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Method for microwave synthesis of glyceryl caprylate-caprate

A technology for glyceryl capric acid and microwave synthesis, which is applied in the fields of oleochemical technology and fine chemical industry, can solve problems such as few reports on the microwave synthesis of caprylic acid-glyceryl capric acid, and avoid product color darkening, yield and esterification. The effect of high rate and shortening the time of maintaining high temperature

Inactive Publication Date: 2017-05-24
广州星业科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are not many reports on the microwave synthesis of caprylic-capric glycerides, and the rapid synthesis of caprylic-capric glycerides with a high esterification rate by using a specific catalyst composition has not yet been reported.

Method used

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  • Method for microwave synthesis of glyceryl caprylate-caprate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0026] In Examples 1-5:

[0027] The catalyst is p-toluenesulfonic acid (PTSA), phosphoric acid (H 3 PO 4 ), hypophosphorous acid (H 2 PO 4 ), phosphotungstic acid [P 2 o 5 24 (WO 3 )·44(H 2 O)], sulfamic acid (NH 2 SO 3 H), sodium bisulfate (NaHSO 4 ), 732 type strongly acidic styrene-based cation exchange resin, 1-butyl-3-methylimidazolium tetrafluoroborate (C 8 h 15 N 2 BF 4 ), 1-butyl-3-methylimidazolium hexafluorophosphate (C 8 h 15 N 2 PF 6 ) A combination of two or more of them.

[0028] In comparative examples 1-4: the catalyst is one of the above catalysts.

Embodiment 1

[0030] 1. Preparation:

[0031] (1) Add caprylic acid, capric acid (mass ratio is 2:1) and glycerin (the total amount of caprylic acid and capric acid to glycerin molar ratio is 3.15:1) into the reactor, the total weight of reactants is about 500g, and the microwave power is 500W, Use phosphoric acid and hypophosphorous acid (phosphoric acid accounts for 45% by mass fraction, hypophosphorous acid accounts for 55% by mass fraction) as catalyst, the quality of catalyst is 1.0% of glycerol, three-stage program temperature rises and reduces pressure, is heated up to with the speed of 10 ℃ / min Keep at 100°C for 10 minutes, then raise the temperature to 120°C at a rate of 10°C / min and hold for 10 minutes, at 120°C, depressurize to -0.055MPa, keep for 10 minutes and then raise the temperature to 150°C at a rate of 10°C / min. Continue to reduce the pressure to -0.095MPa, and react at 150°C and -0.095MPa for 5h to obtain the crude product of caprylic acid-capric glyceride.

[0032] (2)...

Embodiment 2

[0035] 1. Preparation:

[0036](1) Add caprylic acid, capric acid (mass ratio: 9:5) and glycerin (the total amount of caprylic acid and capric acid to glycerin molar ratio is 3.35:1) into the reactor, the total weight of the reactants is about 500g, and the microwave power is 500W, Use p-toluenesulfonic acid, phosphoric acid, hypophosphorous acid mixture as catalyst (p-toluenesulfonic acid 15%; Phosphoric acid: 30%; Hypophosphorous acid: 55%, mass fraction), the quality of catalyst is 1.81% of glycerol, three sections of programmed temperature rise Reduce pressure, raise the temperature to 110°C at a rate of 10°C / min and keep it for 10 minutes, then raise the temperature to 150°C at a rate of 10°C / min and keep it for 10 minutes. Raise the temperature to 180°C at a rate of 10°C / min, continue to reduce the pressure to -0.095MPa, and react at 180°C and -0.095MPa for 3h to obtain the crude caprylic-capric glyceride.

[0037] (2) The crude product of caprylic-capric glyceride was ...

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Abstract

The invention provides a preparation method for microwave synthesis of glyceryl caprylate-caprate. Caprylate-caprate and glycerin are reacted in the presence of a compound catalyst, and a glyceryl caprylate-caprate product is prepared by microwave synthesis. According to the method, the molar ratio of caprylate and caprate in the glyceryl caprylate-caprate is regulated, catalysis of the compound catalyst is combined, and a frequency band of 300 to 3,000MHz is adopted for microwave synthesis, so that the high-quality glyceryl caprylate-caprate of which the molar ratio of the caprylate and the caprate is controllable can be efficiently and rapidly prepared. According to the method, a high esterification rate can be achieved, and meanwhile, the energy consumption and the production cost of a reaction process can be remarkably reduced.

Description

technical field [0001] The invention belongs to the fields of oleochemical technology and fine chemical technology, and in particular relates to a method for synthesizing caprylic-capric glyceride by microwave. Background technique [0002] Medium-chain fatty acid glycerides have unique physical and chemical properties and metabolic characteristics, and have been widely used in food, medicine, cosmetics, nutrition and other fields. In terms of preparation mechanism, there are currently two methods for synthesizing medium-chain fatty acid glycerides at home and abroad: chemical method and enzymatic method. Among them, the enzymatic synthesis technology is still immature and is still in the laboratory stage. Industrialized glyceride products are mostly synthesized by chemical methods, and the key technology lies in the reasonable selection of catalysts and the control of reaction conditions. Conventional chemical synthesis methods require esterification reaction time of more...

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 李建孟巨光郑成莫林峰
Owner 广州星业科技股份有限公司
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