Method for preparing glycol methyl ether acetate

A technology of ethylene glycol methyl ether and acetate, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of non-recyclable, high toxicity, expensive catalyst, etc., and achieve equipment corrosion The effect of small, small dosage, and cheap catalyst

Inactive Publication Date: 2008-08-13
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the above process, there are disadvantages such as expensive catalyst, high toxicity, and inability to recycle.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1 Preparation of solid base catalyst

[0022] Preparation of alkaline earth metal oxides

[0023] Take CaO powder and roast it in a muffle furnace at 800°C for 5 hours to obtain it;

[0024] Step 2 transesterification reaction

[0025] Add 0.6mol ethyl acetate, 0.1mol ethylene glycol methyl ether, and 0.1g solid alkali catalyst into a 250mL three-necked flask equipped with electromagnetic stirring, a thermometer, a rectifying column, an adapter tube, and a recovery flask, and heat to reflux and stir to make The ethanol produced by the reaction is azeotropically distilled from the upper end of the distillation head, and the reaction stops until the temperature at the upper end of the distillation head is higher than the azeotropic temperature of ethyl acetate and ethanol (that is, no ethanol is distilled out);

[0026] Step 3 Catalyst separation and product purification

[0027] Filter the material obtained in the previous step, and the filtered catalyst is dried...

Embodiment 2

[0029] Except the following differences, all the other are the same as Example 1.

[0030] Preparation of Supported Solid Base Catalyst

[0031] Dissolve 4 grams of KF in 25 grams of water, add 10 grams of Al 2 o 3 , after stirring at 60°C for 1h, rotary steaming to dryness, drying the solid in an oven at 100°C for 12h, and calcining in a muffle furnace at 800°C for 5h; the yield is 95%.

Embodiment 3-8

[0033] Except for the following differences, the others are the same as in Example 2, with KF as the active component and different carriers shown in Table 1.

[0034] Table 1

[0035] Example

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PUM

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Abstract

The invention discloses a method for preparing glycol monomethyl ether acetate, comprising using ethyl acetate and glycol methyl ether as materials, performing ester changing reaction in the presence of a solid alkali catalyst, distilling by-product ethanol fro a reaction tank through fractionation, filtering and recoverying the catalyst after reaction, fractionating the reaction liquid to obtain glycol monomethyl ether acetate. The invention has the advantages of: (1) high yield of 95.5-99.6%, (2) cheap catalyst and small usage which is 0.1-1.5% of the total weight of reaction materials; (3) gentle reaction condition, reaction under atmosphere pressure; (4) repeatedly-usable catalyst; (5) samll corrosion on the device and no environmental contamination.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for preparing ethylene glycol methyl ether acetate by transesterification. Background technique [0002] There are both ether bonds and carbonyl groups in the molecule of glycol ether acetate, and the carbonyl groups form an ester structure, so it has properties that general organic solvents do not have. It can dissolve organic molecules, synthetic or natural high Molecular compounds can also be miscible with water or water-soluble compounds to varying degrees. It is a kind of low-toxic high-grade industrial solvent with excellent high-boiling point and two-functional groups. Its performance is better than glycol ether. It is used in automotive paint, containers, mechanical equipment, metal It has been widely used in the production of furniture, appliance surface coatings, inks, water-soluble coatings, colorful spray coatings, paint removers, industria...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/16C07C69/12C07C67/24C07C67/03B01J23/02
Inventor 杨建国龚国珍梁学正王有菲权南南鲍少华何鸣元
Owner EAST CHINA NORMAL UNIV
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