Preparation method of high-substitution-degree octenyl succinic acid modified starch

A technology of octenyl succinic anhydride ester and octenyl succinic acid, which is applied in the field of preparation of high-substitution octenyl succinic acid starch ester, can solve the problems of difficulty in meeting the needs of industrial production, low reaction efficiency of aqueous phase method, and environmental pollution Large and other problems, to achieve good emulsion properties and the ability to embed substances, improve esterification efficiency, and enhance the effect of reactivity

Inactive Publication Date: 2021-12-28
JIANGNAN UNIV
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Problems solved by technology

The aqueous phase method uses water as the reaction medium, adds octenyl succinic anhydride to the starch milk at a certain temperature, and uses alkaline reagents such as sodium hydroxide to keep the starch milk in the range of pH 8 to 10 for reaction, because the acid anhydride is insoluble In water, and prone to side reactions, the reaction efficiency of the water phase method is low, the degree of substitution of starch octenyl succinate ester obtained by most water phase methods is 0.01 to 0.02, and the reaction efficiency is about 10%; the dry method is to combine the organic Solvent-diluted octenyl succinic anhydride was sprayed into starch with a lower moisture content for heating reaction. "Effect of Degree of Substitution of Octenyl Succinate Starch on the Emulsification Activity on Different Oil Phases" reported that natural starch was heated and dried, and mixed with ice The mixture of acetic acid and acid anhydride is reacted in a stainless steel sealed pot, and the DS of the obtained starch acetate product is 0.5-2.5, and the reaction efficiency can reach 100%. The dry process is relatively simple, low cost, high reaction efficiency, and small environmental impact , but because the dry material cannot be fully mixed evenly, resulting in many impurities and low quality of the product; the organic phase method mainly involves the reaction of starch with octenyl succinic anhydride in an inert organic solvent, and usually requires the addition of an alkaline organic solvent (usually certain toxicity) to control the reaction pH value, the method for preparing starch octenyl succinate by the organic phase method recorded in "Research on the Preparation of Starch Octenyl Succinate with High Substitution Degree and Its Embedding Properties" needs to add an organic activator Pyridine, the degree of substitution of the obtained product is 1-2; the reaction efficiency of the organic phase method is high, and the degree of substitution of the prepared starch octenyl succinate is high, but its production cost is high, the environment is polluted, and due to organic The introduction of solvent and the product produced by the residual organic phase method are not suitable for food or cosmetics
[0004] In view of the above deficiencies, more and more current researches focus on the direction of composite modification, such as acidolysis-esterification, moist heat-esterification, enzymatic hydrolysis -Esterification and esterification-enzymatic hydrolysis, esterification-crosslinking, etc., these methods have improved the degree of substitution of the product to a certain extent, and also improved the reaction efficiency, but involve time-consuming, energy-consuming, and difficult to meet industrialization production needs, etc.

Method used

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  • Preparation method of high-substitution-degree octenyl succinic acid modified starch
  • Preparation method of high-substitution-degree octenyl succinic acid modified starch
  • Preparation method of high-substitution-degree octenyl succinic acid modified starch

Examples

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Effect test

Embodiment 1

[0058] Prepare a 20% ethanol solution, weigh a certain amount of cornstarch and place it in a glass container, add the ethanol solution according to the ratio of starch: ethanol solution = 2:3, stir evenly, and send it to a microreactor for heating and heat preservation reaction. The parameters are: heat the reaction substance to 90°C, and keep it warm for 30 minutes to obtain mild alcohol hydrothermal treatment of corn starch. Transfer the product to a certain amount of ethanol solution to make the starch milk with a concentration of 20%. After mixing the two, Send it into a container for reaction, weigh 3% octenyl succinic anhydride and wait for the reaction. The reaction parameters are as follows: the reaction temperature is 45° C., the reaction pH value is 9, and the reaction time is 3 hours. After the reaction, wash with alcohol and filter with suction, put it in a microwave vacuum oven for drying, and dry it at 50°C for 24 hours, then take out the product and put it in a...

