Method for preparing starch sulphate with high degree of substitution

A starch sulfate, high degree of substitution technology, applied in the field of synthesis of fine functional polymer materials, can solve the problems of harsh treatment process, high energy consumption, equipment corrosion, etc., achieve high degree of sulfonation reaction, convenient reaction operation, convenient The effect of recycling

Inactive Publication Date: 2011-04-13
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The usual starch sulfate esterification technology uses concentrated sulfuric acid or chlorosulfonic acid as the esterification agent, both of which are highly corrosive or highly toxic, have high requirements for reaction equipment and operation, are difficult to post-process, and are extremely difficult to apply on a large scale. Large, and the obtained starch sulfate degree of substitution is generally not high, for example, in CN1911852A, with highly toxic chlorosulfonic acid as esterifying agent in chlorinated hydrocarbon solvent, adopt semi-dry method to obtain the maximum degree of substitution starch sulfate ester of 0.12, However, in CN101284878A, concentrated sulfuric acid is used to react at a low temperature of -10 to 0°C. Although starch sulfate with a substitution degree of up to 0.6 is obtained, the whole process needs to be completed at low temperature, with high energy consumption, serious equipment corrosion, and relatively harsh treatment process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Take cornstarch and pre-bake it in an oven at 105°C for 4 hours;

[0028] (2) Weigh 100 g of cornstarch treated according to step (1), put it into a reaction kettle, add 500 g of DMF, stir at a constant speed of 45 rpm for 4 hours at a temperature of 40 ° C, add 150 g of sulfur trioxide pyridine powder, and simultaneously pass it into a dry Nitrogen, heated to 90 ° C constant temperature reaction for 6 hours, then added 10g of isopropanol, finished after 2 hours;

[0029] (3) After the reaction is over, wait for the system to cool down, pour out the mixed solution from the there-necked flask, perform suction filtration, take the filter cake, wash with absolute ethanol, and suction filter 3 times, then use 0.5mol / L alkaline ethanol solution (sodium hydroxide is dissolved in 95% ethanol solution by volume and prepared, the following examples are the same) washing and suction filtration until the product pH value is neutral, and then repeated suction filtration 3 times...

Embodiment 2

[0033] (1) Take tapioca starch and pre-bake it in an oven at 105°C for 4 hours;

[0034] (2) Weigh 50g of cornstarch treated according to step (1), put it into a three-necked bottle, add 200g of DMF, stir at a constant speed of 45rpm for 6 hours at a temperature of 60°C, add 250g of sulfur trioxide pyridine powder, and simultaneously introduce Dry nitrogen, heat up to 95°C and react at a constant temperature for 12 hours, then add 10g of isopropanol, and finish after 2 hours;

[0035] (3) After the reaction is over, wait for the system to cool down, pour out the mixed solution from the there-necked flask, perform suction filtration, take the filter cake, wash with absolute ethanol, and suction filter 3 times, then use 0.8mol / L alkaline ethanol solution , washing and suction filtration until the pH value of the product is neutral, and then repeated suction filtration 3 times with 95% ethanol solution to obtain starch sulfate with a high degree of substitution.

[0036] Using 7...

Embodiment 3

[0039] (1) Take wheat starch and pre-bake it in an oven at 105°C for 4 hours;

[0040] (2) Weigh 50g of cornstarch treated according to step (1), put it into a three-necked bottle, add 150g of DMF, stir at a constant speed of 45rpm for 6 hours at a temperature of 60°C, add 250g of sulfur trioxide pyridine powder, and simultaneously feed Dry nitrogen, continue the constant temperature reaction for 12 hours, then add 200g of ethanol, and finish after 2 hours;

[0041] (3) After the reaction is over, wait for the system to cool down, pour out the mixed solution from the there-necked flask, perform suction filtration, take the filter cake, wash with absolute ethanol, and suction filter 3 times, then use 0.5mol / L alkaline ethanol solution , washing and suction filtration until the pH value of the product is neutral, and then repeated suction filtration 3 times with 95% ethanol solution to obtain starch sulfate with a high degree of substitution.

[0042] Using 78% (v / v) ethanol so...

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Abstract

The invention discloses a method for preparing starch sulphate with high degree of substitution. In the method, sulfur trioxide pyridine is taken as an esterifying agent, dimethylformamide is taken as a dissolvent, and the sulfur trioxide pyridine and the dimethylformamide are used for esterfying starch so as to obtain the starch sulphate with high degree of substitution being 0.2-0.9, wherein the mass ratio of the sulfur trioxide pyridine to the starch is (1:1)-(5:1). Solid sulfur trioxide pyridine is taken as a sulfonating agent, so that the method is easy to control, the reaction operation is convenient and the sulfonation reaction degree is higher; in addition, by utilizing the method, corrosion of strong acid liquids on equipment can be avoided; and the dissolvent is convenient to recycle, thus preferably avoiding pollution to environments.

Description

technical field [0001] The invention particularly relates to a method for preparing starch sulfate with a high degree of substitution, which belongs to the field of synthesis of fine functional polymer materials. Background technique [0002] Polysaccharide sulfate is a sugar derivatized substance that has anti-HIV activity, anti-tumor and anti-virus activities, and also has anti-coagulant and pepsin-inhibiting effects. It has high research value and wide application in the fields of biomedicine and medical materials prospect. [0003] Starch sulfate is the product of starch sulfation. Through sulfation reaction, polysaccharide sulfate with appropriate molecular weight can be obtained, and macromolecular starch sulfate with surface activity can also be obtained. [0004] Starch sulfate is also an important starch derivative. At present, starch sulfate is not yet commercially competitive in terms of physical and chemical properties and production costs, but in the field of b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B31/02
Inventor 陈玉放李建陈文宁侯成敏
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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