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Method for preparing starch high carbonate ester under supercritical condition

A supercritical and carbonate technology, applied in the production of bulk chemicals, can solve the problems of low efficiency of esterification reaction, low utilization rate of esterification agent, increased production cost, etc., to improve product quality and use effect, reduce Dosage and post-processing difficulty, the effect of increasing solubility

Active Publication Date: 2017-03-22
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High carbon esterification agent in supercritical CO 2 It is soluble in medium, but the solubility is limited. As a result, the utilization rate of the esterification agent is still low, and the efficiency of the esterification reaction is not high, especially when preparing starch percarbonate with a higher degree of substitution (>0.10). In the case of a mass ratio of about 500:1 (at this time, the molar ratio of the esterifying agent to the starch glucose unit is about 3:1), the utilization rate of the esterifying agent is less than 10% (see Henky M et al. Synthesia of fatty acid esters insupercritical carbon dioxide.Carbohydrate Polymers,2010,82(2):349, Table 1), which causes excessive waste of esterifying agent and increases production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 100 parts of tapioca starch into the mixer, weigh 5 parts of sodium hydroxide, configure it into a 10% aqueous solution of sodium hydroxide, spray it into the mixer at room temperature and stir and mix for 30 minutes to obtain the activated starch material. Put the activated starch material into the autoclave, cover and seal it, and fill it with high-pressure liquid CO 2 , Exhaust, leak detection; measure 10 parts of cyclohexane, dissolve in 4 parts of octenyl succinic anhydride, and inject the cyclohexane dissolved in octenyl succinic anhydride into the autoclave with a feeding high-pressure pump, and heat up to 50°C. Pressurize to 8.0MPa, heat and hold pressure for 3 hours, cool down to room temperature, release the pressure to normal pressure, collect additives, finally remove the solid product from the bottom of the reaction kettle, adjust the pH to 6.0-7.0, dry, pulverize, and pass through 100 mesh Sieve to get octenyl succinic acid starch ester product.

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Embodiment 2

[0029] Add 100 parts of cornstarch into the mixer, weigh 8 parts of potassium hydroxide, configure it into a 15% potassium hydroxide aqueous solution, spray it into the mixer at room temperature and stir and mix for 40 minutes to obtain the activated starch material. Put the activated starch material into the autoclave, cover and seal it, and fill it with high-pressure liquid CO 2, Exhaust, pick up leaks. Measure 240 parts of n-hexane, dissolve it in 100 parts of hexadecyl fatty acid, and inject the n-hexane dissolved in hexadecyl fatty acid into the high-pressure reactor with a feeding high-pressure pump, raise the temperature to 120°C, pressurize to 28.0MPa, and keep warm and pressurize for reaction After 6 hours, cool down to room temperature, release the pressure to normal pressure, collect additives, and finally remove the solid product from the bottom of the reaction kettle, adjust the pH to 6.0-7.0, dry, pulverize, and pass through a 100-mesh sieve to obtain hexadecyl f...

Embodiment 3

[0032] Add 100 parts of potato starch into the mixer, weigh 10 parts of sodium hydroxide, configure it into 20% sodium hydroxide aqueous solution, spray it into the mixer at room temperature and mix for 50 minutes to obtain activated starch material. Put the activated starch material into the autoclave, cover and seal it, and fill it with high-pressure liquid CO 2 , Exhaust, pick up leaks. Measure 120 parts of acetone, dissolve in 50 parts of hexadecanoic oleic acid, and inject the acetone dissolved in hexadecanyl oleic acid into the high-pressure reactor with a feeding high-pressure pump, raise the temperature to 90 ° C, pressurize to 15.0 MPa, and keep warm and pressurize for reaction For 1 hour, cool down to room temperature, release the pressure to normal pressure, collect the additives, and finally remove the solid product from the bottom of the reaction kettle, adjust the pH to 6.0-7.0, dry, pulverize, and pass through a 100-mesh sieve to obtain hexadecanoyl oleic acid s...

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PUM

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Abstract

The invention relates to a method for preparing starch high carbonate ester under a supercritical condition. Starch is taken as a raw material, C8-C18 carboxylic acid or acid anhydride of the C8-C12 carboxylic acid is taken as an esterification modifying agent, caustic alkali is taken as a catalyst, an accessory ingredient of which the mass is 0.1-0.2 time of the mass of the starch is added into a supercritical CO2 media, and the starch high carbonate ester is prepared through supercritical esterification reaction. The degree of substitution of a starch high carbonate ester product is 0.01-0.50, and the reaction efficiency of an esterifying agent is 55-90%.

Description

technical field [0001] The invention belongs to the technical field of preparation of starch deep-processing products, and in particular relates to the use of supercritical CO 2 A process for preparing starch percarbonate as a reaction medium. Background technique [0002] Starch percarbonate refers to starch esters with high-carbon lipophilic substituent groups produced by esterification of starch with fatty acids with more than eight carbons, oleic acid, lauric acid, alkenyl succinic acid, etc., or the anhydrides and mixed anhydrides of these high carbonic acids. and its derivatives. Starch percarbonate is an excellent biodegradable material with dual functions of hydrophilic and lipophilic. With the increase of the degree of substitution of lipophilic substituents and the growth of the carbon chain of substituent groups, its performance will be further improved. Enhanced, the application field will continue to expand. In view of these characteristics of starch percarbo...

Claims

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Application Information

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IPC IPC(8): C08B31/04
CPCC08B31/04Y02P20/54
Inventor 张友全谢新玲李习都白俊冯文政鞠全亮黄云浩
Owner GUANGXI UNIV
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