Preparation process for cornstalk pentosane sulfate

A straw pentosan sulfate ester and preparation process technology, which is applied in the structural transformation and application field of natural products, can solve the problems of low sulfuric acid substitution degree of esterification products and high equipment requirements, and achieve good market application prospects and sulfation degree High, easy-to-operate effect

Inactive Publication Date: 2017-06-13
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
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  • Claims
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Problems solved by technology

Commonly used sulfonation reagents include chlorosulfonic acid, sulfur trioxide, concentrated sulfuric acid, sulfur dioxide and oxygen, sulfuryl chloride and sulfite, etc., but these esterification methods use strong acid, which requires high equipment requirements, strict anhydrous operation, and the resulting esterification The sulfuric acid substitution degree of the product is not very high

Method used

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  • Preparation process for cornstalk pentosane sulfate
  • Preparation process for cornstalk pentosane sulfate
  • Preparation process for cornstalk pentosane sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Extraction of Corn Stalk Pentosans

[0026] Add 4g of corn stalks (screened through a 60-mesh standard sieve) into 120mL of NaOH solution (ω is 10%), and react at 70°C for 6h. Suction filtration, adjust the pH of the filtrate to 7 with HCl (ω is 9%), concentrate in vacuo to 80 mL, cool to room temperature, add 240 mL of absolute ethanol to settle, and settle at 0°C for 9 hours. Suction filtration, the filter cake was washed 3 times with 20 mL of absolute ethanol, and the filter cake was dried in a vacuum oven at 30° C. for 12 hours to obtain crude pentosan.

[0027] 2. Purification of Corn Stalk Pentosans

[0028] (1) Recrystallization: Add the crude pentosan in Example 1 into 50 mL of NaOH solution (ω is 5%), stir and dissolve, filter with suction, add HCl dropwise to the filtrate (ω is 9%) to adjust the pH of the solution to 7. Concentrate in vacuo to 30 mL, add 90 mL of absolute ethanol after cooling, produce a large amount of white crystals, settle for 8 hours,...

Embodiment 2

[0032] 1. Preparation of Pentosan Sulfate

[0033] (1) Add 40mLNaHSO 3 The solution (ω is 32.5%) was added to a 100mL three-necked flask with a thermometer and a condenser, and slowly added dropwise 10mL NaNO 2 solution (ω is 20%), control the rate of addition, 20 minutes to complete the drop. React at 90°C for 1.5h to obtain the esterification reagent sodium aminotrisulfonate solution (ω is 18.7%).

[0034] (2) Adjust the pH of the sodium aminotrisulfonate solution obtained in step (1) to 9 with NaOH (ω is 5%), add 2g of pentosan from Example 1, and react at 50°C for 5h.

[0035] (3) Concentrate the reaction solution obtained in step (2) to 20 mL in vacuo, add 60 mL of absolute ethanol, settle for 1 hour, filter with suction, and rinse the filter cake with 20 mL of absolute ethanol three times.

[0036] (4) Add 20mL of distilled water to the filter cake obtained in step (3), stir to dissolve, then add 5mL of HCl (ω is 18%) dropwise for acidification, add dropwise slowly, a...

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Abstract

The invention relates to a preparation process for cornstalk pentosane sulfate and belongs to the technical field of natural product structural transformation and application. According to the preparation process for the cornstalk pentosane sulfate, the target product pentosane sulfate is synthesized via a two-step reaction; the molecular structure of the pentosane sulfate is similar to that of heparin and the pentosane sulfate can be used as a raw material for synthesizing an anticoagulant active drug. The preparation process for the cornstalk pentosane sulfate, provided by the invention, has the advantages of simple and convenient operation, small pollution, high sulfation degree, wide raw material source, good market application prospect and so on.

Description

technical field [0001] The invention relates to a preparation process of corn stalk pentosan sulfate, which belongs to the technical field of structural modification and application of natural products. Background technique [0002] Polysaccharides are natural macromolecular substances that widely exist in plants, marine organisms, and microorganisms. They are chain polymers of aldose or ketose formed by dehydration between monosaccharides to form glycosidic bonds, which are connected linearly or branched by glycosidic bonds. , also known as polysaccharides. Due to the different composition of monosaccharide residues, different types of glycosidic bonds, and differences in the position and number of branch points, the molecular structure of polysaccharides is very complicated. In recent years, great progress has been made in the research on the biological activity of polysaccharides and their derivatives from plants, marine organisms and microorganisms. It has significant ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/00
Inventor 米浩宇王佩张龙
Owner CHANGCHUN UNIV OF TECH
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