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Preparation technology for catalytically synthetizing L-(+)-diethyl tartrate by using strong acid cation exchange resin as catalyst

A technology of strong acidic cations and diethyl tartrate, which is applied in the field of spices, can solve the problems of strong corrosiveness that easily causes side reactions, organic solvent pollution, environmental pollution, etc., and achieves excellent reactivity and selectivity, process environmental protection, exchange The effect of high capacity

Inactive Publication Date: 2015-09-23
DONGGUAN BOTON FLAVORS & FRAGRANCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the strong corrosiveness of concentrated H2SO4, it is easy to cause side reactions, and the organic solvent seriously pollutes the environment
Wang Guosheng, Ning Zhigao and others proposed in the patent CN200710011923.7 to use boric acid instead of concentrated H2SO4 to catalyze the product, but when the catalyst is washed off after the esterification reaction, a large amount of waste acid will still be formed when the catalyst and water are washed out together. waste water, and solvent recovery also pollutes the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 3.0Kg L-(+)-tartaric acid, 15.0Kg ethanol, 0.9Kg DOWEX DR 2030 strong acidic cation exchange resin into a three-necked flask equipped with a stirrer, condenser and thermometer in sequence, start stirring, and the reaction temperature is 78 ℃, the reaction time is 18 hours, after the reaction is completed, the reaction system is cooled to room temperature, the catalyst is recovered by filtration, the unreacted ethanol is removed by atmospheric distillation, and the colorless transparent liquid L-( +) - Diethyl tartrate product 2.95Kg.

Embodiment 2

[0033] Add 3.0Kg L-(+)-tartaric acid, 15.0Kg ethanol, 0.6Kg DOWEX DR 2030 type strongly acidic cation exchange resin into a three-necked flask equipped with a stirrer, condenser tube and thermometer in sequence, start stirring, and the reaction temperature is 78 ℃, the reaction time is 18 hours, after the reaction is completed, the reaction system is cooled to room temperature, the catalyst is recovered by filtration, the unreacted ethanol is removed by atmospheric distillation, and the colorless transparent liquid L-( +) - Diethyl tartrate product 2.68 Kg.

Embodiment 3

[0035] Add 3.0Kg L-(+)-tartaric acid, 15.0Kg ethanol, 0.9Kg DOWEX DR 2030 strong acidic cation exchange resin into a three-necked flask equipped with a stirrer, condenser and thermometer in sequence, start stirring, and the reaction temperature is 78 ℃, the reaction time is 12 hours, after the reaction is completed, the reaction system is cooled to room temperature, the catalyst is recovered by filtration, the unreacted ethanol is removed by atmospheric distillation, and the colorless transparent liquid L-( +) - Diethyl tartrate product 2.44 Kg.

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Abstract

The invention relates to the technical field of spices, and relates to a preparation technology for catalytically synthetizing L-(+)-diethyl tartrate by using strong acid cation exchange resin as a catalyst. The preparation technology comprises the following steps: adding L-(+)-tartaric acid, absolute ethyl alcohol and a catalyst to a reaction container, and performing a stirring and heating reaction; after the reaction is completed, cooling the reagent to room temperature, and then filtering the reagent to recycle the catalyst, wherein the catalyst is the strong acid cation exchange resin; and directly distilling a filter liquor to obtain the colorless clear liquid L-(+)-diethyl tartrate. According to the preparation technology, the yield of the L-(+)-diethyl tartrate can be improved, the technology is simple, the operation is convenient, the problems of catalysis and recycling by using a strong acid liquid and a solvent are avoided, the whole technological process is clean and environment-friendly, waste acid, waste water and waste gas cannot be generated, the environment is rarely polluted, and recycled ethyl alcohol and catalyst can be repeatedly used.

Description

technical field [0001] The invention relates to the technical field of perfumes, and relates to a preparation process for catalyzing and synthesizing L-(+)-diethyl tartrate by using strongly acidic cation exchange resin as a catalyst. Background technique [0002] The development of the flavor and fragrance industry relies on the continuous discovery of new high-quality flavor raw materials and the improvement of their preparation processes. L-(+)-diethyl tartrate is a colorless or light yellow oily viscous liquid with a faint wine aroma. It is mainly used in the fields of chiral drugs and asymmetric catalysis, and is a food flavor allowed by GB2760-1996. L-(+)-diethyl tartrate is synthesized by dehydration of L-(+)-tartaric acid and ethanol with CCl4 under the catalysis of concentrated H2SO4. Due to the strong corrosiveness of concentrated H2SO4, it is easy to cause side reactions, and the organic solvent seriously pollutes the environment. Wang Guosheng, Ning Zhigao and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/70C07C67/08
CPCY02P20/584C07C67/08C07C69/70
Inventor 马洪亮李锐吴奇林姜兴涛
Owner DONGGUAN BOTON FLAVORS & FRAGRANCES
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