Embodiment 2

[0060] Prepare a 40% ethanol solution, weigh a certain amount of cornstarch and place it in a glass container, add the ethanol solution according to the ratio of starch: ethanol solution = 1:4, stir evenly, and send it to a microreactor for heating and heat preservation reaction. The parameters are: heat the reaction substance to 70°C and keep it warm for 30 minutes to obtain mild alcoholic hydrothermal treatment of cornstarch. Transfer the product to a certain amount of ethanol solution to make the starch milk with a concentration of 30%. After mixing the two, Send it into a container for reaction, weigh 13% octenyl succinic anhydride and wait for the reaction. The reaction parameters are as follows: the reaction temperature is 35° C., the reaction pH value is 8.0, and the reaction time is 5 hours. After the reaction, wash with alcohol and filter with suction, put it in a microwave vacuum drying oven for drying, and dry it at 50°C for 24 hours, then take out the product and p...

Embodiment 3

[0062] Prepare a 50% ethanol solution, weigh a certain amount of cornstarch and place it in a glass container, add the ethanol solution according to the ratio of starch: ethanol solution = 3:7, stir evenly, and send it into a microreactor for heating and heat preservation reaction. The parameters are: heat the reaction substance to 80°C and keep it warm for 30 minutes to obtain mild alcoholic hydrothermal treatment of corn starch. Transfer the product to a certain amount of ethanol solution to make the starch milk with a concentration of 35%. After mixing the two, Send it into a container for reaction, weigh 20% octenyl succinic anhydride and wait for reaction. The reaction parameters are as follows: the reaction temperature is 40° C., the reaction pH value is 8.3, and the reaction time is 4 hours. After the reaction, wash with alcohol and filter with suction, put it in a microwave vacuum drying oven for drying, and dry it at 50°C for 24 hours, then take out the product and pu...

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Abstract

The invention discloses a preparation method of high-substitution-degree octenyl succinic acid modified starch, and belongs to the technical field of starch modification. The method comprises the following steps of: carrying out heat treatment on starch in an alcoholic solution; and carrying out esterification modification on octenyl succinic anhydride to obtain octenyl succinic acid modified starch. The octenyl succinic acid modified starch is prepared through composite modification, so that the substitution degree is greatly improved, the water absorption rate, hydrophobicity and emulsifying property are greatly improved, the substitution degree reaches 0.07-0.23, the water absorption rate reaches 900-1400%, and the oil absorption rate reaches 200-400%. Besides, the octenyl succinic acid modified starch achieves a small-amount and high-efficiency effect in application; the emulsibility index of an emulsion is measured by a spectrophotometer, and the emulsibility index of the octenyl succinic acid modified starch prepared by alcohol-water treatment is 1400-3000; and the emulsion prepared by a high-speed shearing machine still keeps stable and has certain flowability within 30 days.

Description

technical field [0001] The invention belongs to the technical field of starch modification, in particular to a method for preparing starch octenyl succinate with a high degree of substitution. Background technique [0002] Starch octenyl succinate is one of the important modified starches, generally in the form of sodium starch octenyl succinate. It is a kind of starch ester obtained from raw starch or starch derivatives through esterification of octenyl succinic anhydride or enzymatic hydrolysis. It is a polymer emulsifier with surface activity and has thickening properties. Sex, stability and certain water absorption and water retention, as well as the advantages of being edible and biodegradable, have a variety of functions and excellent comprehensive performance. [0003] There are three main methods for preparing starch octenyl succinate: aqueous phase method, dry method and organic phase method. The aqueous phase method uses water as the reaction medium, adds octenyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B31/04B01J20/24B01J20/30B01J13/04A01N25/30A23L29/30A61K8/73A61K47/36A61Q19/00
CPCC08B31/04B01J20/24B01J13/04A23L29/30A61K8/732A61K47/36A61Q19/00A01N25/30A61K2800/10
Inventor 周星江露陈丽华金征宇王韧赵建伟柏玉香龙杰谢正军
Owner JIANGNAN UNIV
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