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Prepn of tri-and tetra-glycol methyl ether and utilization of side product polyglycol methyl ether

A technology of tetraethylene glycol methyl ether and polyethylene glycol methyl ether, which is applied in the field of organic chemical industry, can solve the problems that the product composition distribution cannot meet the market demand and the market consumption shrinks, and achieve the goal of reducing the overall production cost and unit consumption Effect

Inactive Publication Date: 2003-03-19
JIANGSU YIDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, the market consumption of ethylene glycol methyl ether is gradually shrinking, on the other hand, the market consumption of triethylene glycol methyl ether is steadily expanding, and the composition and distribution of the original products cannot meet the market demand. The production technology of methyl ether as the main target product is inevitable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0033] In a 2L stainless steel reaction kettle, add 288g of methanol and 6.7g of KOH respectively, and use N 2 Replace the air in the kettle, raise the temperature to 110°C under stirring, control the reaction temperature at 110-140°C, and the reaction pressure is less than 0.6MPa, add 1109g of ethylene oxide within 4 hours, complete the addition of ethylene oxide, and keep warm until the pressure does not drop After cooling to below 40°C, 1396g of the product was obtained. The chromatographic analysis showed that the mass composition distribution of the product was as follows: ethylene glycol methyl ether 9.5%, diethylene glycol methyl ether 16.7%, triethylene glycol methyl ether 22.9%, four Ethylene glycol methyl ether 26.3%, pentaethylene glycol methyl ether 20.5%, hexaethylene glycol methyl ether 4.1%.

example 2

[0035] In a 1L stainless steel reaction kettle, add ethylene glycol methyl ether crude product (content is methanol 8.7%, ethylene glycol methyl ether 90%, diethylene glycol methyl ether 1.3%) 320g, KOH 0.8g, and use N 2 Replace the air in the kettle, raise the temperature to 110°C under stirring, control the reaction temperature at 110-140°C, and the reaction pressure is less than 0.6MPa, add 310g of ethylene oxide within 4 hours, complete the addition of ethylene oxide, and keep warm until the pressure does not drop Stop, cool to below 40 ℃ and discharge, get product 629g, chromatographic analysis, the mass composition distribution of product: diethylene glycol methyl ether 18.3%, triethylene glycol methyl ether 35.2%, tetraethylene glycol methyl ether 30.5%, Pentaethylene glycol methyl ether 13.6%, hexaethylene glycol methyl ether 2.5%.

example 3

[0037] In a 2L stainless steel reaction kettle, add methanol 288g, N a OH6.7g, with N 2 Replace the air in the kettle, raise the temperature to 110°C under stirring, control the reaction temperature at 110-140°C, and the reaction pressure is less than 0.6MPa, add 1109g of ethylene oxide within 4 hours, complete the addition of ethylene oxide, and keep warm until the pressure does not drop After cooling to below 40°C, 1398g of the product was obtained. The chromatographic analysis showed that the mass composition distribution of the product was as follows: ethylene glycol methyl ether 8.2%, diethylene glycol methyl ether 12.8%, triethylene glycol methyl ether 19.5%, four ethylene glycol methyl ether 25.6%, pentaethylene glycol methyl ether 23.8%, six or more ethylene glycol methyl ether 10.1%.

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PUM

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Abstract

The present invention relates to the preparation of tri-and tetra-glycol methyl ether and the utilization of side product poly-glycol methyl ether. Alcohol and epoxy ethane are made to react in the presence of alkali metal compound catalyst and the product is depression rectified to obtain separated di, tri- and tetra-glycol methyl ether as well as side product penta-and over glycol methyl ether. The utilization of the side product includes reaction of poly-glycol methyl ether with sodium hydroxide, potassium hydroxide, sodium methoxide or metal sodium to prepare poly-glycol methyl ether sodium or potassium; Williamson reaction with alkylating agent and filtering to prepare side product sodium or potassium salt; and decoloring, adsorption and high vacuum depression distillation to prepare poly-glycol dimethyl ether.

Description

Technical field: [0001] The invention relates to a synthesis method for the preparation of triethylene glycol methyl ether and tetraethylene glycol methyl ether and the reuse of by-product polyethylene glycol methyl ether, which belongs to the technical field of organic chemical industry. Background technique: [0002] The known method of synthesizing ethylene glycol methyl ether is, take methyl alcohol and oxirane as raw material, carry out following reaction under the effect of catalyst: [0003] <chemistry num="002"> <chem file="02138413_cml001.xml" / > < / chemistry> (n=1~5) [0004] Simultaneous reactions of ethylene oxide with methanol and ethylene oxide with glycols result in the formation of mono-, di-, and triethylene glycol methyl ethers and higher molecular weight alcohol ethers. Excess methanol tends to decrease to generate a higher proportion of glycol ether. The molar ratio of methanol to ethylene oxide generally used in industry is 3 to 6. Et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C43/11
Inventor 刘准朱新宝
Owner JIANGSU YIDA CHEM
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