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Preparation method of galloyl konjac glucomannan

A technology of galloyl and mannan, which is applied in the field of preparation of gallokonjac glucomannan, and achieves the effects of wide application prospect, improvement of hydrosol viscosity and stability, and easy process operation.

Inactive Publication Date: 2012-08-08
承德医学院中药研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Currently, there is no report on the modification of konjac glucomannan with gallic acid

Method used

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  • Preparation method of galloyl konjac glucomannan
  • Preparation method of galloyl konjac glucomannan
  • Preparation method of galloyl konjac glucomannan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1: Preparation of galloyl konjac glucomannan

[0045] The implementation steps are as follows:

[0046] (A) Preparation of triacetyl gallic acid

[0047] Add gallic acid (30g, 0.177mol), acetic anhydride (67mL, 0.708mol) and anhydrous pyridine (57mL, 0.708mol) in a molar ratio of 1:4:4 into a 1000mL round-bottomed flask (ice bath), at a temperature of 25 Slowly stir for 12 hours under the condition of ℃, then add 620mL water, that is, 5 times the reaction volume of water to dilute, then add concentrated hydrochloric acid to adjust the pH value of the solution to 1, after that, precipitation occurs, filter with suction, and the obtained solid is washed with a small amount of cold water , dried at a temperature of 55-65° C. to constant weight to obtain 46.46 g of a white powdery solid, identified by the method described in this manual, and the white powdery solid was triacetyl gallic acid. The yield is 87% based on the amount of raw materials used and the amoun...

Embodiment 2

[0055] Embodiment 2: Preparation of galloyl konjac glucomannan

[0056] This example is carried out in the same manner as Example 1, except that in step (A), the molar ratio of gallic acid, acetic anhydride and anhydrous pyridine is adjusted to 1:2:6; step B) the prepared triacetyl gall The mol ratio of acid and thionyl chloride is 1: 2; in step (C), the mass ratio of its konjac glucomannan and triacetyl galloyl chloride is 1: 4; in step (D), step (C) The prepared triacetylgalloyl konjac glucomannan was dissolved in a saturated sodium acetate solution in absolute ethanol at a ratio of 25 mL / g.

[0057] Calculated according to the amount of raw materials used in this embodiment and the amount of the product galloyl konjac glucomannan, the total yield is 56%. The hydrosol viscosity and stability of the galloyl konjac glucomannan prepared in this example were measured by the method described in this specification, and the results were 1.0×10 -3 Pa·s and 5 days.

Embodiment 3

[0058] Example 3: Preparation of galloyl konjac glucomannan

[0059] This example is carried out in the same manner as Example 1, except that in step (A), the molar ratio of gallic acid, acetic anhydride and anhydrous pyridine is adjusted to 1:6:2; the triacetyl prepared in step (B) The mol ratio of gallic acid and sulfur oxychloride is 1: 5; In step (C), the mass ratio of its konjac glucomannan and triacetyl galloyl chloride is 1: 2; In step (D), step (C ) prepared triacetylgalloyl konjac glucomannan was dissolved in saturated sodium acetate in absolute ethanol solution according to the ratio of 60mL / g.

[0060] Calculated according to the amount of raw materials used in this example and the amount of the product galloyl konjac glucomannan, the total yield is 62%. The hydrosol viscosity and stability of the galloyl konjac glucomannan prepared in this example were measured by the method described in this specification, and the results were 0.7×10 -3 Pa·s and 5 days.

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Abstract

The invention relates to a preparation method of galloyl konjac glucomannan. The preparation method comprises the following steps of: preparing triacetyl gallic acid; preparing triacetyl galloyl acryl chloride; preparing triacetyl galloyl konjac glucomannan; preparing the galloyl konjac glucomannan; and the like. According to the preparation method, the gallic acid is utilized to modify konjac glucomannan through esterification; and both the viscosity and the stability of hydrosol of the konjac glucomannan are obviously improved. The preparation method has the advantages of simplicity and convenience in process operation, high production efficiency, low equipment requirement and the like; the total yield can reach over 60 percent; large-scale production can be realized; and the preparation method has high economic and social value and broad application prospect.

Description

【Technical field】 [0001] The invention belongs to the technical field of chemical industry. More specifically, the present invention relates to a preparation method of galloyl konjac glucomannan. 【Background technique】 [0002] Konjac glucomannan (KGM) is a plant polysaccharide with excellent thickening and unique gelling properties. It has important uses in food, chemical industry, textile, medicine, etc., but the stability of KGM hydrosol is poor. limit its wider application. [0003] Gallic acid (3,4,5-trihydroxybenzoic acid) is a polyphenolic substance ubiquitous in nature, which can undergo esterification reaction with hydroxyl groups to generate gallic acid esters, which have the functions of scavenging free radicals, anti-oxidation, and inhibiting polyphenols. Enzyme activity and so on. Gallic acid esters can be used in antioxidants of fat or oil-based foods, biodiesel and certain materials, antioxidant stabilizers and anti-aging agents, anti-tumor and cardiovascul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/02
Inventor 尹志峰李云峰王良友郝婷高杨
Owner 承德医学院中药研究所
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