HPMCAS Grain Size Control via Temperature-Regulated Precipitation

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Solution Overview

Problem

Conventional methods for preparing hydroxypropyl methylcellulose acetate succinate (HPMCAS) result in a low fraction of grains with appropriate grain size and slow dissolving velocity in solvents.

Innovation Solution

A method involving esterification of hydroxypropyl methylcellulose with acetic anhydride and succinic anhydride in the presence of a catalyst, followed by continuous or intermittent addition to water, controlling reaction and granulating temperatures, and using a sufficient amount of water to achieve HPMCAS grains with a high fraction of grains in the 841 to 1,190 µm size range.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If purified water is added to the reaction solution at room temperature to form HPMCAS grains, then the grains are formed, but the fraction of grains with appropriate grain size is low and the dissolving velocity is slow

Engineering Contradiction:
Improvegrain size distributionVSAvoiddissolving velocity
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent applies parameter changes by controlling the reaction solution temperature within 45-60°C and water temperature within 20-30°C during granulation, and adjusting the water-to-reaction-medium ratio to 12-20 times. These parameter optimizations produce grains with appropriate size distribution (25 wt% or greater in 841-1,190 μm range) while maintaining high dissolving velocity, resolving the contradiction between manufacturing precision and productivity

Inventive Principle:
Principle #35Parameter changes

2Ease of manufacture

If the reaction solution is added to water without temperature control, then the process is simple, but the grain size distribution is uncontrolled and dissolving properties are poor

Engineering Contradiction:
Improveprocess simplicityVSAvoidgrain size control
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent implements temperature control parameters (reaction solution: 45-60°C, water: 20-30°C) and water-to-reaction-medium ratio (12-20 times) to achieve controlled grain size distribution. This systematic parameter control maintains ease of manufacture while significantly improving grain size precision and dissolving properties

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The method produces HPMCAS powder with a high fraction of grains in the appropriate size range, leading to increased dissolving velocity and reduced processing time when dissolved in solvents.

Implementation Method 1

esterifying hydroxypropyl methylcellulose (HPMC), acetic anhydride, and succinic anhydride in a reaction medium in the presence of a catalyst (esterification step)

Methodology Applied
Scientific EffectEsterification: Chemical Bonding

Implementation Method 2

forming grains by continuously or intermittently adding the reaction solution to water (granulating step)

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Data Source

PatentEP3091036B1Method for preparing hydroxypropyl methylcellulose acetate succinate (hpmcas) grains having controlled grain size distribution, and hpmcas powder
Publication Date: 2022.01.26 LOTTE FINE CHEMICAL CO LTD
  • EP3091036B1 patent drawingFigure 1
  • EP3091036B1 patent drawingFigure 2
  • EP3091036B1 patent drawing

AI summary

Disclosed are a method for preparing hydroxypropyl methylcellulose acetate succinate (HPMCAS) grains and HPMCAS grains. The disclosed method for preparing HPMCAS grains comprises: a step of esterifying hydroxypropyl methylcellulose (HPMC), acetic anhydride, and succinic anhydride in a reaction medium in the presence of a catalyst so as to obtain a reaction solution containing HPMCAS (esterification step); and a step of continuously or intermittently putting the reaction solution into water so as to form grains (granulating step).