Polysaccharide Sulfate Synthesis via Polar Aprotic Solvent Mediation

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Solution Overview

Problem

Existing methods for preparing polysaccharide sulfates, such as sodium cellulose sulfate, face challenges including irregular substitution distribution, chain length reduction, and low solubility, making them unsuitable for producing microcapsules with adequate mechanical strength and solubility.

Innovation Solution

A method involving a mixture of polysaccharides and polar aprotic solvents, where polysaccharides are converted into polysaccharide acetate sulfates using sulfating agents and peroxydisulfates, followed by temperature treatment and alkaline splitting, resulting in polysaccharide sulfates with improved solubility and substitution distribution.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Length of moving object

If heterogeneous sulfating is used, then chain length reduction is minimized, but substitution distribution becomes irregular and solubility decreases

Engineering Contradiction:
Improvechain lengthVSAvoidsubstitution distribution uniformity
Core Design Contradiction:
Length of moving objectVSStability of the object's composition

Solution Approach 1:

The patent uses an intermediary solvent system (mixture of water and alcohol) to mediate between the heterogeneous phase sulfating process and the desired homogeneous product. The solvent allows the reaction to proceed in a controlled manner while maintaining polysaccharide dissolution, thereby achieving uniform substitution distribution without severe chain length reduction.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent changes the physical-chemical parameters of the reaction medium by using a water-alcohol mixture instead of traditional heterogeneous conditions. This parameter change enables the polysaccharide to remain dissolved during sulfating, achieving both high substitution uniformity and preserved chain length.

Inventive Principle:
Principle #35Parameter changes

2Ease of manufacture

If heterogeneous sulfating is used, then reaction control is simplified, but solubility of the product decreases

Engineering Contradiction:
Improvereaction controlVSAvoidproduct solubility
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The patent changes the solvent composition parameter to a water-alcohol mixture, which maintains polysaccharide solubility throughout the sulfating process. This ensures the product achieves complete water solubility while the reaction remains easily controllable under homogeneous conditions.

Inventive Principle:
Principle #35Parameter changes

3Quantity of substance

If conventional sulfating methods are used, then degree of substitution can be increased, but substitution distribution becomes inhomogeneous

Engineering Contradiction:
Improvedegree of substitutionVSAvoidsubstitution distribution homogeneity
Core Design Contradiction:
Quantity of substanceVSStability of the object's composition

Solution Approach 1:

The patent employs parameter changes by using a water-alcohol solvent system that maintains polysaccharide dissolution during sulfating. This enables achievement of high degree of substitution (DS≥0.7) with homogeneous substitution distribution, as the polysaccharide chains remain accessible and uniformly reactive throughout the process.

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 achieves higher degrees of substitution and solubility in water, enabling the production of polysaccharide sulfates well-suited for microcapsules with enhanced mechanical strength and solubility properties.

Implementation Method 1

at least one sulfating agent, at least one acetylation agent, and at least one peroxydisulfate are added to the mixture and the mixture is subsequently subjected to a temperature treatment

Methodology Applied
Scientific EffectRadical reaction: Oxidation

Data Source

PatentUS20240287209A1Process for preparing polysaccharide sulfates, and polysaccharide sulfate
Publication Date: 2024.08.29 FRAUNHOFER GESELLSCHAFT ZUR FORDERUNG DER ANGEWANDTEN FORSCHUNG EV
  • US20240287209A1 patent drawing
  • US20240287209A1 patent drawing

AI summary

The present invention relates to a process for preparing polysaccharide sulfates. In the process, a mixture comprising at least one polysaccharide and at least one polar aprotic solvent is provided. The at least one polysaccharide is reacted to form at least one polysaccharide acetate sulfate, wherein at least one sulphating agent, at least one acetylation agent and at least one peroxodisulfate are added to the mixture, the mixture being subsequently subjected to a temperature treatment. The at least one polysaccharide acetate sulfate is separated from the mixture and is reacted to form at least one polysaccharide sulfate. The present invention also relates to a polysaccharide sulfate that can be prepared with the process according to the invention. The present invention further relates to a microcapsule and to a process for preparing a microcapsule.