Method for producing safe and environment-friendly carbonic ester series mixed solvents

A mixed solvent, safe and environmentally friendly technology, applied in the preparation of organic carbonates, organic chemistry, coatings, etc., can solve the problems of strong alkaline catalysts and carbonate catalysts, catalyst deactivation, non-existence, and expensive carbonate solvents , to achieve the effect of not easy to deactivate, reduce cost and high activity

Active Publication Date: 2014-10-15
黄志忠
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But in the prior art, the carbonate solvent price represented by DMC, EMC and DEC is relatively expensive, and there is no method to prepare the above-mentioned carbonate mixed solvent in the prior art
In addition, in the prior art, when using the transesterification method to prepare EMC and DEC, strong basic catalysts and carbonate catalysts are prone to catalyst deactivation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The transesterification reaction is carried out under normal pressure in the reactor, and the raw materials are dimethyl carbonate, ethanol and ethyl acetate; the catalyst is sodium methoxide and dibutyltin oxide; the mole of dimethyl carbonate, ethanol and ethyl acetate The ratio is 1:0.75:0.25; the amount of catalyst sodium methylate and dibutyltin oxide is respectively 0.75wt% and 0.25wt% of the total amount of raw materials (dimethyl carbonate, ethanol and ethyl acetate). The transesterification reaction is divided into two stages, the reaction temperature of the first stage is 80° C., and the reaction time is 20 minutes; the reaction temperature of the second stage is 120° C., and the reaction time is 30 minutes. After separation of low-boiling substances with a boiling point of methanol below 70°C by distillation, the obtained fraction content of 90-91°C is: 15.8wt%, and the fraction content of 108-110°C is: 21.5wt%, and the fraction content of 126-128°C For: 18.5...

Embodiment 2

[0022] Carry out transesterification reaction under the pressure condition of 0.2MPa in the reactor, the molar ratio of raw material dimethyl carbonate and ethanol, isobutyl acetate is 1: 1: 0.5; 1.0 wt% and 0.50 wt% of the total amount. The transesterification reaction is divided into two stages, the reaction temperature of the first stage is 80°C, and the reaction time is 20min; the reaction temperature of the second stage is 130°C, and the reaction time is 30min. After separation of low-boiling substances with a boiling point of methanol below 70°C by distillation, the obtained fraction content of 90-91°C is: 10.2wt%, and the fraction content of 108-110°C is: 18.5wt%, and the fraction content of 126-128°C For: 25.5wt%, fraction above 130°C: 15.7wt%. The carbonate-based mixed solvent obtained in the present invention can replace paint solvents containing 90-140°C boiling point components, such as toluene, xylene series, etc.; and the toxicity of the carbonate-based mixed so...

Embodiment 3

[0024] The transesterification reaction is carried out under the pressure condition of 0.2MPa in the reactor, the molar ratio of the raw material dimethyl carbonate, isopropanol and isobutyl acetate is 1:1:0.5; the catalyst is sodium ethylate, triethanolamine and tetratitanate The consumption of butyl ester is respectively 0.5wt%, 0.5wt% and 0.5wt% of the total amount of raw materials. The transesterification reaction is divided into two stages. The reaction temperature of the first stage is 85° C., and the reaction time is 20 minutes; the reaction temperature of the second stage is 135° C., and the reaction time is 30 minutes. After separation of low-boiling substances with a boiling point of methanol below 70°C by distillation, the obtained fraction content of 90-91°C is: 10.5wt%, and the fraction content of 108-110°C is: 17.5wt%, and the fraction content of 126-128°C For: 28.5wt%, fraction above 130°C: 20.1wt%. The carbonate-based mixed solvent obtained in the present inve...

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Abstract

The invention relates to a method for producing safe and environment-friendly carbonic ester series mixed solvents. Raw materials of dimethyl carbonate and an initiator in the presence of a catalyst are subjected to a transesterification. The initiator comprises a first initiator, which is at least one selected from the group containing ethanol, isopropyl alcohol, isobutyl alcohol, n-butyl alcohol, glycol, diglycol and glycerol, and a second initiator, which is least one selected from the group consisting of ethyl acetate, isopropyl acetate, SEC-butyl acetate and isobutyl acetate. The catalyst comprises a first catalyst, which is at least one selected from the group consisting of sodium methoxide, sodium ethoxide, potassium methoxide, potassium ethoxide, triethanolamine and polyethylene glycol, and a second catalyst, which is at least one selected from the group consisting of dibutyltin oxide, tetrabutyl titanate, rare earth salt and rare earth oxide. The through selection of catalyst and initiator, the invention uses an ester exchange method to obtain carbonic ester series solvents with different boiling points, which can be used as green and environment-friendly coating solvents.

Description

technical field [0001] The invention relates to the field of chemical industry, and more specifically, the invention relates to a method for preparing a carbonate-based mixed solvent by using dimethyl carbonate as a raw material through transesterification. Background technique [0002] The boiling point of dimethyl carbonate (DMC) is 90°C, which is between ethyl acetate (73°C) and toluene (110°C); it was recognized as a non-toxic solvent by the European Union in 1993; and it is compatible with polyurethane, polyacrylic acid, It is compatible with various resins such as nitrocellulose, and miscible with various industrial solvents such as benzene, ketones, acetates, and ethers. As a green solvent, it began to be popularized and used in the market at the end of the last century. [0003] Ethyl methyl carbonate (EMC) has a boiling point of 108-109°C. As an asymmetric carbonate compound, it is mainly used as a solvent and an intermediate in organic synthesis, especially as a so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/06C09D7/12
CPCC07C68/06C09D7/20C07C69/96
Inventor 黄清粘张辉郑秋鉴廖启武
Owner 黄志忠
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