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Preparation method of modified laminarin by synergistic effect

A technology of laminar polysaccharide and synergistic effect, which is applied in the field of preparation of synergistically modified laminar polysaccharide, can solve the problems of long reaction time and high reaction temperature, and achieve the effect of simple and easy operation, low reaction temperature and pollution reduction

Inactive Publication Date: 2018-09-14
LUDONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional phosphorylation modification reaction of natural polysaccharides is carried out in alkaline solution, the reaction temperature is high, and the reaction time is long

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A method for preparing synergistically modified laminarin, the steps are as follows:

[0041] (1) Mix laminarin, 3-amino-1-hydroxypropylidene diphosphonic acid disodium salt, urea and calcium chloride at 18-22°C; among them, laminarin, 3-amino-1- The mass ratio of hydroxypropylene diphosphonic acid disodium salt, urea and calcium chloride is 1.0:0.9:0.11:12;

[0042] (2) Heating the mixture in step (1) to 60°C and reacting for 5 hours to obtain a reaction mixture;

[0043] (3) Add distilled water to the reaction mixture in step (2), and heat to 50°C to dissolve; wherein, the mass ratio of the reaction mixture to distilled water is 1:160;

[0044](4) The solution obtained in step (3) was concentrated, ethanol precipitated, and dried to obtain the product 3-amino-1-hydroxypropylidene diphosphonic acid laminarin calcium. The phosphate content in the product was 11.27%, and the calcium content was 19.35 %.

Embodiment 2

[0046] A method for preparing synergistically modified laminarin, the steps are as follows:

[0047] (1) Mix laminarin, 3-amino-1-hydroxypropylidene diphosphonic acid disodium salt, urea and calcium chloride at 23-26°C; among them, laminarin, 3-amino-1- The mass ratio of hydroxypropylene diphosphonic acid disodium salt, urea and calcium chloride is 1.0:0.8:0.1:10;

[0048] (2) Heating the mixture in step (1) to 70°C and reacting for 5 hours to obtain a reaction mixture;

[0049] (3) Add distilled water to the reaction mixture in step (2), and heat to 60°C to redissolve; wherein, the mass ratio of the reaction mixture to distilled water is 1:160;

[0050] (4) The solution obtained in step (3) was concentrated, ethanol precipitated, and dried to obtain the product 3-amino-1-hydroxypropylidene diphosphonic acid laminarin calcium. The phosphate content in the product was 10.24%, and the calcium content was 17.31 %.

Embodiment 3

[0052] A method for preparing synergistically modified laminarin, the steps are as follows:

[0053] (1) Mix laminarin, 3-amino-1-hydroxypropylidene diphosphonic acid disodium salt, urea and calcium chloride at 18-21°C; among them, laminarin, 3-amino-1- The mass ratio of hydroxypropylene diphosphonic acid disodium salt, urea and calcium chloride is 1.0: 0.7: 0.12: 12;

[0054] (2) Heating the mixture in step (1) to 55°C and reacting for 7 hours to obtain a reaction mixture;

[0055] (3) Add distilled water to the reaction mixture in step (2), and heat to 50°C to redissolve; wherein, the weight ratio of the reaction mixture to distilled water is 1:170;

[0056] (4) The solution obtained in step (3) was concentrated, ethanol precipitated, and dried to obtain the product 3-amino-1-hydroxypropylidene diphosphonic acid laminarin calcium. The phosphate content in the product was 10.07%, and the calcium content was 18.25 %.

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Abstract

The invention belongs to the technical field of polysaccharide derivatives, and particularly relates to a preparation method of modified laminarin by a synergistic effect. A low-thermosetting phase one-step synthesis method with advantages of low reaction temperature, low energy consumption and simple operation steps is adopted and organic solvents are not used or less used, the environmental pollution can be reduced, so that the requirements of green chemistry are met, and the method has the potential of development and utilization. 3-amino-1-hydroxypropylenedi modification is carried out onlaminarin, phosphonyl group, amidogen and hydroxyl can be introduced, a hydrophilic surface structure can be constructed for the laminarin, so that the water solubility activity of the laminarin can be effectively improved. Compared with the prior art, the phosphate radical content and calcium content of the prepared 3-amino-1-hydroxypropylenedi laminarin product are both greatly improved, the laminarin is green and environmentally friendly, the operation process is simple and operated easily, and the industrialization and technical promotion are convenient.

Description

technical field [0001] The invention belongs to the technical field of polysaccharide derivatives, in particular to a method for preparing synergistically modified laminarin polysaccharides. Background technique [0002] Natural polysaccharides are natural high polymers composed of aldose and / or ketose linked by glycosidic bonds, which are abundant and various in nature. It is also an important part of biological organisms. It has good biomass characteristics and plays a very important role in the normal physiological functions of organisms. It has many advantages such as wide sources, low cost, good biological activity, and natural and easy degradation. [0003] Yantai, located on the Jiaodong Peninsula, is rich in seafood resources and is an important kelp breeding production base in China. Kelp is rich in polysaccharides, which have a variety of biological functions and a wide range of biological activities. After molecular modification of polysaccharides, a variety of ...

Claims

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Application Information

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IPC IPC(8): C08B37/00
CPCC08B37/00
Inventor 殷平魏立军杨正龙刘希光徐彦宾姜玮任淑华
Owner LUDONG UNIVERSITY
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