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Novel technology for preparing hydroxypropyl methyl cellulose derivative

A technology of hydroxypropyl methylcellulose and derivatives, which is applied in the field of new preparation process of cellulose ether ester, which can solve the problems of environmental pollution, high content of free acid in products, strong corrosion of equipment, etc.

Inactive Publication Date: 2016-01-27
TAIAN RUITAI CELLULOSE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation of hydroxypropylmethylcellulose esterified derivatives such as hydroxypropylmethylcellulose titanate and hydroxypropylmethylcellulose succinate at home and abroad mainly adopts the reaction system of glacial acetic acid-sodium acetate. There are many disadvantages in industrial production, such as the reaction medium is highly corrosive to the equipment, the solvent is not recyclable, the environmental pollution is serious, and the free acid content of the product is too high, which seriously affects the quality and performance of the product.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Dissolve 10g of hydroxypropyl methylcellulose in dioxane (100mL), then add 10g of phthalic anhydride to react overnight at room temperature, add an appropriate amount of ethyl acetate to the reaction system to precipitate the product, filter under normal pressure, and the filtrate After recovery, it can be reused after being concentrated under reduced pressure and dried in vacuum; the filtered product is washed and filtered with dilute hydrochloric acid and ethyl acetate in turn, and dried in a vacuum oven to obtain the target product hydroxypropyl methylcellulose titanate. The degree of acylation is 15.1%, and the content of free acid is 0.16%.

Embodiment 2

[0018] Dissolve 10g of hydroxypropyl methylcellulose in dioxane (100mL), then add 20g of phthalic anhydride and then raise the temperature to 60°C for 5 hours; cool to room temperature, add an appropriate amount of ethyl acetate to the reaction system to make The product is precipitated, filtered under normal pressure, the filtrate is recovered, concentrated under reduced pressure and dried in vacuum before being reused; the filtered product is washed with dilute hydrochloric acid and ethyl acetate and filtered, and dried in a vacuum oven to obtain the target product hydroxypropyl methylcellulose Titanate, the degree of acylation is 31.5% and the content of free acid is 0.27%.

Embodiment 3

[0020] Dissolve 10g of hydroxypropyl methylcellulose in dimethylformamide (80mL), then add 10g of succinic anhydride and react overnight at room temperature; then add an appropriate amount of ethyl acetate to the reaction system to precipitate the product, filter under normal pressure, and the filtrate After recovery, it can be reused after being concentrated under reduced pressure and dried in vacuum; the filtered product is washed with dilute hydrochloric acid and ethyl acetate and filtered, and dried in a vacuum oven to obtain the target product hydroxypropyl methylcellulose succinate. The degree of acylation is 11.7%, and the content of free acid is 0.41%.

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Abstract

The invention discloses a novel technology for preparing a hydroxypropyl methyl cellulose derivative. The novel technology comprises the steps that hydroxypropyl methyl cellulose, a solvent, a catalyst and an esterifying agent are added into a reaction container, stirring and heating are carried out for an esterification reaction, the temperature is decreased to indoor temperature after the reaction is finished, a precipitating agent is added, and precipitate is filtered and washed to obtain the hydroxypropyl methyl cellulose derivative. The preparation technology is simple and efficient, and has the advantages that the reaction condition is moderate, product aftertreatment is simple, the product yield is high, and acid residue amount is small.

Description

technical field [0001] The invention relates to a novel preparation process of cellulose ether ester, which belongs to the field of chemical synthesis. Background technique [0002] Hydroxypropyl methylcellulose titanate and hydroxypropyl methylcellulose succinate are new pH-sensitive film coating materials. Significantly improve the bioavailability and targeting of the loaded drug, it has been widely used in enteric-coated preparations, sustained-release preparations and targeted preparations, and it is also a cellulose derivative excipient that needs to be developed and applied urgently in my country. [0003] At present, the preparation of hydroxypropylmethylcellulose esterified derivatives such as hydroxypropylmethylcellulose titanate and hydroxypropylmethylcellulose succinate at home and abroad mainly adopts the reaction system of glacial acetic acid-sodium acetate. There are many disadvantages in industrial production, such as strong corrosion of reaction medium to e...

Claims

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Application Information

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IPC IPC(8): C08B13/00
Inventor 唐汝培吕兴富孙建刚
Owner TAIAN RUITAI CELLULOSE
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