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Method for preparing tributyrin by utilizing PVC (Polyvinyl Chloride) reisn-supported heteropolyacid catalyst

A technology of glycerol tributyrate and loaded heteropoly acid is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc. Production efficiency, emission reduction, good reusability

Inactive Publication Date: 2017-07-14
JIANGSU RUICHEN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this patented technology, the reaction is carried out in the organic solvent chloroform, and the subsequent treatment needs to remove the organic solvent in the organic phase, which increases the difficulty of treatment, and the preparation process is not environmentally friendly.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: a kind of method that utilizes the catalyst of PVC resin load heteropolyacid to prepare tributyrin, described method is as follows: Glycerin, butyric acid and water-carrying agent are pre-mixed, preheated, then enter and be filled with catalyst The esterification reaction is carried out in the reaction column, the temperature of the esterification reaction is controlled between 140-150°C, and the reaction time is 18-20h; the catalyst used is a catalyst of macroporous PVC resin loaded with phosphotungstic acid; after the esterification reaction, vacuum distillation is used to remove Butyric acid is removed, and the removed butyric acid is returned to the reactor for recycling; zinc stearate is used as an acid-binding agent to absorb residual butyric acid to remove the butyric acid odor;

[0022] Then use active carbon to decolorize and deodorize, and refine to obtain tributyrin finished product with a content greater than or equal to 98.5%.

[0023] The cat...

Embodiment 2

[0024] Embodiment 2: a kind of method that utilizes the catalyst of PVC resin load heteropolyacid to prepare tributyrin, described method is as follows: Glycerin, butyric acid and water-carrying agent are pre-mixed, preheated, then enter and be filled with catalyst The esterification reaction is carried out in the reaction column, the temperature of the esterification reaction is controlled at 145°C, and the reaction time is 22 hours; the catalyst used is a catalyst of macroporous PVC resin loaded with silicotungstic acid; after the esterification reaction, the butyric acid is removed by vacuum distillation, and the The removed butyric acid is returned to the reactor for recycling; then calcium stearate is used as an acid-binding agent to absorb the residual butyric acid to remove the butyric acid odor; then activated carbon is used for decolorization and deodorization, and refined to obtain tributyrin finished product , the content is greater than or equal to 98.5%.

[0025] ...

Embodiment 3

[0026] Embodiment 3: a kind of method that utilizes the catalyst of PVC resin load heteropolyacid to prepare tributyrin, described method is as follows: Glycerin, butyric acid and water-carrying agent are pre-mixed, preheated, then enter and be filled with catalyst The esterification reaction is carried out in the reaction column, the temperature of the esterification reaction is controlled at 135 ° C, and the reaction time is 24 hours; the catalyst used is a catalyst of macroporous PVC resin loaded with silicotungstic acid; after the esterification reaction, the butyric acid is removed by vacuum distillation, and the removed The removed butyric acid is returned to the reactor for recycling; then molecular sieves are used as an acid-binding agent to absorb the residual butyric acid to remove the butyric acid odor; Equal to 98.5%.

[0027] The catalyst in this example is prepared by using macroporous PVC resin to load heteropolyacid by precipitation adsorption method, filtering...

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Abstract

The invention discloses a method for preparing tributyrin by utilizing a PVC (Polyvinyl Chloride) reisn-supported heteropolyacid catalyst. The method comprises the following steps of (a) pre-mixing glycerinum, butyric acid and a water-carrying agent, preheating, then feeding in a reaction column filled with the catalyst for carrying out esterification reaction, wherein the esterification reaction temperature is controlled to be 120 to 160 DEG C, the reaction time is 18 to 25h, the catalyst is the macroporous PVC reisn-supported heteropolyacid catalyst, and heteropoly acid is at least one of phosphotungstic acid and silicotungstic acid; (b) after finishing esterification reaction, utilizing vacuum distillation for removing the butyric acid, and then adopting organic alkali as an acid-binding agent for absorbing residual butyric acid; (c) then adopting activated carbon for decoloring and deodorizing, and refining to obtain a tributyrin finished product. Through the manner, the method provided by the invention is not only high in catalytic activity, good in selectivity and good in recycling, but also environmental-friendly, the production efficiency is greatly improved, and the discharge of the three wastes is reduced.

Description

technical field [0001] The invention relates to the field of preparation of chemical products, in particular to a preparation method of tributyrin. Background technique [0002] Glyceryl tributyrate, CAS No. 60-01-5, molecular formula C15H26O6, colorless oily liquid, bitter taste, should be sealed and stored in a cool place, as a substrate for the determination of lipase (Esterase) and lipase (Lipase) , plasticizers, spices. [0003] Short-chain fatty acids can provide energy for the colon, are the preferred energy source of enterocytes, and are easily absorbed in the intestinal lumen. Among them, butyric acid is the main energy source of colonic mucosal epithelial cells, accounting for about 70% of the energy produced by the oxygen consumption of short-chain fatty acids, and providing up to 30% of the maintenance energy for animals. Butyric acid has a strong creamy, cheese-like unpleasant smell, which can cause a lot of inconvenience to operators during feed processing. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/30C07C67/48
CPCC07C67/08C07C67/48C07C69/30
Inventor 陈祥宋宇飞钱建强陈伟张勇钱冬
Owner JIANGSU RUICHEN CHEM
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