Method for synthesizing high-purity sucrose monoester

A sucrose monoester, high-purity technology, applied in the field of sucrose ester manufacturing, can solve the problems of low monoester content, difficult to reach medical consumption, toxic solvents, etc., and achieve the effect of preventing caramelization reaction

Active Publication Date: 2021-08-03
武汉臻治生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the synthesis of sucrose ester has solvent method, solvent-free method, microemulsion method and phase transfer catalysis method, etc., but the reaction cost of solvent method is expensive, and the residual solvent is toxic and difficult to remove, and the product is difficult to reach medical consumption. According to the standards, the sucrose esters produced by the solvent-free method generally have low yield, low monoester content, and darker color

Method used

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  • Method for synthesizing high-purity sucrose monoester
  • Method for synthesizing high-purity sucrose monoester
  • Method for synthesizing high-purity sucrose monoester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A method for synthesizing high-purity sucrose monoesters, carried out as follows:

[0031] Step 1: Put sucrose, high-grade fatty acid ester, high-grade fatty acid salt, and catalyst in a high-energy ball mill for dry milling, the ball milling speed is 400r / min, the ball milling time is 5 hours, the protective atmosphere is nitrogen, and the ball mill is mixed evenly to obtain a mixture. Among them, the higher fatty acid ester is methyl stearate, the higher fatty acid salt is potassium stearate, the molar ratio of sucrose to higher fatty acid ester is 1:1, and the quality of higher fatty acid salt is sucrose and higher fatty acid ester. 10% of the total mass, the rest is catalyst, the catalyst is mixed with potassium carbonate and potassium hydroxide in a molar ratio of 1:2, and the molar ratio of potassium ion and sucrose in the catalyst is 2:5;

[0032] Step 2: Add the ball-milled mixture into a three-necked flask, and preheat it in a vacuum oven at 70°C for 1.5 hours;...

Embodiment 2

[0039] The difference between this embodiment and the above-mentioned Embodiment 1 is that:

[0040] Step 3: the preheated mixture is placed in an induction furnace for heating and stirring, the protective atmosphere is nitrogen, the heating temperature is 110 ° C, and the stirring is performed for 5 hours, the stirring speed is 400 r / min, and the reaction pressure is 1.5 kPa to obtain a crude product;

[0041] Other conditions remain unchanged.

Embodiment 3

[0043] The difference between this embodiment and the above-mentioned Embodiment 1 is that:

[0044] Step 3: The preheated mixture is placed in an induction furnace for heating and stirring, the protective atmosphere is argon gas, the heating temperature is 100 ° C, and stirring is performed for 3 hours, the stirring speed is 400 r / min, and the reaction pressure is 1.5 kPa to obtain a crude product ;

[0045] Other conditions remain unchanged.

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Abstract

The invention relates to a method for synthesizing high-purity sucrose monoester, which comprises the following steps of: ball-milling and uniformly mixing sucrose, higher fatty acid ester, higher fatty acid salt and a catalyst to obtain a mixture, preheating the ball-milled mixture in vacuum, and heating and stirring in an induction furnace to obtain a crude product; adding warm water into the crude product while hot, stirring, neutralizing with acetic acid, adding a calcium chloride solution, filtering and precipitating to obtain a mixed solution; carrying out ultrasonic oscillation on the mixed solution, standing for layering, and separating to obtain an aqueous solution and an organic solution; placing the organic liquid in ice water in a water bath to separate out white crystals, filtering, and drying under reduced pressure to obtain a product A; placing the aqueous solution in ice water for water bath, adding a sodium chloride solution for recrystallization, removing a lower-layer aqueous phase, and drying under reduced pressure to obtain a product B; before synthesis, ball milling is firstly performed to obtain a uniformly mixed material, and the ball-milled material is preheated in a vacuum drying oven at 50-70 DEG C, so that all the substances can be preliminarily molten at a relatively low temperature, and caramelization reaction of sucrose at a high temperature is prevented.

Description

technical field [0001] The invention relates to the field of sucrose ester manufacture, in particular to a method for synthesizing high-purity sucrose monoester. Background technique [0002] Sucrose ester is the abbreviation of sucrose fatty acid ester. It is usually obtained by esterification or transesterification of sucrose and long-chain fatty acid or fatty acid ester. It has both hydrophilic sugar groups and lipophilic fatty acid side chains. It is a kind of non- Ionic surfactant. Studies have shown that sucrose esters have good emulsifying ability, are non-toxic, and are easily biodegradable, so they are widely used in industries such as medicine, cosmetics, and food. Due to the presence of multiple hydroxyl reactive sites on the sucrose structure, the reaction product is a mixture of monoesters, diesters and polyesters. Among them, sucrose monoester has better water solubility and certain antibacterial activity, which makes sucrose monoester have higher economic va...

Claims

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Application Information

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IPC IPC(8): C07H1/00C07H13/06
CPCC07H1/00C07H13/06
Inventor 蓝平马丁·格哈特·班威尔孙强滕英来马亚茹解梦飞
Owner 武汉臻治生物科技有限公司
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