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Distillation method for purifying glyceryl monobutyrate

A technology of glycerol monobutyrate and a distillation method, which is applied in the field of distillation for purifying glycerol monobutyrate, can solve the problems of reducing the content of glycerol monobutyrate, affecting the yield and the like, and achieves reduced odor, simple operation, and reaction conditions. Easy-to-control effects

Pending Publication Date: 2022-05-10
SHANDONG CHENGWU YIXIN ENVIRONMENTAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ordinary distillation and rectification technology, the liquid heating temperature is high, but the excess butyric acid in the semi-finished product of glycerol monobutyrate will continue to undergo esterification reaction with glycerol monobutyrate at a temperature higher than 95 ° C to form dibutyl glyceryl monobutyrate and glyceryl tributyrate, resulting in a significant reduction in the content of glyceryl monobutyrate, affecting its yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A distillation method for purifying monobutyrin, comprising:

[0023] Mix butyric acid, glycerin and solid acid catalyst in a ratio of 40:100:0.004 and preheat;

[0024] Adding the mixed solution into a vacuum reactor for esterification reaction to obtain raw material oil, and the raw material oil contains monobutyrin, dibutyrin, tributyrin and unreacted butyric acid and glycerin;

[0025] Put the raw material oil in a reaction tank at 80°C, maintain the pressure in the reaction tank not exceeding 50mmHg, and remove the air in the raw material oil;

[0026] Use the first short-diameter molecular distillation equipment to perform primary purification of the raw oil to remove glycerin; specific: control the operating temperature of the first short-diameter molecular distillation equipment's thin-film evaporator and molecular still to 90°C, and control the raw oil to 1mL / min, control the vacuum degree of thin film evaporator and molecular still at 35mmHg;

[0027] The s...

Embodiment 2

[0031] A distillation method for purifying monobutyrin, comprising:

[0032] Preheat butyric acid, glycerin and solid acid catalyst in a ratio of 45:100:0.006;

[0033] Adding the mixed solution into a vacuum reactor for esterification reaction to obtain raw material oil, and the raw material oil contains monobutyrin, dibutyrin, tributyrin and unreacted butyric acid and glycerin;

[0034] Put the raw material oil in a reaction tank at 85°C, maintain the pressure in the reaction tank not exceeding 50mmHg, and remove the air in the raw material oil;

[0035] The first short-diameter molecular distillation equipment is used to perform primary purification of the raw material oil to remove glycerin; specifically: the operating temperature of the thin-film evaporator and molecular still of the first short-diameter molecular distillation equipment is controlled at 93°C, and the raw material oil is controlled at 1.5 mL / min, control the vacuum degree of thin film evaporator and molec...

Embodiment 3

[0040] A distillation method for purifying monobutyrin, comprising:

[0041] Mix butyric acid, glycerin and solid acid catalyst in a ratio of 50:100:0.008 to preheat;

[0042] Adding the mixed solution into a vacuum reactor for esterification reaction to obtain raw material oil, and the raw material oil contains monobutyrin, dibutyrin, tributyrin and unreacted butyric acid and glycerin;

[0043] Put the raw material oil in a reaction tank at 90°C, maintain the pressure in the reaction tank not exceeding 50mmHg, and remove the air in the raw material oil;

[0044] Use the first short-diameter molecular distillation equipment to perform primary purification of the raw oil to remove glycerin; specific: control the operating temperature of the first short-diameter molecular distillation equipment's thin-film evaporator and molecular still to 95°C, and control the raw oil to 2mL / min, control the vacuum degree of thin film evaporator and molecular still at 50mmHg;

[0045] The se...

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PUM

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Abstract

The invention belongs to the technical field of preparation of glyceryl monobutyrate, and discloses a distillation method for purifying glyceryl monobutyrate, which comprises the following steps: raw oil is placed in a reaction tank, air in the raw oil is removed through pretreatment, and the raw oil is obtained through esterification reaction of butyric acid and glyceryl ester; short-diameter molecular distillation equipment is adopted to purify the raw oil, the operating temperatures of a film evaporator and a molecular distiller of the short-diameter molecular distillation equipment are controlled not to exceed 95 DEG C, the raw oil is controlled to be 1-2 mL / min, and the vacuum degrees of the film evaporator and the molecular distiller are controlled to be 0-50 mmHg, so that high-purity glyceryl monobutyrate is obtained; in conclusion, based on the molecular distillation method provided by the invention, the impurities such as butyric acid, glycerol, dibutyrin and tributyrin can be effectively removed, so that the peculiar smell of the glyceryl monobutyrate can be effectively reduced, and the purity of the obtained glyceryl monobutyrate finished product is ensured to reach 90% or above.

Description

technical field [0001] The invention belongs to the technical field of monobutyrin preparation, and in particular relates to a distillation method for purifying monobutyrin. Background technique [0002] Glycerol monobutyrate is an ester compound formed by the esterification of one molecule of glycerin and one molecule of butyrate, and butyric acid is bound to the first position (α position) of glycerin. In the actual production, the molar ratio of butyric acid and glycerol is 1.1:1. Under the action of catalyst, stirring and heating up, esterification reaction occurs, and glycerol monobutyrate is produced. The esterification rate is 93%. The product of glycerol monobutyrate Contains dibutyrin, tributyrin and incompletely reacted butyric acid and glycerin and other impurities. In order to extract pure monobutyrin, it is necessary to distill and rectify the above-mentioned semi-finished products containing impurities. Ordinary distillation and rectification technology, the l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/54C07C69/30
CPCC07C67/54C07C69/30
Inventor 孙献冲陈意
Owner SHANDONG CHENGWU YIXIN ENVIRONMENTAL TECH CO LTD
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