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Preparation method of diethyl sebacate in presence of catalyst namely methyl sulfonic acid

A technology of diethyl sebacate and methanesulfonic acid, which is applied in the field of preparation of diethyl sebacate, can solve the problems of ineffective treatment of three wastes, complex catalyst preparation, long reaction time, etc., and achieve large-scale Industrial production, shortening the reaction time of esterification, and the effect of short reaction time

Active Publication Date: 2015-12-09
XUZHOU CURRENCY MAGNETOELECTRICITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there have been reports in China on the catalytic preparation of diethyl sebacate with p-toluenesulfonic acid, ion exchange resin, solid acid, sodium bisulfate, ferric chloride, heteropoly acid, etc., but there are different degrees of long reaction time and large amount of ethanol And once added, the temperature rises too fast, ethanol is taken out by the solvent without participating in the reaction, the catalyst preparation is complicated, the cost is high, the product needs vacuum distillation, consumes a lot of energy, it is unsafe, and it is difficult to implement industrially. Disadvantages such as handling

Method used

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  • Preparation method of diethyl sebacate in presence of catalyst namely methyl sulfonic acid
  • Preparation method of diethyl sebacate in presence of catalyst namely methyl sulfonic acid

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Experimental program
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Embodiment 1

[0027] The selected sebacic acid, absolute ethanol, methanesulfonic acid, and cyclohexane are 99.5% analytically pure products; activated carbon is used for medicine;

[0028] Add 50 mL of cyclohexane, 44.22 g of absolute ethanol I and 2 g of methanesulfonic acid into a three-necked round-bottomed flask equipped with an electric mixer, a thermometer, a condenser, and a water separator, and add 40.45 g of sebacic acid while stirring, and control the rotation speed. Heat to reflux at 450r / min, separate the water produced by the reaction from the water separator, stop heating at 84°C, cool down to 50°C, anhydrous ethanol II 11.06g, continue to heat and reflux to 84°C, stop heating, and reflux for 1h , lower the temperature to 50°C, stand still to remove methylsulfonic acid, and obtain material liquid I, which is added with 5% sodium hydroxide aqueous solution and stirred to neutralize unreacted sebacic acid, remove the alkali aqueous layer, and obtain Feed liquid II; alkaline wat...

Embodiment 2

[0030] The selected sebacic acid, absolute ethanol, methanesulfonic acid, and cyclohexane are 99.5% analytically pure products; activated carbon is used for medicine;

[0031] Add 50mL of cyclohexane, 44.22g of absolute ethanol I, 0.3g of fresh methanesulfonic acid and 1.7g of recovered methanesulfonic acid into a flask equipped with an electric mixer, a thermometer, a condenser, and a water separator, and add them under stirring. Sebacic acid 40.45g, the speed is controlled at 450r / min, heated to reflux, the water produced by the reaction is separated from the water separator, the heating is stopped at 84°C, the temperature is lowered to 50°C, absolute ethanol II is 11.06g, continue to heat and reflux to Stop heating at 84°C, reflux for 1 hour, cool down to 50°C, stand still to remove methanesulfonic acid to obtain material liquid I, add 5% sodium hydroxide aqueous solution to the material liquid I and stir to neutralize unreacted decane acid, remove the alkaline water layer ...

Embodiment 3

[0033] The selected sebacic acid, absolute ethanol, methanesulfonic acid, and cyclohexane are 99.5% analytically pure products; activated carbon is used for medicine;

[0034] Add 50 mL of cyclohexane, 44.22 g of absolute ethanol, and 2 g of methanesulfonic acid into a flask equipped with an electric mixer, a thermometer, a condenser, and a water separator, add 39 g of sebacic acid under stirring, and recover 3.0 g of sebacic acid ( Wet weight), the speed is controlled at 450r / min, heated to reflux, the water produced by the reaction is separated from the water separator, the heating is stopped at 84°C, the temperature is lowered to 50°C, and absolute ethanol is 11.06g, and the heating is continued to reflux to 84°C to stop Heating, total reflux for 1 hour, cooling down to 50°C, standing still to remove methanesulfonic acid to obtain material liquid I, adding 5% sodium hydroxide aqueous solution to material liquid I and stirring to neutralize unreacted sebacic acid, removing A...

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Abstract

The invention discloses a preparation method of diethyl sebacate in the presence of a catalyst namely methyl sulfonic acid, and belongs to the field of catalytic synthesis of diethyl sebacate. According to the method, sebacic acid and anhydrous ethanol are taken as the raw materials, methyl sulfonic acid is taken as the catalyst, cyclohexane is taken as the water carrying agent, and after the reactions the reaction product is subjected to neutralization, water washing, distillation, and purification so as to obtain diethyl sebacate. Cyclohexane is taken as the water carrying agent, the reaction time is short, methyl sulfonic acid can be degraded, a product with a good appearance can be obtained without vacuum distillation, the acid / alkali using amount is little, the method is pollution-free; the product yield can reach at least 94% after one hour of reactions, the production cost is low, and the synthesis method is efficient and environment-friendly and can be applied to massive industrial production.

Description

Technical field [0001] The present invention involves the preparation method of dizenate, especially a method of catalysis of methylsulfonic acid. Background technique [0002] Antidicate is also known as sebate ethyl, sebate di ethyl. It is a colorless to pale yellow liquid. It has the aroma of wine, fruits, and melon. It can be mixed with organic matter such as ethanol, ether, oil, etc.It is mainly used to prepare edible flavors and daily chemical flavors such as grapes, pears, and can also be used as organic solvents, commonly used as plasticizers or organic synthetic intermediates in light and electrochemical sensors.With the increasingly improved environmental awareness of environmental protection and environmental protection regulations, the development and production of ate -diathrin ethyl has excellent development prospects. [0003] Antidic acid di ethyl is usually used as raw materials with dietic acid and water -free ethanol. Under the influence of catalysts, it is syn...

Claims

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Application Information

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IPC IPC(8): C07C69/50C07C67/08
CPCC07C67/08C07C69/50
Inventor 李敢王德堂刘颖田华夏先伟王金兴
Owner XUZHOU CURRENCY MAGNETOELECTRICITY
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