Process for preparing Curdlan sulfate (2024)

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A technology of codran sulfate and chlorosulfonic acid, which is applied in the field of polymer compound preparation, can solve the problems of slow reaction, low activity of sulfonating agent, low sulfur content, etc., achieve high efficiency, shorten reaction time, shorten The effect of the process

Inactive Publication Date: 2004-04-28

TIANAN BIOLOGIC MATERIAL NINGBO

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Problems solved by technology

The sulfonating agent used in this method has low activity, resultin

Method used

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Experimental program

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Effect test

Embodiment 1

[0019] Add 5.0 kg of dried Cortran into 900 liters (ρ=1.1 g / ml) of dimethyl sulfoxide solution, stir to dissolve. Measure 5.5 liters of pyridine (ρ=0.983g / ml), add it into the dimethyl sulfoxide solution containing Cortran, and stir evenly.

[0020] After the above solution was stirred and cooled, 3.2 liters of chlorosulfonic acid (ρ=1.75 g / ml) was added under stirring. The reaction continued for 5 hours to obtain a cotran sulfate solution. Then pour the Cordland sulfate solution into the ethanol solution containing 3% sodium hydroxide under stirring state, so that the initial reaction product of Cortran sulfate is precipitated. After the precipitate was filtered, the filter cake was washed twice with ethanol. Dissolve the washed filter cake in deionized water. The aqueous solution is desalinated by ultrafiltration membrane. The solution obtained after desalination was poured into ethanol containing 3% sodium hydroxide and stirred for precipitation. Then filter, the filte...

Embodiment 2

[0023] Add 3.0 kg of dried Cortran into 300 liters (ρ=1.1 g / ml) of dimethyl sulfoxide solution, stir to dissolve. Measure 10.0 liters of pyridine (ρ=0.983g / ml), add it into the dimethyl sulfoxide solution containing Cortran, and stir evenly.

[0024] After the above solution was stirred and cooled, 4.0 liters of chlorosulfonic acid (ρ=1.75 g / ml) was added under stirring. The reaction continued for 2 hours to obtain a cotran sulfate solution. Then pour the Cordland sulfate solution into the ethanol solution containing 5% sodium acetate under stirring state, so that the initial reaction product of Cortran sulfate is precipitated. After the precipitate was filtered, the filter cake was washed twice with ethanol. Dissolve the washed filter cake in deionized water. The aqueous solution is desalinated by ultrafiltration membrane. The solution obtained after desalination was poured into ethanol containing 5% sodium acetate and stirred for precipitation. Then filter, the filter c...

Embodiment 3

[0027] Take 10.0 kg of dried Cortran and add it into 200 liters (ρ=1.1 g / ml) dimethyl sulfoxide solution, stir to dissolve. Measure 150 liters of pyridine (ρ=0.983g / ml), add it into the dimethyl sulfoxide solution containing Cortran, and stir evenly.

[0028] After the above solution was stirred and cooled, 55 liters of chlorosulfonic acid (ρ=1.75 g / ml) was added under stirring. The reaction was continued for 3 hours to obtain a cotran sulfate solution. Then pour the Cordland sulfate solution into the ethanol solution containing 10% sodium acetate under stirring state, so that the initial reaction product of Cortran sulfate is precipitated. After the precipitate was filtered, the filter cake was washed twice with ethanol. Dissolve the washed filter cake in deionized water. The aqueous solution is desalinated by ultrafiltration membrane. The solution obtained after desalination was poured into ethanol containing 10% sodium acetate and stirred for precipitation. Then filter...

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Abstract

The preparation process of Curdlan sulfate includes dissolving Curdlan in dimethyl sulfoxide solution via stirring, adding pyridine and chlorosulfonic acid while stirring to form Curdlan sulfate solution, pouring the Curdlan sulfate solution into alkali ethanol solution to deposit Curdlan sulfate, filtering, washing and desalting the Curdlan sulfate precipitate, further deposition, filtering, washing, and drying to obtain the Curdlan sulfate product. The present invention has simple technological process, high efficiency and high sulfur content in the product.

Description

technical field [0001] The invention relates to a preparation method of a polymer compound. Background technique [0002] Cortlan is a poorly water-soluble β-(1-3) glucan. It does not have anti-HIV activity itself, but the anti-HIV activity of its sulfate has been reported (see US Patent 5.512.672). In addition to its obvious anti-HIV activity, codran sulfate has very low toxicity and anticoagulant activity, so codran sulfate is expected to be used for HIV treatment. In addition, according to literature reports, the sulfur content of codran sulfate is directly proportional to the anti-HIV activity (see Br.Polym.J.1990.23(3).245-50). At present, Ketlan is used as a raw material to prepare its sulfate using a two-step reaction (see U.S. Patent U.S. 5,512,672). The specific steps are as follows: first react hexahydropyridine with sulfuric acid to obtain the sulfonating agent hexahydropyridine sulfate; then react hexahydropyridine sulfate with cotran dimethy...

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IPC IPC(8): C08B37/02

Inventor 章亦华

Owner TIANAN BIOLOGIC MATERIAL NINGBO