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Preparation method of hydroxypropyl methyl cellulose phthalate

A technology of hydroxypropyl methylcellulose and phthalate, which is applied in the field of preparation of hydroxypropyl methylcellulose phthalate, can solve the problem of high water consumption and phthaloyl content Low-level problems, to achieve the effect of reducing water consumption, improving purity, and reducing the content of non-target products

Active Publication Date: 2014-12-24
HERCULES TIANPU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the phthaloyl content of the product prepared by this method is low, and the water consumption in the production process is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Add 1.0kg of phthalic anhydride, 3.0kg of acetic acid and 0.7kg of sodium acetate into the reaction kettle, stir and heat up to 40°C.

[0035] (2) Weigh 0.9kg hydroxypropyl methylcellulose, add it in the reactor under stirring, and feed N into the reactor. 2 Pressurize to 0.9MPa, raise temperature to 70°C, and keep constant temperature until completely dissolved.

[0036] (3) Raise the temperature to 90° C., maintain the pressure in the reaction vessel at 0.3 MPa to 0.9 MPa, and react at a constant temperature for 3.5 hours.

[0037] (4) After the reaction is finished, cool down to 30° C. and discharge.

[0038] (5) Stir and granulate at a speed of 200r / min to 400r / min.

[0039] (6) Wash with water at 0°C to 50°C until the pH is neutral, centrifuge, dry and pulverize to obtain the product.

Embodiment 2

[0041] (1) Add 1.1kg of phthalic anhydride, 3.5kg of acetic acid and 0.6kg of sodium acetate into the reaction kettle, stir and heat up to 45°C within 30 minutes.

[0042] (2) Weigh 0.8kg hydroxypropyl methylcellulose, add it in the reactor under stirring, and feed N into the reactor. 2 Pressurize to 0.7MPa, raise temperature to 75°C, and keep constant temperature until completely dissolved.

[0043] (3) Raise the temperature to 85° C., maintain the pressure in the reaction vessel at 0.3 MPa to 0.9 MPa, and react at a constant temperature for 4 hours.

[0044] (4) After the reaction is finished, cool down to 35° C. and discharge.

[0045] (5) Stir and granulate at a speed of 200r / min to 400r / min.

[0046] (6) Wash with water at 0°C to 50°C until the pH is neutral, centrifuge, dry and pulverize to obtain the product.

Embodiment 3

[0048] (1) Add 1.2kg of phthalic anhydride, 4.0kg of acetic acid and 0.5kg of potassium acetate into the reaction kettle, stir and heat up to 35°C.

[0049] (2) Weigh 1.0kg of hydroxypropyl methylcellulose, add it into the reactor under stirring, and feed N into the reactor. 2 Pressurize to 0.5MPa, raise temperature to 78°C, and keep constant temperature until completely dissolved.

[0050] (3) Raise the temperature to 90° C., maintain the pressure in the reaction vessel at 0.3 MPa to 0.9 MPa, and react at a constant temperature for 4 hours.

[0051] (4) After the reaction is finished, cool down to 40°C and discharge.

[0052] (5) Stir and granulate at a speed of 200r / min to 400r / min.

[0053] (6) Wash with water at 0°C to 50°C until the pH is neutral, centrifuge, dry and pulverize to obtain the product.

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Abstract

The invention belongs to the field of auxiliary materials of medicines, particularly relates to a preparation method of hydroxypropyl methyl cellulose phthalate, and aims to provide the preparation method for the hydroxypropyl methyl cellulose phthalate, wherein the hydroxypropyl methyl cellulose phthalate prepared according to preparation method is higher in phthalic acyl content. The preparation method disclosed by the invention is characterized in that the reaction temperature is raised to 85-100 DEG C, the internal pressure of a reaction container is maintained to 0.3-0.9MPa, and the reacting time is 3.5-6 h. For the preparation method disclosed by the invention, the aim of promoting a positive reaction is achieved by adjusting the reaction temperature and reaction pressure, and the phthalic acyl content of a product can be increased to 25% from 21%. The preparation method disclosed by the invention has the advantages that the synthetic technology is simple, and the reaction condition is easy to control, so that the preparation method is suitable for expanding the production.

Description

technical field [0001] The invention belongs to the field of pharmaceutical excipients, and in particular relates to a preparation method of hydroxypropyl methylcellulose phthalate. Background technique [0002] Hydroxypropyl methylcellulose phthalate, white odorless and tasteless granules, is a kind of enteric coating material with excellent performance, which can make the drugs work in the intestinal tract or absorb in the small intestine. It is released in the intestine to avoid stomach discomfort or nausea caused by irritating drugs, so enteric coating plays an important role in fully exerting the curative effect of the drug and ensuring the stability of the drug. [0003] U.S. Patent No.3629237 discloses a kind of utilization 15cp~100cp of hydroxypropyl methylcellulose mixed with phthalic anhydride and sodium acetate in acetic acid solvent to produce hydroxypropyl methylcellulose phthalate method of preparation. However, the phthaloyl content of the product prepared b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B13/00A61K47/38
Inventor 胡少琴杜维密杨羽茂周能武谢显春周光华
Owner HERCULES TIANPU CHEM
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