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Method for preparing polysaccharide sulfate by virtue of electrochemical reaction

A technology of sodium alginate diester and electrochemical reaction is applied in the field of preparing sodium alginate diester by electrochemical reaction, which can solve the problems of screening, complicated process, low purity of intermediates and the like

Inactive Publication Date: 2015-07-15
CP PHARMA QINGDAO CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to completely solve the problem that the traditional method cannot be screened according to the molecular weight, obtain a product with a reasonable molecular weight and an objective yield, and solve the problem that the traditional method is cumbersome and the obtained intermediate has low purity

Method used

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  • Method for preparing polysaccharide sulfate by virtue of electrochemical reaction
  • Method for preparing polysaccharide sulfate by virtue of electrochemical reaction
  • Method for preparing polysaccharide sulfate by virtue of electrochemical reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] The main body of this embodiment is the method for quickly and effectively removing sulfate in the PSS bulk drug:

[0010] (1) Experimental procedure: take PSS raw material medicine (tablet raw material medicine, batch number: 0801121, SO 4 2- =12.34%) 100g, dissolved in 2L water (solution concentration 5%), poured the solution into the ultrafiltration and nanofiltration roll-type membrane system, and carried out experiments with 200-300 Da nanofiltration membrane and 1000 Da ultrafiltration membrane respectively. Add 4L of water each time, add water repeatedly to concentrate until the conductivity becomes about 10, concentrate the filtrate to 2L, pour it out, wash the sample on the filter membrane with water, and combine it with the concentrated solution, spray the filtrate to dry, weigh The mass of the sample obtained was used to calculate the yield, and the sulfate content and molecular weight were determined.

[0011] (2) Experimental results and discussion:

[0...

Embodiment 2

[0018] The main body of this embodiment is the selection of ultrafiltration conductance in the preparation of PSS bulk drug:

[0019] (1) Experimental steps: Take PSS API (batch number: 0801121, SO 4 2- =12.34%) 100g, dissolved in 2L water (solution concentration 5%), poured the solution into a nanofiltration instrument, and used a 1000 Da ultrafiltration membrane for ultrafiltration desalination, adding 4L water each time, repeatedly adding water to concentrate until the conductivity Change to about 500, start sampling in the range of 500-10 conductance, 100mL each time (every sampling is guaranteed to be concentrated to about 2L), evaporate each sample to dryness, and use ion chromatography (IC) Determine the most suitable ultrafiltration conductance value by measuring its sulfate content with barium chloride colorimetry.

[0020] (2) Experimental results and discussion

[0021] Ultrafiltration conductivity test results

[0022]

[0023] As can be seen from the result...

Embodiment 3

[0025] The present invention will be further described in conjunction with the main process steps of sodium alginate diester, including five processes of raw material emulsification treatment, acidification chain breaking treatment, esterification treatment, sulfonation treatment and salt formation.

[0026] (1) Raw material emulsification treatment: Take 120 g of alginic acid, moisten it with a small amount of water, dissolve it in polyethylene glycol solution, slowly add 2% of Tween 20, Tween 80 (2:4) compound emulsifier, Put it in a colloid mill and grind for 15 minutes, grind it repeatedly three times to make a uniform oil phase, and transfer it to a reaction tank, gradually add purified water, and stir while adding, until an emulsion is finally formed, usually stirring for 30 minutes to obtain the raw material emulsion ;

[0027] (2) Acidification chain breaking treatment: put the raw material emulsion into the reaction kettle, add 1000 ml of 0.6 mol / L hydrochloric acid w...

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Abstract

The invention relates to a method for preparing polysaccharide sulfate by virtue of electrochemical reaction. The method is introduced into the production of polysaccharide sulfate by virtue of electrochemical reaction and is used for solving the problems that during the production of polysaccharide sulfate, chains are difficult to break, different in length after chain breakage and are poor in selection. After the introduction of electrochemistry, after the positive and negative poles of an electrode are matched with the charge quality of each electrode and screened molecular broken chains, a needed product can be distinguished very easily, so that the production efficiency of polysaccharide sulfate is greatly improved, then the difficult problem that the conventional method cannot perform screening according to the molecular weight is completely solved, a product with a reasonable molecular weight and an objective yield is obtained, and the problems that the conventional method is complicated in process and an obtained intermediate is low in purity are solved. According to the method provided by the invention, the introduced electromechanical technology ensures that a target substance is enriched and convenient to collect; the method is high in selectivity; the obtained intermediate is high in content; and the stability of the product is greatly improved.

Description

technical field [0001] The invention relates to a method for preparing sodium alginate diester by electrochemical reaction, which uses alginic acid as a raw material and is completed through the process steps of emulsification, acidification, esterification, sulfonation and salt formation, and belongs to the technical field of chemical raw material preparation. Background technique [0002] Sodium alginate diester is the first drug derived from marine resources in my country. It is the first product independently developed by our company. It is a natural component extracted from marine plants kelp and kelp. It has the advantages of rich resources, low price, safety and high efficiency. Our company is the setter of quality standards and an enterprise with approval documents for raw materials and preparations. Won 24 awards including the new invention gold medal in the 15th International Exposition. Xinhua News Agency reported that "the successful research of sodium alginate d...

Claims

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Application Information

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IPC IPC(8): C08B37/04
Inventor 王明刚陈阳生任莉刘晓霞孙桂玉韩佳佳汪泓
Owner CP PHARMA QINGDAO CO LTD
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