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Preparation method and application of oligomeric sodium alginate sulfate salt

A technology of alginate sulfate and alginate, which is applied in the field of preparation of alginate, can solve the problems of complicated process steps and high manufacturing cost, achieve the effects of optimizing the degradation process, reducing production cost, and improving hyperlipidemia

Inactive Publication Date: 2016-08-03
天津中津药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, Guan Huashi of Ocean University of China introduced sulfonyl and propylene glycol groups on the hydroxyl and carboxyl groups of alginic acid molecules to prepare sodium alginate diester for the treatment of hyperlipidemia; the application number is also disclosed in the invention patent of 200910017257.7 A method for preparing sodium alginate diester is disclosed, which discloses another method for preparing sodium alginate diester, using alginic acid as a raw material, and completing the process steps of emulsification, acidification, esterification, sulfonation and salt formation, However, the process steps in this application are complicated and the manufacturing cost is high

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  • Preparation method and application of oligomeric sodium alginate sulfate salt
  • Preparation method and application of oligomeric sodium alginate sulfate salt
  • Preparation method and application of oligomeric sodium alginate sulfate salt

Examples

Experimental program
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Effect test

Embodiment 1

[0071] Embodiment 1 prepares oligomeric alginic acid

[0072] Preparation method one:

[0073] Add 1000g of alginic acid to 10L of deionized water, keep the temperature at 0.2MPa and 120°C for 3 hours, then cool down to 40°C, and obtain alginic acid with a weight average molecular weight below 40,000 Daltons;

[0074] Dissolve the prepared alginic acid in a polyethylene glycol solution, add a compound emulsifier to grind to the oil phase, add water and stir until the raw material emulsion is formed;

[0075] Add 0.7 mol / L hydrochloric acid to the raw material emulsion in an amount of 12 L at 110°C, react for 4 hours, filter and wash the precipitate with ethanol 5 times, and vacuum-dry at 50°C to obtain the dry material oligomeric alginic acid.

[0076] Preparation method two:

[0077] Add 1000g of alginic acid to 9L of deionized water, keep the temperature at 0.2MPa and 125°C for 3 hours, then cool down to 40°C to obtain alginic acid with a weight average molecular weight be...

Embodiment 2

[0083] Take 100g of the oligomeric alginic acid prepared by the present invention, add 5000ml of distilled water to swell for 24 hours, then add 5000ml of 2N oxalic acid, reflux in a boiling water bath for 10 hours, then filter to remove the acid solution, rinse the filtered product with 3000ml of distilled water, and use a ratio of 100g of filtrate to 1g Add solid Na 2 CO 3 . At this time, it is in the state of sol, adjust the pH to 3.0 with hydrochloric acid, then centrifuge (3000 rpm) to separate, take the supernatant, use 100g of 717 and 732 anion and cation exchange resins for desalination, remove the resin, add 3 times the solution A certain amount of ethanol is used for precipitation, and the resulting precipitate is dried at 60°C to obtain oligomeric alginic acid. A total of 163 g of oligomeric alginic acid was obtained. Take 100g of the above-mentioned dried oligomeric alginic acid, put it in a 3000ml three-necked bottle, install the stirring device and thermometer...

Embodiment 3

[0086] Preparation method of sodium alginate sodium sulfate with low sulfur content

[0087] The main raw materials and proportions used in this example: 1000 g of dry oligomeric alginic acid in Preparation Example 2, 30 L of formamide, and 2 L of chlorosulfonic acid. First put oligomeric alginic acid into a 100L sulfonation reactor, then add formamide and stir evenly, then add ice-water mixture outside the reactor to cool down. Add chlorosulfonic acid dropwise while stirring, keep the temperature below 5°C to complete the dropwise addition of chlorosulfonic acid, then raise the temperature of the reaction mixture to about 65°C and react for 2 hours, add ethanol to make the final concentration of ethanol in the reaction mixture exceed 75%, so that Oligomeric sodium alginate sodium sulfate is precipitated, and the precipitate is washed three times with 95% ethanol (50L each time), and 10% sodium hydroxide is added to adjust the pH to 8, and the crude product solution of oligome...

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Abstract

The invention relates to a preparation method and application of an oligomeric alginate sulfate ester salt, belonging to the field of raw material preparation of chemicals. The preparation method of the oligomeric alginate sulfate provided by the invention is to add pyridine and chlorosulfonic acid after degradation, emulsification and washing to prepare oligomeric alginate sulfate, and use potassium ions, sodium ions or ammonia water to form a salt, Potassium oligomeric alginate sulfate, sodium oligomeric sodium alginate sulfate or ammonium oligomeric ammonium alginate sulfate are generated. The preparation method provided by the invention overcomes the problems of complex process in the prior art through direct sulfonation, and optimizes the degradation process of alginic acid.

Description

【Technical field】 [0001] The invention relates to a preparation method of alginate, in particular to a preparation method and application of oligomeric alginate sulfate. 【Background technique】 [0002] Alginic acid (C 6 h 8 o 6 )n, also known as alginic acid, alginic acid, seaweed, is a natural polysaccharide present in the cell wall of brown algae, composed of monofurose aldehyde β-D-mannuronic acid (M) and α-L-guluronic aldehyde Acid (G) is a linear polymeric polysaccharide linked by 1,4 glycosidic bonds in a combination of M-M, G-G or M-G, with a molecular weight ranging from 10,000 to 600,000 Daltons. The pure product is usually in the form of white to tan fibers, granules or powder. It is usually prepared by reacting the extract from seaweed and sodium hydroxide with strong acids such as sulfuric acid, or by using nitrogen-fixing bacteria and pseudomonas to biosynthesize alginic acid. [0003] Because alginic acid has the effect of quickly absorbing water, it is of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/04C13K13/00A61K31/737A61K31/7024A61P9/12A61P13/12A61P3/10A61P3/06
CPCC08B37/0084A61K31/7024A61K31/737C13K13/00
Inventor 宋富智梁世昌宋德顺
Owner 天津中津药业股份有限公司
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