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Method for synthesizing diatomic alcohol ether acid ester

A technology of glycol ether and synthesis method, which is applied in the field of synthesis of glycol ether ester, can solve the problems of high loss of azeotropic dehydrating agent, high solubility, fast hydrolysis speed, etc., and achieve less environmental pollution in production and less water entrainment less, safe to use

Inactive Publication Date: 2009-07-08
NANJING FORESTRY UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the clean synthesis process of glycol ether and fatty acid direct esterification method to prepare glycol ether ester, the core is to select a suitable low-toxic or non-toxic azeotropic dehydrating agent and determine reasonable reaction conditions to improve the efficiency of the esterification reaction. Activity, selectivity and yield of esterification; and the disadvantages of the azeotropic dehydrating agent are that the solubility in water is relatively large and the hydrolysis speed is relatively fast, which makes the loss of the azeotropic dehydrating agent much during the reaction.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0029]Add ethylene glycol butyl ether (EB) 360g, acetic acid 185g, p-toluenesulfonic acid 0.7g, sec-butyl acetate 96g respectively in the 1000ml three-necked flask that has water separator, back distillation condenser φ 20 * 1000 packing tower, control The reaction temperature was 120-170°C, and the reactant was always in a boiling state. After 5 hours of reaction, 52.5 g of water was separated to obtain 553.6 g of crude product. The composition of the reaction system was analyzed by gas chromatography as shown in the following table:

[0030] composition water acetic acid EB sec-butanol sec-butyl acetate EBA content(%) 0.2 3.1 4.4 0.4 10.7 78.0

[0031] The content and composition of organic matter in the by-product water are as follows:

[0032] composition water acetic acid EB sec-butanol sec-butyl acetate EBA content(%) 96.1 1.9 / 1.1 0.4 /

example 2

[0034] Add ethylene glycol butyl ether (EB) 360g, acetic acid 220g, p-toluenesulfonic acid 1.3g, sec-butyl acetate 51g respectively in the 1000ml three-necked flask that has water separator, back distillation condenser φ 20×1000 packing tower, control The reaction temperature was 120-170°C, and the reactants were kept in a boiling state. After 5 hours of reaction, 54.6 g of water was separated to obtain 530.4 g of crude product. The composition of the reaction system was analyzed by gas chromatography as shown in the following table:

[0035] composition water acetic acid EB sec-butanol sec-butyl acetate EBA content(%) 0.3 9.6 6.6 / 4.4 78.1

[0036] The content and composition of organic matter in the by-product water are as follows:

[0037] composition water acetic acid EB sec-butanol sec-butyl acetate EBA content(%) 93.0 5.7 / / 0.6 /

example 3

[0039] Add ethylene glycol butyl ether (EB) 360g, acetic acid 170g, p-toluenesulfonic acid 1.1g, sec-butyl acetate 60g respectively in the 1000ml three-necked flask that has water separator, back distillation condenser φ 20×1000 packing tower, control The reaction temperature was 120-170°C, and the reactant was always in a boiling state. After 5 hours of reaction, 51.5 g of water was separated to obtain 537.8 g of crude product. The composition of the reaction mixture was analyzed by gas chromatography as shown in the following table:

[0040] composition water acetic acid EB sec-butanol sec-butyl acetate EBA content(%) 0.11 0.49 4.91 1.50 8.75 83.65

[0041] The content and composition of organic matter in the by-product water are as follows:

[0042] composition water acetic acid EB sec-butanol sec-butyl acetate EBA content(%) 98.49 0.33 0.04 0.86 0.28 /

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Abstract

The invention relates to a method for synthesizing glycol ether ester. The method comprises the following steps that: glycol ether and fatty acid as raw materials are directly esterified and synthesized into glycol ether acetic ester at a temperature of between 80 and 180 DEG C in the presence of an acidic catalyst and an azeotropic dehydrating agent; and the acidic catalyst is paratoluenesulfonic acid or methanesulfonic acid, and dosage of the catalyst is 0.05 to 1 percent of total weight of reaction materials. The method is characterized in that the mol ratio of the fatty acid to the glycol ether is 1.0:0.8-1.5; and the azeotropic dehydrating agent is isobutyl acetate or 2-butanol acetate, and dosage of the azeotropic dehydrating agent is 5 to 30 percent of the total weight of the reaction materials. The method has the advantages that compared with butyl acetate, the azeotropic dehydrating agent used in the reaction has a lower boiling point and a lower azeotropic point, smaller solubility and lower hydrolysis speed, so that energy consumption during reacting and reclaiming the azeotropic dehydrating agent can be reduced, the reaction speed is improved, and water entrainment of a side product is reduced.

Description

1. Technical field [0001] The invention relates to a method for synthesizing glycol ether esters, in particular to a method for directly esterifying glycol ethers and fatty acids into glycols under the action of an acidic catalyst and a low-toxicity azeotropic dehydrating agent. Synthetic method of ether ester. 2. Background technology [0002] There are both ether bonds and ester structures in the glycol ether ester molecule. These two functional groups not only restrict and repel each other, but also play their own inherent roles. They can dissolve non-polar substances and polar substances to a certain extent. Ability, the total solvency should be said to be the result of the comprehensive effect of various functional groups. It can dissolve small organic molecules, organic macromolecules and synthetic or natural polymers, and can be miscible with water or water-soluble compounds to varying degrees. It has properties that general organic solvents do not have, and its solu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/708
Inventor 朱新宝刘准曹惠庆吴逊何长碧吴亦飞
Owner NANJING FORESTRY UNIV
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