Cellulose Acetate Triacetate I Crystal Structure Resin Compatibility

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Solution Overview

Problem

Current cellulose acetate technologies fail to achieve excellent compatibility with resins, reinforcement of resin materials, and maintain thermal stability while retaining the natural cellulose microfibril structure.

Innovation Solution

Cellulose acetate with a cellulose triacetate I crystal structure, having a weight loss of 5% at 200°C or higher when heated, and a controlled sulfuric acid content of 20-500 ppm, along with an average degree of substitution between 2.0 and 3.0, is produced through acetylation using a solvent system including acetic acid and a poor solvent for cellulose acetate, followed by washing and dispersion in acidic water.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Adaptability or versatility

If natural cellulose is chemically modified to increase hydrophobicity and compatibility with resins, then compatibility with hydrophobic resins improves, but the crystal structure of natural cellulose is lost

Engineering Contradiction:
Improvecompatibility with resinsVSAvoidcrystal structure
Core Design Contradiction:
Adaptability or versatilityVSStability of the object's composition

Solution Approach 1:

The patent controls the degree of substitution parameter within a specific range (0.56-2.52, preferably 1.5-2.5) to achieve hydrophobicity while preserving crystal structure. This parameter optimization allows the cellulose nanofiber to maintain its crystalline arrangement despite chemical modification, resolving the contradiction between compatibility improvement and structural stability.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite structure where chemically modified cellulose nanofibers (with improved resin compatibility) are combined with thermoplastic resins to form a fiber-reinforced composite material. This composite approach allows the modified cellulose to provide both compatibility and reinforcement without requiring complete structural transformation.

Inventive Principle:
Principle #40Composite materials

2Adaptability or versatility

If highly acetylated cellulose is produced to improve resin compatibility, then compatibility with hydrophobic resins improves, but thermal stability deteriorates

Engineering Contradiction:
Improvecompatibility with resinsVSAvoidthermal stability
Core Design Contradiction:
Adaptability or versatilityVSReliability

Solution Approach 1:

The patent optimizes the degree of substitution parameter within a controlled range (0.56-2.52) rather than achieving complete acetylation. This moderate modification level provides sufficient hydrophobicity for resin compatibility while avoiding excessive acetylation that would cause thermal degradation, thus resolving the contradiction between compatibility and thermal stability.

Inventive Principle:
Principle #35Parameter changes

3Productivity

If sulfuric acid is used as catalyst for acetylation to improve reaction efficiency, then productivity improves, but combined sulfuric acid content increases causing harmful effects

Engineering Contradiction:
Improveacetylation reaction efficiencyVSAvoidcombined sulfuric acid content
Core Design Contradiction:
ProductivityVSObject-generated harmful factors

Solution Approach 1:

The patent acknowledges that sulfuric acid catalyst residue causes thermal stability issues, but uses controlled amounts (20-500 ppm) during acetylation to maintain reaction efficiency. The process converts the potentially harmful catalyst into a controlled variable that, when properly managed, enables productive synthesis while minimizing harmful effects through subsequent washing steps.

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

Solution Approach 2:

The patent controls the combined sulfuric acid content parameter within a specific range (20-500 ppm) to balance reaction efficiency and thermal stability. This parameter control allows the acetylation reaction to proceed effectively while preventing excessive catalyst residue that would harm thermal properties, resolving the contradiction between productivity and harmful effects.

Inventive Principle:
Principle #35Parameter changes

4Strength

If cellulose nanofiber is used to reinforce resin material, then strength of resin material improves, but dispersibility in hydrophobic resins deteriorates due to hydrophilic nature

Engineering Contradiction:
Improvestrength of resin materialVSAvoiddispersibility in resins
Core Design Contradiction:
StrengthVSAdaptability or versatility

Solution Approach 1:

The patent modifies the chemical composition parameter of cellulose nanofiber by introducing acetyl groups to replace hydroxyl groups, changing the surface properties from hydrophilic to hydrophobic. This parameter change improves dispersibility in hydrophobic resins while maintaining the reinforcing capability, resolving the contradiction between strength enhancement and dispersibility.

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 resulting cellulose acetate exhibits excellent compatibility with resins, enhances resin reinforcement, and possesses superior thermal stability, maintaining the microfibril structure and ensuring effective dispersibility.

Implementation Method 1

acetylating fibrous raw material cellulose by reacting the fibrous raw material cellulose with acetic anhydride

Methodology Applied
Scientific EffectAcetylation reaction: Chemical Bonding

Implementation Method 2

acetylating fibrous raw material cellulose by reacting the fibrous raw material cellulose with acetic anhydride in a solvent containing a poor solvent for cellulose acetate and acetic acid; separating cellulose acetate obtained by the acetylation as a solid

Methodology Applied
Scientific EffectSolubility-based separation: Solvation

Implementation Method 3

dispersing fibrous cellulose acetate obtained by the washing and the drying in water under an acidic condition

Methodology Applied
Scientific EffectAcidic dispersion: Dispersion (of waves)

Data Source

PatentEP3808780B1Cellulose acetate, cellulose acetate fibers, cellulose acetate composition, method for producing cellulose acetate, and method for producing cellulose acetate composition
Publication Date: 2023.04.26 NIPPON PAPER IND CO LTD
  • EP3808780B1 patent drawingFigure 1
  • EP3808780B1 patent drawingFigure 2
  • EP3808780B1 patent drawingFigure 3A

AI summary

An object of the present invention is to provide cellulose acetate that has excellent compatibility with a resin, can reinforce a resin, and has excellent thermal stability. An embodiment of the present invention is cellulose acetate having a cellulose triacetate I crystal structure, wherein a temperature at which a weight loss relative to weight at 100°C reaches 5% is 200°C or higher when the cellulose acetate is heated at a heating rate of 10°C/min under a nitrogen atmosphere.