Cellulose Nanofiber Esterification for Stable Dispersion

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Solution Overview

Problem

Current methods for preparing cellulose nanofibers face challenges such as low production efficiency, insufficient dispersion, and poor compatibility with synthetic resins due to strong hydrogen bonding and hydrophilic surfaces, leading to weak reinforcement and water resistance in composite materials.

Innovation Solution

A method involving simultaneous mechanical breaking and surface modification through esterification reactions, where cellulose is mixed with an organic solvent and an esterification agent, allowing for stable dispersion of cellulose nanofibers with diameters between 2-1000 nm and improved compatibility with synthetic resins.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If high pressure homogenizing method is used to prepare cellulose nanofibers, then nanofiber production is achieved, but processing time is long and production efficiency is low

Engineering Contradiction:
Improveproduction efficiencyVSAvoidprocessing time
Core Design Contradiction:
ProductivityVSLoss of time

Solution Approach 1:

The patent combines mechanical breaking and surface modification into a single simultaneous process step. The cellulose is subjected to mechanical force to break it into nanofibers while esterification reaction occurs concurrently to modify the surface, eliminating the need for separate oxidation and dispersion steps required in prior art methods.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent changes the chemical parameters of the cellulose surface by introducing ester groups through esterification reaction. This chemical modification alters the surface properties of the nanofibers, providing steric hindrance that prevents aggregation and enables stable dispersion in both polar and non-polar solvents without requiring lengthy processing times.

Inventive Principle:
Principle #35Parameter changes

2Adaptability or versatility

If cellulose nanofibers with hydrophilic surfaces are used, then dispersion in water is achieved, but compatibility with synthetic resins is poor and water resistance is weak

Engineering Contradiction:
Improvecompatibility with synthetic resinsVSAvoidwater resistance
Core Design Contradiction:
Adaptability or versatilityVSStability of the object's composition

Solution Approach 1:

The patent modifies the chemical parameters of the cellulose surface by introducing ester groups through esterification reaction. This changes the surface from hydrophilic to hydrophobic character, enabling compatibility with synthetic resins while maintaining stable dispersion. The ester groups provide both steric stabilization and chemical compatibility with organic matrices.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite structure at the molecular level by grafting ester groups onto the cellulose nanofiber surface. This composite approach combines the mechanical strength of cellulose with the hydrophobic and resin-compatible properties of ester groups, achieving both reinforcement and water resistance in the final composite material.

Inventive Principle:
Principle #40Composite materials

3Strength

If strong hydrogen bonding interactions among nanofiber units are present, then mechanical strength is high, but preparation of nanofibers becomes very difficult

Engineering Contradiction:
Improvemechanical strengthVSAvoidpreparation difficulty
Core Design Contradiction:
StrengthVSEase of manufacture

Solution Approach 1:

The patent changes the chemical parameters at the nanofiber surface by introducing ester groups that create steric hindrance. This modification weakens the strong hydrogen bonding interactions between adjacent nanofibers, allowing them to be separated into individual nanofibers during mechanical processing while maintaining the intrinsic mechanical strength of each nanofiber unit.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The ester groups act as intermediary structures between the cellulose chains. They provide steric hindrance that prevents direct hydrogen bonding between adjacent nanofibers, serving as a physical barrier that facilitates nanofiber separation while preserving the core mechanical properties of the cellulose structure.

Inventive Principle:
Principle #24Intermediary (Mediator)

4Productivity

If oxidation method is used to introduce surface charges, then electrostatic repulsion and dispersion are achieved, but procedures require accurate control and are complex

Engineering Contradiction:
Improvedispersion efficiencyVSAvoidprocedure complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent replaces the chemical oxidation process with a mechanical breaking process combined with esterification. Instead of using complex oxidation procedures that require precise control of reagents and conditions, the method uses mechanical force to break cellulose into nanofibers while simultaneously performing esterification, simplifying the overall procedure.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent merges the nanofiber breaking process and surface modification process into a single operation. The mechanical breaking that separates cellulose into nanofibers occurs simultaneously with the esterification reaction that modifies the surface, eliminating the need for separate, carefully controlled oxidation steps.

Inventive Principle:
Principle #5Merging (Combining)

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

This method enables high-efficiency production of stably dispersed cellulose nanofibers with enhanced compatibility and strength in composite materials, improving the mechanical properties and water resistance of the final products.

Implementation Method 1

an esterification reaction is occurred at the same time when the cellulose is being mechanically disintegrated, the nanofibers may be prepared in high efficiency and in big batch. The cellulose processed in the method keeps the fine fiber structure, while the cellulose is esterified and disintegrated by introducing ester group(s) into the contacting interfaces of the adjacent fine fibers.

Methodology Applied
Scientific EffectEsterification reaction: Chemical Bonding

Implementation Method 2

Cellulose and dispersant solvent are added into a ball mill pot with hard balls made of metal or ceramic. The cellulose is dissociated through the impact force of the hard balls from rotation and vibration of the ball mill pot.

Methodology Applied
Scientific EffectImpact force: Impact Force

Implementation Method 3

The fine particles are obtained from the suspension liquid by a high pressure homogenizer, in which the liquid is erupted from slim tubes under high pressure and hits onto the solid wall.

Methodology Applied
Scientific EffectHigh pressure: Pressure Increase

Implementation Method 4

The obtained suspension liquid is subjected to centrifugal separation, so that the dispersed nanofibers are collected.

Methodology Applied
Scientific EffectCentrifugal separation: Centrifugal Separation

Data Source

PatentUS9725583B2Method for preparing cellulose nanofiber capable of being stably dispersed
Publication Date: 2017.08.08 TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
  • US9725583B2 patent drawing
  • US9725583B2 patent drawing
  • US9725583B2 patent drawing

AI summary

A method for preparing stably dispersed cellulose nanofibers comprises the following steps: 1) mixing cellulose and an organic solvent, the percentage of the cellulose being 1% to 15% in weight; 2) adding an esterification agent into the resultant mixture of step 1), the molar ratio of the esterification agent to the cellulose being from 1:0.1 to 4; and 3) physically breaking the resultant mixture of step 2) until a suspension liquid with stably dispersed cellulose nanofibers of 2-1000 nm in diameter and 10-100 μm in length is obtained, an esterification reaction of hydroxyl group(s) on the surface of cellulose fibers occurring at the time of the breaking. Also disclosed are dispersed cellulose nanofibers with improved compatibility to the matrix than the untreated cellulose and an improved strength of the composite materials.