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: 2013-11-20
ADANA FOOD TECH LIUZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the general solvent-free method has a high reaction temperature, the reaction is not easy 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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  • Preparation method of sucrose ester

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Add 4g of calcium oxide as a dewatering agent to 30g of methyl stearate, stir to remove a small amount of water and free fatty acids in the methyl stearate, and then transfer the dehydrated methyl stearate to a three-necked bottle Add 51g of crushed and ground sucrose, use 3.2g of calcium oxide as a catalyst, quickly stir and evenly disperse for 30 minutes, adjust and set the oil bath temperature to 130°C, synthesize sucrose ester under normal pressure or reduced pressure, continue stirring, Stop heating after 4 hours of reaction, filter the product to remove the catalyst, transfer the reaction liquid to a separatory funnel, let stand for stratification, remove the lower aqueous phase, and then wash the upper oil phase with distilled water until it is neutral, and then The product is distilled under reduced pressure at 80°C to obtain pure sucrose ester.

Embodiment 2

[0024] Add 6g of calcium oxide as a dewatering agent to 36g of methyl stearate, stir to remove a small amount of water and free fatty acids in the methyl stearate, and then transfer the dehydrated methyl stearate to a three-necked bottle Add 103g of crushed and ground sucrose, use 6.9g of calcium oxide as a catalyst, quickly stir and uniformly disperse for 30 minutes, adjust and set the oil bath temperature to 90℃, synthesize sucrose ester under normal pressure or reduced pressure, continue stirring, After 2 h of reaction, stop heating, filter the product to remove solid catalyst, transfer the reaction liquid to a separatory funnel, let stand for stratification, remove the lower water phase, and then wash the upper oil phase with distilled water until it is neutral, then The product is distilled under reduced pressure at 80°C to obtain pure sucrose ester.

Embodiment 3

[0026] Add 7g of calcium oxide as a water remover to 42g of methyl stearate, stir to remove a small amount of water and free fatty acids in the methyl stearate, and then transfer the dehydrated methyl stearate to a three-necked bottle Add 217g of crushed and ground sucrose, use 15.5g of calcium oxide as a catalyst, quickly stir and evenly disperse for 30 minutes, adjust and set the oil bath temperature to 160°C, synthesize sucrose ester under normal pressure or reduced pressure, continue stirring After the reaction has proceeded for 42 hours, stop heating, filter the product to remove the solid catalyst, transfer the reaction liquid to a separatory funnel, stand for stratification, remove the lower aqueous phase, and then wash the upper oil phase with distilled water until it is neutral, then The product is distilled under reduced pressure at 80°C to obtain pure sucrose ester.

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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 non-ionic 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, microemulsification method, solvent-free method and enzymatic method. The solvent method uses DMF or DMSO as solvents, but both of these solvents are toxic, which limits the application of sucrose esters in food and other industries. The microemulsification 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 homogeneous. The solvent-free method is to add emulsifiers or surfactants to the reaction system to make the molten phase into a homogeneous phase, and the reaction is stable. However, the general solvent-free method has a higher reaction temperature, the reaction is not easy to proceed, the yield is low, and the product ...

Claims

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Application Information

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Patent Type & Authority Applications(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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