Method for preparing hydroxypropyl methylcellulose acetate succinate

A technology of hydroxypropyl methylcellulose and hypromellose acetate, which is applied in the field of preparation of enteric coating materials, can solve the problems of too many solvents, human hazards, unfavorable industrial production, etc., and achieve simple production operations and mild reaction conditions , the effect of less by-products

Inactive Publication Date: 2015-04-29
ANHUI SUNHERE PHARMA EXCIPIENTS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are microwave radiation method and solvent method to prepare hypromellose acetate succinate. In microwave radiation method, microwave radiation is harmful to human body and is not conducive to i

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Pump 110kg of glacial acetic acid and 65kg of acetic anhydride into the stainless steel reaction kettle, start stirring, then add 25kg of anhydrous sodium acetate, 22kg of succinic anhydride, 25kg of hypromellose E50, 25kg of hypromellose E100 and permanganate Put 160g of potassium into the reactor, fill the reactor with nitrogen, until the pressure in the reactor is 0.15Mpa, heat, control the temperature at 40°C, keep it for 1 hour, raise the temperature to 55°C, keep it for 1.5 hours, increase Temperature to 75°C, reaction for 5 hours, washing, crushing, centrifugation, drying, sieving and packaging.

[0020] After testing, the content of methoxyl group is 16.2% (mass fraction, the same below), the content of hydroxypropoxyl group is 9.4% (mass fraction, the same below), the content of acetyl group is 8.6% (mass fraction, the same below), and the content of succinyl group is 10.9% % (mass fraction, the same below), viscosity 6500mpa.s.

Embodiment 2

[0022] Pump 120kg of glacial acetic acid and 75kg of acetic anhydride into the stainless steel reaction kettle, start stirring, then add 22kg of anhydrous sodium acetate, 26kg of succinic anhydride, 40kg of hypromellose E50, 10kg of hypromellose E100 and permanganate Put 250g of potassium into the reactor, fill the reactor with nitrogen, until the pressure in the reactor is 0.2Mpa, heat, control the temperature at 50°C, keep it for 1.5 hours, raise the temperature to 60°C, keep it for 1.5 hours, increase Temperature to 90°C, reaction for 6 hours, washing, crushing, centrifugation, drying, sieving and packaging.

[0023] After testing, the content of methoxy group is 13.5%, the content of hydroxypropoxy group is 6.2%, the content of acetyl group is 11.4%, the content of succinyl group is 19.6%, and the viscosity is 320mpa.s.

Embodiment 3

[0025] Pump 120kg of glacial acetic acid and 75kg of acetic anhydride into the stainless steel reaction kettle, start stirring, then add 22kg of anhydrous sodium acetate, 26kg of succinic anhydride, 43kg of hypromellose E50, 7kg of hypromellose E100 and permanganate Put 260g of potassium into the reactor, fill the reactor with nitrogen, until the pressure in the reactor is 0.2Mpa, heat, control the temperature at 50°C, keep it for 1.5 hours, raise the temperature to 60°C, keep it for 2 hours, increase Temperature to 85°C, reaction for 6 hours, washing, crushing, centrifugation, drying, sieving and packaging.

[0026] After testing, the content of methoxy group is 14.1%, the content of hydroxypropoxy group is 7.2%, the content of acetyl group is 12.5%, the content of succinyl group is 18.4%, and the viscosity is 120mpa.s.

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Abstract

The invention discloses a method for preparing hydroxypropyl methylcellulose acetate succinate. The method comprises the following two steps: an esterification step: adding hydroxypropyl methylcellulose, acetic acid, anhydrous sodium acetate, acetic anhydride, succinic anhydride and a catalyst in proportion to a reaction vessel, and heating and stirring to undergo an esterification reaction; a purification step: after the completion of the reaction, slowly pouring a product into water while stirring, washing the product, crushing and drying to obtain the hydroxypropyl methylcellulose acetate succinate, wherein a three-step temperature raising method is adopted by heating. The method provided by the invention has the advantages of simplicity in industrial production operation, less by-products, mild reaction conditions, and adjustability of viscosity within 100-10000mpa.s, and is suitable for different application requirements.

Description

technical field [0001] The invention relates to a method for preparing an enteric coating material, in particular to a method for preparing hypromellose acetate succinate. Background technique [0002] Hydroxypropyl cellulose acetate succinate (HPMCAS) is a mixed ester of hydroxypropyl methylcellulose (HPMC) acetate and succinate. It is a new type of enteric coating material with superior performance and has been approved by Japan and the United States. Used in medicine and food. In addition to being used for enteric coating, it can also be used to prepare microcapsules, microspheres and sustained-release and controlled-release preparations of drugs with polymer carriers. It has the characteristics of stable performance and long shelf life, which is longer than the shelf life of the excellent HPMCP currently on the market. More than double the length, the film-forming performance is good, the film flexibility is appropriate and not brittle, the solubility is good, safe and ...

Claims

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Application Information

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IPC IPC(8): C08B13/00
Inventor 武蛟毕勇刘传祥李杰余伟夏叶青叶永超徐玉勋朱岩陈晓雪
Owner ANHUI SUNHERE PHARMA EXCIPIENTS
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