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Method for preparing ethyl sorbate through catalysis of supported p-toluenesulfonic acid

A technology of p-toluenesulfonic acid and ethyl sorbate, which is applied in the directions of carboxylate preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of long reaction time, many side reactions, poor product quality, etc. Achieve recovery and reuse, improved yield and purity, and minimal loss of catalytic activity

Active Publication Date: 2022-05-31
广西金源生物化工实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the catalysts of the acid catalysis method include sulfuric acid, p-toluenesulfonic acid, etc., but the use of sulfuric acid as a catalyst is likely to cause problems such as equipment corrosion, many side reactions, poor product quality, long reaction time, large wastewater discharge, and complicated post-treatment processes. And p-toluenesulfonic acid also has the problems that catalyst recovery is difficult and waste liquid is more; in addition, the yield of sorbic acid ethanol is not satisfactory
At the same time, the synthesis of sorbic acid is mostly obtained by condensing ketene and crotonaldehyde into polyester in the presence of a zinc salt catalyst, followed by hydrolysis and refining, but this method also has problems such as complicated process and low yield.

Method used

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  • Method for preparing ethyl sorbate through catalysis of supported p-toluenesulfonic acid
  • Method for preparing ethyl sorbate through catalysis of supported p-toluenesulfonic acid
  • Method for preparing ethyl sorbate through catalysis of supported p-toluenesulfonic acid

Examples

Experimental program
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Effect test

preparation example 1

[0046] Acidify 100 g of sodium montmorillonite with 1 L of 2 mol / L hydrochloric acid for 3 h, collect the solid by suction filtration and wash repeatedly until the pH of the filtrate is > 6, dry the filter cake under vacuum at 60°C and grind to obtain activated montmorillonite ; It was added to 500ml of 25wt% p-toluenesulfonic acid aqueous solution, stirred at 50°C for 4h, then incubated for 8h, filtered under reduced pressure, and the filter cake was repeatedly washed and then dried and ground under vacuum at 70°C. After cooling, 131 g of supported p-toluenesulfonic acid catalyst 1 was obtained. Calculated by weight method, the p-toluenesulfonic acid loading was 33 wt%.

preparation example 2

[0048]Acidify 100 g of Na-based montmorillonite with 1 L of 3 mol / L hydrochloric acid for 3 h, collect the solid by suction filtration and wash repeatedly until the pH of the filtrate > 6, dry the filter cake under vacuum at 60°C and grind to obtain activated montmorillonite It was added to 500ml of 35wt% p-toluenesulfonic acid aqueous solution, stirred at 50°C for 4h, then kept for 8h and aged for 8h, filtered under reduced pressure, and the filter cake was repeatedly washed and then dried and ground under vacuum at 70°C. After cooling, 135 g of loaded p-toluenesulfonic acid catalyst 2 was obtained. Calculated by weight method, the p-toluenesulfonic acid loading was 37 wt%.

preparation example 3

[0050] Add 1 kg (14.3 mol) of crotonaldehyde, 93 g (0.7 mol) of aluminum trichloride, and 166 g (0.7 mol) of copper isobutyrate into the reaction kettle, and continuously bubble ketene under stirring (from acetic acid at 740-780 Cracked at a high temperature), the temperature of ketene does not exceed 25°C, the temperature of the reaction solution is controlled at 35-40°C, and the reaction is stirred for 3 hours to obtain polyester. After the reaction, the unreacted crotonaldehyde was recovered by distillation under reduced pressure; 2L of concentrated hydrochloric acid was added at a temperature lower than 40°C, the temperature was raised to 70°C, stirred for 1h, and then the temperature was further raised to 95°C, and stirred for 2h. After the reaction liquid is lowered to room temperature, filter, wash with water several times, and dry to obtain crude sorbic acid; place it in 70% ethanol, heat up to 65°C and stir to dissolve completely, add activated carbon for decolorizatio...

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Abstract

The invention provides a method for preparing ethyl sorbate through catalysis of supported p-toluenesulfonic acid. According to the preparation method disclosed by the invention, the p-toluenesulfonic acid can be recycled and reused, the catalytic efficiency is also improved, and the yield and purity of the product are improved. Meanwhile, the preparation method of the sorbic acid is simple, and the yield of the sorbic acid is relatively high. Therefore, the preparation method of the ethyl sorbate is suitable for industrial application.

Description

technical field [0001] The invention relates to the technical field of chemical material preparation, in particular to a method for preparing ethyl sorbate by catalyzing loaded p-toluenesulfonic acid. Background technique [0002] Ethyl Sorbate (Ethyl Sorbate) is a colorless to light yellow transparent liquid, its molecular formula is: [0003] [0004] Ethyl sorbate is an internationally recognized low-toxic and high-efficiency food antiseptic and antifungal agent and pharmaceutical additive. It has a good prospect in flavoring, natural fruit juice antiseptic and fresh-keeping, and pharmaceuticals. [0005] Ethyl sorbate is mainly obtained by esterification of sorbate, and the esterification methods include acid catalysis and enzymatic alcoholization. Among them, the catalysts of the acid catalysis method include sulfuric acid, p-toluenesulfonic acid, etc., but the use of sulfuric acid as a catalyst is likely to cause problems such as equipment corrosion, many side reac...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/587C07C51/00C07C57/10B01J31/02
CPCC07C67/08C07C51/00B01J31/0225C07C69/587C07C57/10Y02P20/584
Inventor 程克梁顺香韦悦朱宏文黄园园蒙社兰徐小菊吴进辉岑米间黄晓磊田宇
Owner 广西金源生物化工实业有限公司
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