The preparation method of sucrose ester

A technology of sucrose ester and sucrose, applied in the field of non-ionic surfactants, can solve the problems of unguaranteed product quality, complicated separation and purification steps, easy to generate a large amount of waste water, etc., to achieve product safety, simple pretreatment method, and satisfactory Purity and non-toxic properties of the required effect

Active Publication Date: 2016-04-27
ADANA FOOD TECH LIUZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction temperature of the general solvent-free method is high, the reaction is difficult to carry out, the yield is low, and the product quality cannot be guaranteed.
Moreover, the current solvent-free method usually uses alkali metal hydroxide such as potassium hydroxide or sodium hydroxide as a catalyst, and the catalyst residue in the product is serious, which strictly limits its application in the food industry. waste water

Method used

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  • The preparation method of sucrose ester

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Experimental program
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Effect test

Embodiment 1

[0022] 4g of calcium oxide is added in 30g methyl stearate as dewatering agent, stir, remove a small amount of water and free fatty acid in methyl stearate, then the methyl stearate after dewatering is transferred to three-necked bottle , add 51g of crushed and ground sucrose, use 3.2g of calcium oxide as a catalyst, stir and disperse evenly for 30 minutes, adjust and set the oil bath temperature to 130°C, synthesize sucrose ester under normal pressure or reduced pressure, and continue stirring. After the reaction was carried out for 4 hours, the heating was stopped, the product was filtered to remove the catalyst, the reaction solution was transferred to a separatory funnel, the layers were left to stand, the lower water phase was removed, and the upper oil phase was washed with distilled water until it was neutral. The purer sucrose ester can be obtained by vacuum distillation of the product at ℃.

Embodiment 2

[0024] 6g calcium oxide is added in 36g methyl stearate as dewatering agent, stir, remove a small amount of water and free fatty acid in methyl stearate, then the methyl stearate after dewatering is transferred to three-necked bottle Add 103g of crushed and ground sucrose, use 6.9g of calcium oxide as a catalyst, stir and disperse evenly for 30 minutes, adjust and set the oil bath temperature to 90°C, synthesize sucrose ester under normal pressure or reduced pressure, and continue stirring. After the reaction was carried out for 2 hours, the heating was stopped, the product was filtered to remove the solid catalyst, the reaction solution was transferred to a separatory funnel, and the layers were left to stand, the lower water phase was removed, and the upper oil phase was washed with distilled water until it was neutral, and then in Purified sucrose esters can be obtained by vacuum distillation of the product at 80°C.

Embodiment 3

[0026] 7g calcium oxide is added in 42g methyl stearate as dewatering agent, stir, remove a small amount of water and free fatty acid in methyl stearate, then the methyl stearate after dewatering is transferred to three-necked bottle In the process, add 217g of crushed and ground sucrose, use 15.5g of calcium oxide as a catalyst, stir and disperse evenly for 30 minutes, adjust and set the oil bath temperature to 160°C, synthesize sucrose ester under normal pressure or reduced pressure, and continue stirring After the reaction is carried out for 42 hours, the heating is stopped, the product is filtered to remove the solid catalyst, the reaction solution is transferred to a separatory funnel, the layers are left to stand, the lower water phase is removed, and the upper oil phase is washed with distilled water until it is neutral, and then Purified sucrose esters can be obtained by distilling the product under reduced pressure at 80°C.

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Abstract

The invention discloses a preparation method of sucrose ester, which belongs to the technical field of non-ionic surfactants. The method comprises the following steps of: removing a small amount of water and free fatty acids out of fatty acid methyl ester at first, and then adding a solid catalyst in the water-removed fatty acid methyl ester, mixing uniformly and adding sucrose in a certain ratio. In the existing industrial preparation of sucrose ester, an alkali metal hydroxide is commonly used as a catalyst, and subsequent product purification steps are cumbersome, and lots of wastewater is generated; however, according to the preparation method disclosed by the invention, a common industrial alkaline earth metal oxide is used as the solid catalyst, the reaction conditions are moderate, and the solid catalyst is not left in the product, can be repeatedly utilized and is environment-friendly and thus cost is reduced.

Description

technical field [0001] The invention relates to the technical field of nonionic surfactants, in particular to a method for sucrose esters. Background technique [0002] There are four main methods for the synthesis of sucrose esters: solvent method, microemulsion method, solvent-free method and enzyme-catalyzed method. The solvent method uses DMF or DMSO as the solvent, but these two solvents are toxic, which limits the application of sucrose esters in food and other industries. The microemulsion method uses propylene glycol or water instead of the toxic solvent used in the solvent method, and adds an emulsifier to make the reaction system approximately a homogeneous system. The solvent-free method is to make the molten phase into a homogeneous phase by adding emulsifier or surfactant in the reaction system, and the reaction is stable. However, the general solvent-free method has high reaction temperature, is difficult to carry out the reaction, and the yield is low, and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/06C07H1/00
Inventor 牛宝乐常志东吴国勇
Owner ADANA FOOD TECH LIUZHOU
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