the circulation tank, preheat the temperature to 230°C, pump the preheated raw material into the fixed bed reactor, and the liquid space velocity is 1h -1 , the reaction temperature is 230°C, and the product after the etherification reaction is directly analyzed on-line by gas chromatography at regular intervals. After 2 hours of reaction, the conversion rate of ethylene glycol reached 90%, and the selectivity of ethylene glycol monomethyl ether reached 68%. After 30 hours of reaction, the conversion rate of ethylene glycol reached 91%, and the selectivity of ethylene glycol monomethyl ether reached 65%. After another part of the reaction material is separated, ethylene glycol monomethyl ether is ...

Embodiment 2

[0024] Put the aluminum phosphorus molecular sieve into the fixed bed reactor, take the SAPO series as an example, feed 40ml / min nitrogen as the carrier gas, and control the reaction pressure to maintain at about 1MPa. Prepare the ethylene glycol-methanol solution with a molar ratio of 1 / 8 and put it in the circulation tank, preheat the temperature to 250°C, the preheated raw material is carried into the fixed bed reactor by the carrier gas, and the liquid space velocity is 1h -1 , the reaction temperature is 200°C, and the product after the etherification reaction is directly analyzed on-line by gas chromatography at regular intervals. After 2 hours of reaction, the conversion rate of ethylene glycol reached 85%, and the selectivity of ethylene glycol monomethyl ether reached 49%.

Embodiment 3

[0026] Put the ion exchange resin in a fixed-bed reactor, taking the Amberlyst series as an example, feed 40ml / min of nitrogen, and control the reaction pressure to maintain around 1MPa. Prepare an ethylene glycol-methanol solution with a molar ratio of 1 / 6 and put it in the circulation tank, preheat the temperature to 210°C, the preheated raw material is carried into the fixed bed reactor by the carrier gas, and the liquid space velocity is 0.5 h -1 , the reaction temperature is 180°C, and the product after the etherification reaction is directly analyzed on-line by gas chromatography at regular intervals. After 2 hours of reaction, the conversion rate of ethylene glycol reached 65%, and the selectivity of ethylene glycol monomethyl ether reached 56%.

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Abstract

The invention discloses a method of preparing ethylene glycol monomethyl ether through a continuous etherification method. In the method, the ethylene glycol monomethyl ether is prepared with ethylene glycol and methanol as raw materials in a fixed bed reaction apparatus under the effect of a multiphase etherification catalyst in a continuous etherification manner. The method can increase the selectivity on the main product and inhibit generation of too many side products. Cyclic utilization on the reaction material can be achieved. The method is carried out with the multiphase etherification catalyst so that corrosion on devices due to usage of liquid acid and the like catalysts is avoided. The product is high in quality and can be applied in large scale.

Description

technical field [0001] The invention relates to a method for preparing ethylene glycol monomethyl ether, in particular to a method for preparing ethylene glycol monomethyl ether by a continuous etherification method. Background technique [0002] Ethylene glycol monoether compounds contain ether bonds, hydroxyl groups and different alkyl groups in their structure. They are not only water-soluble, but also can dissolve organic molecules, synthetic polymers and natural polymers. They are a universal green solvent and are widely used As an industrial solvent, it can also be used as antifreeze, surfactant, printed circuit board adhesive, skin care product additive, etc. It has broad application prospects in industry. [0003] At present, the synthesis methods of ethylene glycol monoether compounds include Williamson synthesis method, ethylene oxide ring-opening etherification method, ethylene addition method, methyl ether coupling method, etc. (Chemical Industry and Engineering ...

Claims

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Application Information

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IPC IPC(8): C07C41/09C07C43/13
Inventor 于维强徐杰路芳陈帅陈佳志高进苗虹车鹏华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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