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Method for preparing starch carbonic ester by utilizing starch/CO2 and application of starch carbonic ester

A technology of CO2 and carbonate, which is applied in the field of starch carbonate preparation using starch/CO2, which can solve the problem of not being green

Inactive Publication Date: 2019-04-26
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) Ionic liquids and traditional non-green continuous dissolution systems are required

Method used

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  • Method for preparing starch carbonic ester by utilizing starch/CO2 and application of starch carbonic ester
  • Method for preparing starch carbonic ester by utilizing starch/CO2 and application of starch carbonic ester
  • Method for preparing starch carbonic ester by utilizing starch/CO2 and application of starch carbonic ester

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0084] In order to illustrate the applicable protection scope of the starch of the present invention, we use different types of starch to synthesize starch carbonate materials.

[0085] Take DMSO (15.3g) and add it to the reactor, then add DBU (18.51mmol2.8182g) and stir and mix evenly at room temperature, then add different types of starch (6.17mmol1g) and stir and mix at room temperature, so that the cornstarch is uniformly dispersed in DMSO, Maintain the reaction system CO 2 The pressure is 1.0MPa. The reaction kettle was moved into a 30°C oil bath for 3h reaction, and a translucent liquid was obtained after the reaction. Then cool to room temperature and add benzyl bromide (18.51mmol2.2mL) in situ and then react at 30°C and 4Mpa for 24h. After the reaction, a transparent light yellow liquid is obtained, which is precipitated by adding 100mL of ethanol drop by drop. After separation by filtration, use Washed once with 100 mL of ethanol to obtain a white powder.

[0086] ...

experiment example 2

[0091] In order to illustrate the applicable protection scope of the halogenated reagent of the present invention, we synthesized starch carbonate materials with different structures by using halogenated reagents with different structures.

[0092] Get DMSO (15.3g) and add in the reactor, then add DBU (18.51mmol2.8182g) and stir and mix at room temperature, then add cornstarch (6.17mmol1g) and stir and mix at room temperature, so that cornstarch is uniformly dispersed in DMSO, maintaining Reaction system CO 2 The pressure is 5MPa. The reaction kettle was moved into a 50° C. oil bath for 10 hours of reaction, and a translucent liquid was obtained after the reaction was completed. Then cool to room temperature and add a halogenating reagent in situ (the molar ratio of -X to -OH on the cellulose is 1:1), and then react at 30°C and 4Mpa for 24h. After the reaction, a transparent light yellow liquid is obtained. 100 mL of methanol was added dropwise to precipitate out, separated ...

experiment example 3

[0098] In order to illustrate the applicable protection scope of the organic base of the present invention, we synthesized starch carbonate materials by using different types of organic bases.

[0099] Take DMSO (15.3g) into the reaction kettle, then add different organic bases (18.51mmol2.8182g) and stir and mix at room temperature, then add corn starch (6.17mmol1g) and stir and mix at room temperature, so that the corn starch is evenly dispersed in DMSO , to maintain the reaction system CO 2 The pressure is 0.1 MPa. The reaction kettle was moved into an oil bath at 80° C. for 1 h, and a translucent liquid was obtained after the reaction was completed. Then cool to room temperature and add a halogenating reagent in situ (the molar ratio of -X to -OH on the cellulose is 1:1), and then react at 30°C and 4Mpa for 24h. After the reaction, a transparent light yellow liquid is obtained. Add 200mL of water dropwise to precipitate, filter and separate, and then wash with 200mL of e...

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Abstract

The invention discloses a method for preparing starch carbonic ester by utilizing starch / CO2. The method comprises the following steps: (1) mixing starch, an organic solvent and organic alkali under stirring to obtain a solution A product; (2) putting the A product into a closed environment, filling CO2 to enable the pressure of the closed environment to be 0.1 to 5 MPa and the temperature to be 30 to 80 DEG C, and performing reaction for 0.1 to 10 hours to obtain a starch-based CO2 reversible ionic liquid B product; (3) adding a halogenated compound into the B product and performing reactionfor 0.1 to 48 hours under the conditions that the CO2 pressure is 0.1 to 10 MPa and the temperature is 10 to 100 DEG C to obtain a C product, wherein the molar ratio of the halogenated compound to thestarch-based CO2 reversible ionic liquid compound is (0.1-2):1; and (4) after the reaction, adding water or lower fatty alcohol of C1 to C3 into the C product, regenerating precipitate, completely washing and drying to obtain the starch carbonic ester material. The method has the following characteristics: the starch carbonic ester material is novel in structure and adjustable in property and functionality; the synthesis method is novel; the process is simple and convenient to operate; and the solvent can be recycled.

Description

technical field [0001] The present invention relates to a kind of method for preparing starch carbonate and its application, especially a kind of using starch / CO 2 Method for preparing starch carbonate and its application. Background technique [0002] Polysaccharides in natural polymer materials are renewable and sustainable resources with abundant content and diverse structures. Among them, starch exists in various plant cells and is the polymer compound with the largest reserves. Starch has the characteristics of biodegradability and bioabsorbability, and it has a wide range of applications in the fields of pharmaceuticals, textiles, papermaking, and oil drilling. Realizing the full and high-value utilization of this renewable resource is of great significance for alleviating the crisis of oil resources and realizing the sustainable development of human society (Nonhlanhla Masina et al. Carbohydrate Polymers, 2017(157): 1226-1236). [0003] Starch carbonate is an import...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B31/04
CPCC08B31/04
Inventor 谢海波金隆明郑强
Owner GUIZHOU UNIV
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