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Preparation method of starch octenyl succiniade under supercritical condition

An octenyl succinic acid and supercritical technology, applied in the production of bulk chemicals, etc., can solve the problems of increasing the complexity of the post-treatment process, improving the esterification efficiency of the esterification reaction, prolonging the production cycle of the product, and achieving esterification reaction High efficiency, guaranteed food safety, fast penetration effect

Active Publication Date: 2012-03-07
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The three processes have their own advantages and disadvantages. Considering that OSAS is mainly used in the fields of food and medicine, the influence of the preparation process route cannot be ignored to ensure the safety of the product.
[0003] However, the following unavoidable and difficult problems exist in the wet process using water as the medium: (1) Alkenyl succinic anhydride is a substance that is insoluble in water, and it is necessary to increase the mass transfer of alkenyl succinic anhydride by increasing the mass transfer interface In order to effectively speed up the reaction; (2) Alkenyl succinic anhydride will undergo hydrolysis reaction in acidic, neutral or alkaline environment, and the degree of hydrolysis reaction has an important impact on the reaction efficiency; (3) For the convenience of post-processing, the reaction temperature It must be controlled below the starch gelatinization temperature, the starch remains in a granular state (solid state), and the reaction system is a liquid-liquid-solid three-phase heterogeneous reaction system. The requirements for controlling the reaction conditions are quite strict, and it is difficult to improve the efficiency of the esterification reaction. Esterification efficiency; (4) Although the aqueous phase method can effectively remove impurities such as unreacted reagents, it is necessary to use water, isopropanol, acetone and other solvents to repeatedly wash the product after the reaction, which increases the complexity of the post-treatment process , which prolongs the product production cycle and greatly increases the cost of product preparation
So far, there is no report on the research results of the preparation of starch octenyl succinate by supercritical synthesis technology at home and abroad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 100 parts of cornstarch, 0.3 parts of oxidant, 5 parts of esterification agent, 2.0 parts of sodium hydroxide, 15 parts of water in the supercritical reactor, and use supercritical CO 2 As the reaction medium, at the supercritical temperature of 35°C, the supercritical pressure of 7.5MPa, and the rotation speed of 200r / min, the oxidation and esterification reactions are simultaneously carried out under the stirring state. The reaction time is 1 hour. After the reaction is completed, the extraction temperature is 40°C and the pressure is 18MPa. , CO 2 The product was extracted and purified under supercritical conditions with a flow rate of 15 L / h to obtain a powdered starch octenyl succinate product.

[0027] The product obtained in this example has a degree of substitution of 0.0052 and a viscosity of 10 mPa·s (6%, 95°C).

Embodiment 2

[0029]Add 100 parts of cornstarch, 3.8 parts of oxidizing agent, 18 parts of esterification agent, 2.0 parts of sodium carbonate, 30 parts of water in the supercritical reactor, and use supercritical CO 2 As the reaction medium, at the supercritical temperature of 80°C, the supercritical pressure of 28MPa, and the rotation speed of 400r / min, the oxidation and esterification reactions are simultaneously carried out under stirring. The reaction time is 6 hours. After the reaction is completed, the extraction temperature is 60°C and the pressure is 28MPa CO 2 The product was extracted and purified under supercritical conditions with a flow rate of 15 L / h to obtain a powdered starch octenyl succinate product.

[0030] The product obtained in this example has a degree of substitution of 0.105 and a viscosity of 12 mPa·s (6%, 95°C).

Embodiment 3

[0032] Add 100 parts of potato starch, 1.5 parts of oxidant, 10 parts of esterification agent, 22 parts of water, 3.0 parts of sodium hydroxide in the supercritical reactor, and use supercritical CO 2 As the reaction medium, at the supercritical temperature of 65°C, the supercritical pressure of 12MPa, and the rotation speed of 280r / min, the oxidation and esterification reactions are simultaneously carried out under stirring. The reaction time is 4 hours. After the reaction is completed, the extraction temperature is 45°C and the pressure is 22MPa CO 2 The product was extracted and purified under supercritical conditions with a flow rate of 20 L / h to obtain a powdered starch octenyl succinate product.

[0033] The product obtained in this example has a degree of substitution of 0.073 and a viscosity of 18 mPa·s (6%, 95°C).

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Abstract

The invention discloses a preparation method of starch octenyl succiniade under the supercritical condition. The method comprises the following steps: simultaneously performing an oxidation reaction and an esterification reaction using starch as a raw material, hydrogen peroxide or sodium hypochlorite as an oxidant, ocentyl succinic anhydride as an esterifying agent and supercritical CO2 as a reaction medium under stirring to obtain an esterification product; and extracting the esterification product with supercritical CO2 to obtain the purified powdery starch octenyl succiniade of which viscosity is 5-25mPa.s (6%, 95 DEG C) and degree of substitution is 0.005-0.12. The invention provides an environmentally-friendly green chemical synthesis method; and the method has the advantages of lowimpurity content, high reaction efficiency, good product quality and the like.

Description

technical field [0001] The invention belongs to the technical field of food additive preparation, in particular to supercritical CO 2 Process for the preparation of starch octenyl succinate as a reaction medium. Background technique [0002] Octenyl Succinic Anhydride Modified Starch (OSAS for short) is an environmentally friendly, green and safe modified starch that can be widely used in food, medicine, cosmetics, biological products and other fields. For example, the Food and Agriculture Organization of the United Nations and the World Health Organization (FAO / WHO) once commented that there is no need for special regulations on the daily allowance, and it can be used for food, and there is no limit to the scope of use. According to the results of domestic and foreign research and production literature reports related to OSAS, the OSAS preparation process mainly adopts the wet process based on the aqueous phase method, and some solvent and dry processes use organic solvent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B31/04C08B31/18
CPCY02P20/54
Inventor 张友全谢新玲童张法唐爱星覃雯
Owner GUANGXI UNIV
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