Method and device for synthesizing triethyl citrate by applying vapor permeation dehydration technique

A technology of triethyl citrate and osmotic dehydration is applied in the separation/purification of carboxylate, the preparation of carboxylate, chemical instruments and methods, etc. Avoid secondary evaporation, high product esterification rate and high production efficiency

Inactive Publication Date: 2017-03-22
JIANGSU NINE HEAVEN HIGH TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Using ethanol as a water-carrying agent is the development direction, and some processes are as Chinese patents, "A Method for Synthesizing Triethyl Citrate" disclosed by Authorized Publication No. CN102584590 B, "A Method for Synthesizing Triethyl Citrate" disclosed by Authorized Publication No. "Preparation Method" and "A Preparation Method of Non-toxic and High-efficiency Plasticizer Triethyl Citrate" disclosed by Application Publication No. CN102336667A all describe the use of absolute ethanol as the reactant and water-carrying agent, but none of the patents mentions And the problem of ethanol recovery, and the actual amount of ethanol used in the reaction process is far greater than the reaction consumption

Method used

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  • Method and device for synthesizing triethyl citrate by applying vapor permeation dehydration technique
  • Method and device for synthesizing triethyl citrate by applying vapor permeation dehydration technique
  • Method and device for synthesizing triethyl citrate by applying vapor permeation dehydration technique

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Embodiment 1

[0036] Steam permeation dehydration technology is used for the method for synthesizing triethyl citrate, the device that adopts is as figure 1 As shown, the operation process includes the following steps:

[0037] Put 5 kg of citric acid, 6.17kg of absolute ethanol, and 45g of p-toluenesulfonic acid into the reactor 1 for heating and reaction, and carry out the esterification reaction under the catalysis of the catalyst. The temperature in the reactor is 115°C, and the rising steam in the reactor Heat and mass transfer with the descending reflux liquid in the rectification column 2, the temperature at the top of the rectification column is controlled at about 78°C, and the feed liquid (mainly ethanol) evaporated from the top of the column is condensed by the top condenser 3 and then flows into In the ethanol receiving tank 5, a part of the overhead distillate is used as the reflux liquid with a reflux ratio of 1, and the other part is used as the raw material liquid in the ste...

Embodiment 2

[0043] Steam permeation dehydration technology is used for the method for synthesizing triethyl citrate, the device that adopts is as figure 1 As shown, the operation process includes the following steps:

[0044] Put 5 kg of citric acid, a certain amount of 95vol% ethanol or absolute ethanol, and 45g of p-toluenesulfonic acid into the reaction kettle 1 for heating and reaction, and carry out the esterification reaction under the catalytic action of the catalyst. The temperature in the reaction kettle is 120°C. The ascending steam and descending reflux liquid in the still conduct heat and mass transfer in the rectification column 2, the temperature of the top of the rectification column is controlled at about 78°C, and the liquid (mainly ethanol) evaporated from the top of the tower is condensed at the top of the tower After being condensed by the device 3, it flows into the ethanol receiving tank 5, a part of the overhead distillate is used as the reflux liquid, and the reflu...

Embodiment 3

[0050] Steam permeation dehydration technology is used for the method for synthesizing triethyl citrate, the device that adopts is as figure 1 As shown, the operation process includes the following steps:

[0051] Put 5 kg of citric acid, 6.17 kg of absolute ethanol, and 45 g of catalysts (cationic catalytic resin, concentrated sulfuric acid, p-toluenesulfonic acid) into reactor 1 for heating and reaction, and carry out esterification reaction under the catalysis of the catalyst. The temperature in the reactor is The rising steam and the descending reflux liquid in the reactor conduct heat and mass transfer in the rectification column 2. The temperature at the top of the rectification column is controlled at about 78°C, and the liquid (mainly ethanol) evaporated from the top of the ) flows into the ethanol receiving tank 5 after being condensed by the tower top condenser 3, a part of the tower top distillate is used as the reflux liquid, and the reflux ratio is 1.5, and the ot...

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Abstract

The invention relates to a method and a device for synthesizing triethyl citrate by applying a vapor permeation dehydration technique, belonging to the technical field of permeation gasification membrane separation application and organism synthesis. The method comprises the following steps: adding citric acid, ethanol and a catalyst into a reaction kettle according to a certain ratio, and heating to certain temperature, wherein triethyl citrate and water are mainly generated from reactants under the catalytic action of the catalyst. In the reaction process, rising vapor and downstream backflow liquid inside the reaction kettle play roles of heat conduction and mass transfer in a rectifying column, generated ethanol and water are distilled out from the tower top of the rectifying column, and the distillate is dehydrated as a vapor permeation dehydration raw material. After the distillate is dehydrated, ethanol vapor with relatively high purity is condensed and fed back to the reaction kettle. As ethanol is adopted as a water carrying agent, water carried by the raw materials and water generated in the reaction process can be continuously removed, the reaction can be promoted to the direction of ester production, and thus the conversion rate of the reaction can be increased. According to the method and the device, the triethyl citrate is high in esterification rate and purity, ethanol amount is low, recycling process is not needed, the process is simple and the operation energy consumption is low.

Description

technical field [0001] The invention relates to a method and a device for synthesizing triethyl citrate by steam permeation dehydration technology, and belongs to the technical field of pervaporation membrane separation application and organic compound synthesis. Background technique [0002] Triethyl citrate is an important chemical raw material, mainly used as a plasticizer for thermoplastic resins such as cellulose and vinyl. In the food industry, it is widely used as an additive, antioxidant and flavor enhancer. In the tobacco industry, it is the best substitute for triacetin, a plasticizer for cellulose acetate filter rods. The U.S. Food and Drug Administration has approved triethyl citrate as a non-toxic plasticizer for food packaging, medical devices, children's toys and personal hygiene products. Therefore, researching and developing triethyl citrate has very important significance. [0003] At present, triethyl citrate is mainly synthesized in industry by ester...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/48C07C67/52C07C67/08C07C67/54
CPCC07C67/48C07C67/08C07C67/52C07C67/54C07C69/704
Inventor 郭海超相里粉娟孔维芳余从立
Owner JIANGSU NINE HEAVEN HIGH TECH
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