Method for preparing tributyrin

A technology of tributyrin and tributyric acid, which is applied in the field of tributyrin preparation, can solve the problems of poor catalyst selectivity and low reuse rate, and achieve high selectivity, low production cost and cost reduction Effect

Inactive Publication Date: 2018-02-09
LUTIAN CHEM CORP
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0005] In view of the above deficiencies, the present invention provides a method for preparing tributyrin to solve the problems of poor catalyst selectivity, low reuse rate, post-treatment environmental protection pressure and the like in the existing method for the preparation of n-butyrin

Method used

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  • Method for preparing tributyrin

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Effect test

Embodiment 1

[0023] A kind of preparation method of tributyrin

[0024] First, 75.6g of butyric acid and 25.1g of glycerin were added to the reaction kettle in sequence, and after stirring was started, the reaction temperature was gradually increased to 110°C. Add 3 g of ionic liquid catalyst composed of α-pyrrolidone cation and hydrogen sulfate into the reaction kettle to carry out esterification reaction. After the esterification reaction, the reaction solution was statically stratified for 15 minutes, and the tributyrin product in the upper layer and the ionic liquid catalyst in the lower layer were separated and obtained. The obtained tributyrin product was sequentially washed three times with 3% sodium hydroxide solution in alkali and water, and then a feed grade tributyrin product with a conversion rate of 75.8%, a purity of 95.2%, and an acidity value of 3% could be obtained.

Embodiment 2

[0026] A kind of preparation method of tributyrin

[0027] First, 80g of butyric acid and 25g of glycerin were added to the reactor in sequence, and after stirring was started, the reaction temperature was gradually increased to 110°C. 5 g of ionic liquid catalyst composed of α-pyrrolidone cation and p-toluenesulfonate were added into the reaction kettle to carry out esterification reaction. After the esterification reaction, the reaction solution was statically stratified for 15 minutes, and the tributyrin product in the upper layer and the ionic liquid catalyst in the lower layer were separated and obtained. The obtained tributyrin product was sequentially washed with 3% sodium hydroxide solution in alkali and water for three times, and then a feed grade tributyrin product with a conversion rate of 84.8%, a purity of 96.8%, and an acidity value of 2.6% could be obtained.

Embodiment 3

[0029] A kind of preparation method of tributyrin

[0030] First, 78g of butyric acid and 25g of glycerin were added to the reactor in sequence, and after stirring was started, the reaction temperature was gradually increased to 110°C. Add 3 g of ionic liquid catalyst composed of α-pyrrolidone cation and dihydrogen phosphate into the reaction kettle to carry out esterification reaction. After the esterification reaction, the reaction solution was statically stratified for 15 minutes, and the tributyrin product in the upper layer and the ionic liquid catalyst in the lower layer were separated and obtained. The obtained tributyrin product was sequentially washed three times with 3% sodium hydroxide solution in alkali and water, and then a feed grade tributyrin product with a conversion rate of 72.6%, a purity of 92.4%, and an acidity value of 5.8% could be obtained.

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Abstract

The invention discloses a preparation method of tributyrin. The method comprises the following steps: adding tributyric acid and glycerin according to a mol ratio being 3:(0.8-1) in order, stirring the materials, gradually increasing the reaction temperature to 100-110 DEG C, adding an acidic ion-type liquid catalyst accounting for 1-5% of total mass of tributyric acid and glycerin, and reacting the materials for 2-8 h to obtain the tributyrin product with a conversion rate being 70-90%. Compared with the traditional catalyst, the catalyst prepared by tributyric acid and glycerin has higher selectivity, the esterified tributyrin is easily separated from a reaction system, the separated ionic liquid can be continuously used, and the catalytic activity can be kept better. The preparation method has the advantages of simple process, low production cost, and convenient operation, can rapidly prepare the tributyrin product, and is suitable for industrial large-scale production.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, in particular to a method for preparing tributyrin. Background technique [0002] Tributyrin is esterified from butyric acid and glycerol. When it enters the intestinal tract of animals as a feed additive, it can be slowly released into butyric acid and glycerin under the action of pancreatic lipase, repairing the animal's small intestinal villi and inhibiting intestinal tract. Harmful bacteria, promote the absorption and utilization of nutrients. When tributyrin is used on young animals, it can effectively reduce the diarrhea and weaning stress of young animals after weaning, and increase the survival rate and daily gain of young animals. [0003] The current preparation method of tributyrin mainly uses tributyric acid and glycerin as raw materials, and by adding strong acid catalysts such as toluenesulfonic acid and phosphoric acid, under the action of water-carrying agents suc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/30
CPCC07C67/08C07C69/30
Inventor 龙平蒋弟勇辜凯德傅利才任春华陈钢宁忠培谭光军刘孔满
Owner LUTIAN CHEM CORP
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