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Synthesizing, purifying and identifying method of citric acid diethyl ester

A technology of triethyl citrate and citric acid, which is applied in the field of hydrothermal azeotropic synthesis of diethyl citrate, can solve the constraints on the industrial production of diethyl citrate and the lack of synthesis of diethyl citrate , purification methods, and problems affecting the application of diethyl citrate

Inactive Publication Date: 2010-07-14
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ethyl citrate is mostly a mixture of monoethyl citrate, diethyl citrate, and triethyl citrate. At present, there is a lack of effective synthesis and purification methods for diethyl citrate. Therefore, diethyl citrate Ester cannot be purchased on the market, which restricts the industrialized production of diethyl citrate and also affects the application of diethyl citrate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The first step is carried out in a 1000ml reaction kettle with agitator, thermometer, extractor and condenser, citric acid 1mol, ethanol 372.6ml, benzene is added as an entrainer, dehydrating agent silicon dioxide is added in the extractor, and the reaction 6 hours.

[0014] The second step is to evaporate the excess ethanol and benzene from the reacted mixture through a rotary distiller at 85°C, add petroleum ether to the extractor to extract the ester layer several times, evaporate the petroleum ether at 70°C in the rotary distiller, and then extract several times with distilled water. Once, the aqueous layer was extracted, distilled under reduced pressure for 10 min, and filtered while hot to obtain colorless and transparent diethyl citrate.

[0015] The third step is to spread the silica gel G plate, activate it in the oven at 110°C for 30 minutes after drying, point citric acid, diethyl citrate and triethyl citrate respectively, develop in the chromatography tank, ...

Embodiment 2

[0017] The first step is carried out in a 1000ml three-neck flask (replacing the reaction kettle) with agitator, thermometer, extractor, condenser, citric acid 1mol, 95% ethanol 460ml, add carbon tetrachloride as entrainer, extractor Add dehydrating agent silicon dioxide in, react 3.5 hours.

[0018] In the second step, evaporate the excess ethanol and carbon tetrachloride from the reacted mixture through a rotary distiller at 62°C, add petroleum ether to the extractor to extract several times to extract the ester layer, evaporate the petroleum ether at 70°C in the rotary distiller, and then use Extract with distilled water several times, extract the water layer, distill under reduced pressure for 10 min, and filter while hot to obtain colorless and transparent diethyl citrate.

[0019] The third step is to spread the silica gel G plate, activate it in the oven at 110°C for 30 minutes after drying, point citric acid, diethyl citrate and triethyl citrate respectively, develop i...

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Abstract

The invention relates to a synthesizing, purifying and identifying method of citric acid diethyl ester, which adopts the technical scheme that: in a reactor with a mixer, a thermometer, an extractor and a condenser, the molar ratio of the citric acid and the ethanol is 1: 1 to 30, entrainer and dehydration agent are added into the reactor, the products are evaporated at the temperature of 30 to 150 DEG C and cooled after being reacted for 2 to 10 hours, petroleum ether and distilled water are sequentially extracted for a plurality of times, the water layer is extracted, the products are distilled for 10 minutes after the pressure is released, and the products are thermally filtered to obtain the citric acid diethyl ester. Citric acid, citric acid diethyl ester and triethyl citrate are respectively potted on a silicon rubber G bed board and are unfolded inside a saturate tank, the unfolding agent is: butanol: glacial acetic acid: water= 4: 1: 5, iodine and bromcresol green alcohol are respectively used for color development, and the result of the color development by the iodine and the bromcresol gren alcohol is consistent with each other, the RT value of the citric acid is 3, and the RT value of the citric acid diethyl ester and triethyl citrate is 3.6. The citric acid diethyl ester which is synthesized by the above method has the advantages of high yield, high purity, good color, low cost and the like.

Description

technical field [0001] The present invention relates to the technical field of organic coordination chemistry synthesis, specifically a kind of hydrothermal azeotropic synthesis of diethyl citrate (also known as diethyl citrate, Diethyl Citrate) method Background technique [0002] As a non-toxic, non-polluting, non-irritating and biodegradable "green chemical product", ethyl citrate is widely used in food, textile, plastic, leather, detergent, cosmetics, tobacco and other industries , as a lubricant, plasticizer, emulsifier, wetting agent, softener, detergent, conditioner, deodorant, synergist, additive and antioxidant, etc., is an additive that is absolutely safe for the human body. It can also prevent and treat acne when used in medicine. However, triethyl citrate is currently widely used and synthesized and purified. The U.S. Food and Drug Administration (FDA) has approved triethyl citrate as a non-toxic plasticizer for food packaging, medical appliances, and children's...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08
Inventor 李美如昝英欧妍陈钊桂保松姚钢炼
Owner XI AN JIAOTONG UNIV
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