Preparation method for xylan polysulfate

A technology of xylan and sulfate, applied in the field of preparation of xylan polysulfate, can solve the problems of no practical value, low sulfonation rate, environmental pollution, etc., achieve excellent sulfonation ability, low toxicity, avoid The effect of severe environmental pollution burden

Inactive Publication Date: 2018-11-30
GUANGXI INST OF BOTANY THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second, using water as a solvent, utilizes sodium aminotrisulfonate as a sulfonating agent to prepare (such as Chinese patent CN102875698B), although this method solves the environmental pollution problem of the first method, but because it is a process in water In addition to the sulfonation reaction, there is also a serious hydrolysis desulfonation reaction at the same time, so the sulfonation rate is extremely low, resulting in products that do not have practical value

Method used

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  • Preparation method for xylan polysulfate
  • Preparation method for xylan polysulfate
  • Preparation method for xylan polysulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation method of the xylan polysulfate of the present embodiment, comprises the steps:

[0037] Step 1: Prepare the First Mixture

[0038] Weigh 60g xylan and 254g sulfur trioxide pyridine complex respectively, place them in a reaction kettle to obtain the first mixture;

[0039] Step 2: Prepare the Second Mixture

[0040] Add 750 mL of dimethyl sulfoxide to the first mixture obtained in step 1, react at 55° C. for 3 hours while stirring, and then lower it to room temperature of 20° C. to obtain the second mixture;

[0041] Step 3: Preparation of Crude Xylan Polysulfate

[0042] Dissolve 72g of NaOH in 100mL of water to obtain NaOH lye; add the above-mentioned lye to the second mixture obtained in step 2, stir well, then add 2L of methanol, filter the precipitate and dry to obtain 149g of xylan polysulfuric acid Crude salt;

[0043] Step 4: Preparation of xylan polysulfate finished product

[0044] Take 50 g of the crude xylan polysulfate obtained in step ...

Embodiment 2

[0049] The preparation method of the xylan polysulfate of the present embodiment, comprises the steps:

[0050] Step 1: Prepare the First Mixture

[0051] Weigh 100g of xylan and 411g of sulfur trioxide triethylamine complex respectively, and place them in a reaction kettle to obtain the first mixture;

[0052] Step 2: Prepare the Second Mixture

[0053] Add 2.5L of N,N-dimethylformamide to the first mixture obtained in step 1, react at 95°C for 1 hour while stirring, and then lower it to room temperature of 22°C to obtain the second mixture;

[0054] Step 3: Preparation of Crude Xylan Polysulfate

[0055] Dissolve 127g of KOH in 200mL of water to obtain KOH lye; add the above-mentioned KOH lye to the second mixture obtained in step 2, stir thoroughly, then add 5L of ethanol, filter the precipitate and dry to obtain 284g of xylan polysaccharide crude sulfate;

[0056] Step 4: Preparation of xylan polysulfate finished product

[0057] Take 100g of the crude xylan polysulfate...

Embodiment 3

[0061] The preparation method of the xylan polysulfate of the present embodiment, comprises the steps:

[0062] Step 1: Prepare the First Mixture

[0063] Weigh 45g xylan and 142g sulfur trioxide trimethylamine compound respectively, place in the reaction kettle, obtain the first mixture;

[0064] Step 2: Prepare the Second Mixture

[0065] Add 750 mL of N,N-dimethylacetamide to the first mixture obtained in step 1, react at 75°C for 2 hours while stirring, and then lower it to room temperature of 23°C to obtain the second mixture;

[0066] Step 3: Preparation of Crude Xylan Polysulfate

[0067] 38g Ca(OH) 2 Dissolve in 250mL water to make a suspension to obtain Ca(OH) 2 lye; to the second mixture obtained in step 2, add the above Ca(OH) 2 After fully stirring the lye, add 2L of a mixture of methanol and ethanol in any proportion, filter the precipitate and dry it to obtain 127g of xylan polysulfate crude product;

[0068] Step 4: Preparation of xylan polysulfate finishe...

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Abstract

The invention discloses a preparation method for xylan polysulfate, and belongs to the technical field of xylan polysulfate. The preparation method for the xylan polysulfate comprises the following steps of 1, preparing a first mixture; 2, preparing a second mixture; 3, preparing a xylan polysulfate crude product; and 4, preparing a xylan polysulfate finished product. The preparation method has the advantages that the xylan polysulfate is prepared by taking a sulfur trioxide compound as a sulfonating agent in a polar organic solvent, so that 1, the high sulfonating efficiency can be ensured through the organic solvent, 2, the serious environmental pollution burden caused by pyridine as a solvent in the prior art can be avoided, and 3, the sulfur trioxide compound is stable in property andgood in safety and can be conveniently applied in production.

Description

technical field [0001] The invention relates to a preparation method of xylan polysulfate, belonging to the technical field of xylan polysulfate. Background technique [0002] Heparin Sodium is a mucopolysaccharide sulfate anticoagulant. Heparin sodium is the sodium salt of aminodextran sulfate extracted from the intestinal mucosa of animals such as pigs or cattle, and belongs to mucopolysaccharides. However, because of its low content in raw materials, it is difficult to extract and complicated to purify, resulting in high price, and heparin sodium comes from animals, which may introduce other pathogens. Therefore, the synthesis of heparan-like sodium structure compounds by sulfonating natural polysaccharides has become an important solution. [0003] In the prior art, the preparation method of xylan polysulfate mainly contains two kinds: the first kind, add sulfonating agent chlorosulfonic acid in the system that pyridine is solvent and prepare (such as Chinese patent CN...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/14
CPCC08B37/0057
Inventor 王磊覃香香陈海珊
Owner GUANGXI INST OF BOTANY THE CHINESE ACAD OF SCI
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