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Method for preparing sevelamer carbonate

The technology of sevelamer carbonate and sevelamer hydrochloride is applied in the field of biomedicine, and can solve the problems of high impurity content of sevelamer carbonate, affecting the quality of sevelamer carbonate, affecting the quality of final products, etc. Reaction time and solvent, strong anti-pollution ability and good stability

Inactive Publication Date: 2012-11-28
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yet the impurity content in the carbonic acid sevelamer that this method prepares is high, has influenced the quality of carbonic acid sevelamer
[0004] In addition, epichlorohydrin is used as a crosslinking agent in the existing preparation process of sevelamer carbonate. Under alkaline conditions, the hydrolysis products of epichlorohydrin are relatively complicated, which are related to temperature and alkali concentration, and can generate 3 - Components such as chloroglycerin, glycidol, polyglycerol and glycerin form a variety of impurities that affect the quality of the final product

Method used

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  • Method for preparing sevelamer carbonate

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preparation example 1

[0058] Preparation of polyallylamine hydrochloride

[0059] Add 800g of water, 500g of allylamine hydrochloride monomer, and 4.26g of benzoyl peroxide initiator in a 3000 ml four-neck flask equipped with a stirrer, a thermometer, and a reflux condenser. Adjust the rotation speed under stirring, then raise the temperature to 45°C, keep it warm for 10 hours, then raise the temperature to 85°C and keep it warm for 8 hours, cool down and discharge, wash with water, wash with methanol Soxhlet extraction, and dry to obtain 500g of white granules as the target product.

preparation example 2

[0061] 1,3-dichloroglycerin preparation method (1)

[0062] Add 2 kg of epichlorohydrin into the reaction kettle, lower the temperature to -10°C, add hydrochloric acid dropwise under stirring, react at the same temperature for 10 hours after adding, and let stand overnight. The next day, add sodium carbonate to neutralize to neutral, let stand and separate layers, separate 1,3-dichloroglycerin, extract the water layer with dichloromethane for three times, combine the extracts, recover dichloromethane under normal pressure, and the raffinate The 96-100°C / 50mmHg fraction was collected by fractional distillation to obtain 2.4 kg of the target product with a content of 99.5% and a yield of 86%.

preparation example 3

[0064] 1,3-dichloroglycerin preparation method (2)

[0065] Mix 8kg of glycerin and 670g of glacial acetic acid and heat to 100°C, pass through 7.8kg of dry hydrogen chloride gas, cool down after passing through enough, neutralize with solid sodium carbonate to pH 7.5, cool and filter sodium chloride, distill the filtrate under reduced pressure, and collect 96 -100°C / 50mmHg fraction, 7.5kg, yield 90%, purity 95%.

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Abstract

The invention provides a method for preparing sevelamer carbonate. The method comprises the following steps: a) polymerizing poly(allylamine hydrochloride) and 1, 3-dichloro-2-propanol at the temperature of between 30 and 70DEG C and the pH of 7-10, washing, and collecting the polymerized product to obtain sevelamer hydrochloride; b) dispersing the sevelamer hydrochloride in an alkali solution at the pH of 8-12 to obtain alkaline sevelamer; c) washing the alkaline sevelamer with water until neutrality to obtain an alkaline sevelamer cationic resin; and d) mixing a carbonic acid solution and the alkaline sevelamer cationic resin to obtain the sevelamer carbonate. By the method for preparing the sevelamer carbonate, the sevelamer carbonate has high purity; and in addition, by a Soxhlet extraction method, the mass transfer velocity can be improved and the reaction time is saved.

Description

technical field [0001] The invention relates to the field of biomedicine, in particular to a preparation method of sevelamer carbonate. Background technique [0002] The aliphatic polyamine cationic resin mainly includes Sevelamer Hydrochloride, Sevelamer Hydrochloride, Sevelamer Carbonate and any other possible salts, Colesevelam Hydrochloride, etc. These products have been used in the treatment of diseases, mainly for the treatment of hyperphosphatemia, hyperlipidemia, diabetes, gout, lowering uric acid, and even the adsorption of related ions. The principle of application of this type of aliphatic polyamine is essentially the adsorption of the resin. The adsorption of resin has been widely used in industry, agriculture or environmental protection. [0003] As a kind of aliphatic polyamine polymer, sevelamer carbonate has been disclosed by many prior art methods for its preparation. Its preparation method is disclosed in U.S. Patent Application Publication No. US2010 / 01...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/04C08J3/24C08K5/053C08L79/02
Inventor 郭欲晓徐环昕易崇勤王振国丁继军李劲任爱国
Owner NEW FOUNDER HLDG DEV LLC
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