Preparation method of xylan polysulfate sodium

Abstract

The invention discloses a preparation method of xylan polysulfate sodium, and belongs to the technical field of xylan polysulfate sodium. The preparation method of xylan polysulfate sodium includes the following steps that 1, a first mixture is prepared; 2, a second mixture is prepared; 3, a crude xylan polysulfate product is prepared; 4, a finished xylan polysulfate sodium product is prepared. According to the preparation method of xylan polysulfate sodium, chlorosulfonic acid serves as a sulfonating agent, xylan polysulfate sodium is prepared in polar organic solvent, pyridine serving as solvent in the prior art is reduced in dosage or completely eradicated, and therefore serious environment pollution caused by pyridine serving as the solvent is avoided or reduced.

Description

technical field

[0001] The invention relates to a preparation method of sodium xylan polysulfate, belonging to the technical field of sodium xylan polysulfate. Background technique

[0002] Sodium xylan polysulfate (alias sodium pentosan polysulfate) is a drug used to treat interstitial cystitis. In the prior art, the synthesis method of sodium xylan polysulfate uses pyridine as a solvent and chlorosulfonic acid as a sulfonating agent (for example, Chinese patent CN101942041B and US patent US2010 / 0105889A1). This method uses pyridine as a solvent, and there is a serious stench in the production process. Not only is the production environment bad, but a large amount of pyridine makes wastewater treatment and solvent recovery difficult, causing serious environmental pollution problems.

[0003] In view of this, it is necessary to develop a new preparation method of sodium xylan polysulfate to solve the deficiencies in the prior art. Contents of the invention

[0004] The p...

Examples

Embodiment 1

[0027] The preparation method of the sodium xylan polysulfate of the present embodiment may further comprise the steps:

[0028] Step 1: Prepare the First Mixture

[0029] Add 500mL dimethyl sulfoxide to a 1L flask, carefully add 50mL chlorosulfonic acid under stirring conditions, and obtain the first mixture after the exothermic end;

[0030] Step 2: Prepare the Second Mixture

[0031] Add 30 g of xylan solids to the first mixture obtained in step 1, and react at 55° C. for 3 hours while stirring, and then lower to room temperature of 20° C. to obtain the second mixture;

[0032] Step 3: Preparation of Crude Xylan Polysulfate

[0033] Dissolve 45.6g of NaOH in 100mL of water to obtain NaOH solution; add the above-mentioned NaOH solution to the second mixture obtained in step 2, and stir thoroughly to obtain the third mixture, then add 2L of ethanol to the above-mentioned third mixture, filter the precipitate and remove Dried to obtain 78g sodium xylan polysulfate crude pro...

Embodiment 2

[0040] The preparation method of the sodium xylan polysulfate of the present embodiment may further comprise the steps:

[0041] Step 1: Prepare the First Mixture

[0042] Add 900mL of N,N-dimethylformamide and 65mL of pyridine into a 2L flask, carefully add 53mL of chlorosulfonic acid under stirring conditions, and obtain the first mixture after the exothermic end;

[0043] Step 2: Prepare the Second Mixture

[0044] Add 60 g of xylan solids to the first mixture obtained in step 1, and react at 95° C. for 1 hour while stirring, and then lower to room temperature of 25° C. to obtain the second mixture;

[0045] Step 3: Preparation of Crude Xylan Polysulfate

[0046] Dissolve 72g of NaOH in 100mL of water to obtain a NaOH solution; add the above solution to the second mixture obtained in step 2, stir well, then add 2L of methanol, filter and dry the precipitate to obtain 153g of crude xylan polysulfate ;

[0047] Step 4: Prepare the finished product of sodium xylan polysulf...

Embodiment 3

[0053] The preparation method of the sodium xylan polysulfate of the present embodiment may further comprise the steps:

[0054] Step 1: Prepare the First Mixture

[0055] Add 300mL of N,N-dimethylacetamide to a 500mL flask, carefully add 20mL of chlorosulfonic acid under stirring conditions, and obtain the first mixture after the exothermic end;

[0056] Step 2: Prepare the Second Mixture

[0057] Add 15 g of solid xylan to the first mixture obtained in step 1, and react at 55° C. for 3 hours while stirring, and then lower it to room temperature of 20° C. to obtain the second mixture;

[0058] Step 3: Preparation of Crude Xylan Polysulfate

[0059] Dissolve 18.24g of NaOH in 80mL of water to obtain NaOH solution; add the above-mentioned NaOH solution to the second mixture obtained in step 2, and stir thoroughly to obtain the third mixture, then add the above-mentioned third mixture 1L of ethanol and methanol mixture, and the precipitate Thing is filtered and dried, obtains 4...

technical field

[0001] The invention relates to a preparation method of sodium xylan polysulfate, belonging to the technical field of sodium xylan polysulfate. Background technique

[0002] Sodium xylan polysulfate (alias sodium pentosan polysulfate) is a drug used to treat interstitial cystitis. In the prior art, the synthesis method of sodium xylan polysulfate uses pyridine as a solvent and chlorosulfonic acid as a sulfonating agent (for example, Chinese patent CN101942041B and US patent US2010 / 0105889A1). This method uses pyridine as a solvent, and there is a serious stench in the production process. Not only is the production environment bad, but a large amount of pyridine makes wastewater treatment and solvent recovery difficult, causing serious environmental pollution problems.

[0003] In view of this, it is necessary to develop a new preparation method of sodium xylan polysulfate to solve the deficiencies in the prior art. Contents of the invention

[0004] The p...

Examples

Embodiment 1

[0027] The preparation method of the sodium xylan polysulfate of the present embodiment may further comprise the steps:

[0028] Step 1: Prepare the First Mixture

[0029] Add 500mL dimethyl sulfoxide to a 1L flask, carefully add 50mL chlorosulfonic acid under stirring conditions, and obtain the first mixture after the exothermic end;

[0030] Step 2: Prepare the Second Mixture

[0031] Add 30 g of xylan solids to the first mixture obtained in step 1, and react at 55° C. for 3 hours while stirring, and then lower to room temperature of 20° C. to obtain the second mixture;

[0032] Step 3: Preparation of Crude Xylan Polysulfate

[0033] Dissolve 45.6g of NaOH in 100mL of water to obtain NaOH solution; add the above-mentioned NaOH solution to the second mixture obtained in step 2, and stir thoroughly to obtain the third mixture, then add 2L of ethanol to the above-mentioned third mixture, filter the precipitate and remove Dried to obtain 78g sodium xylan polysulfate crude pro...

Embodiment 2

[0040] The preparation method of the sodium xylan polysulfate of the present embodiment may further comprise the steps:

[0041] Step 1: Prepare the First Mixture

[0042] Add 900mL of N,N-dimethylformamide and 65mL of pyridine into a 2L flask, carefully add 53mL of chlorosulfonic acid under stirring conditions, and obtain the first mixture after the exothermic end;

[0043] Step 2: Prepare the Second Mixture

[0044] Add 60 g of xylan solids to the first mixture obtained in step 1, and react at 95° C. for 1 hour while stirring, and then lower to room temperature of 25° C. to obtain the second mixture;

[0045] Step 3: Preparation of Crude Xylan Polysulfate

[0046] Dissolve 72g of NaOH in 100mL of water to obtain a NaOH solution; add the above solution to the second mixture obtained in step 2, stir well, then add 2L of methanol, filter and dry the precipitate to obtain 153g of crude xylan polysulfate ;

[0047] Step 4: Prepare the finished product of sodium xylan polysulf...

Embodiment 3

[0053] The preparation method of the sodium xylan polysulfate of the present embodiment may further comprise the steps:

[0054] Step 1: Prepare the First Mixture

[0055] Add 300mL of N,N-dimethylacetamide to a 500mL flask, carefully add 20mL of chlorosulfonic acid under stirring conditions, and obtain the first mixture after the exothermic end;

[0056] Step 2: Prepare the Second Mixture

[0057] Add 15 g of solid xylan to the first mixture obtained in step 1, and react at 55° C. for 3 hours while stirring, and then lower it to room temperature of 20° C. to obtain the second mixture;

[0058] Step 3: Preparation of Crude Xylan Polysulfate

[0059] Dissolve 18.24g of NaOH in 80mL of water to obtain NaOH solution; add the above-mentioned NaOH solution to the second mixture obtained in step 2, and stir thoroughly to obtain the third mixture, then add the above-mentioned third mixture 1L of ethanol and methanol mixture, and the precipitate Thing is filtered and dried, obtains 4...

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