One-Pot Multi-Functionalized Cellulose for Nanofibrillation

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Solution Overview

Problem

Existing methods for preparing multi-functionalized cellulose fibers are costly, time-consuming, and do not achieve high yields, limiting their industrial application in composite materials and other fields.

Innovation Solution

A method involving one-pot simultaneous functionalization reactions to graft two or more functionalities onto cellulose fibers, including a carboxyl-containing group for facilitating nanofibrillation, under specific reactant concentrations and alkaline conditions.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Adaptability or versatility

If conventional sequential functionalization methods are used to prepare multi-functionalized cellulose, then multiple functional groups can be grafted onto cellulose, but the process becomes costly and time-consuming

Engineering Contradiction:
Improvemulti-functionality of celluloseVSAvoidreaction time
Core Design Contradiction:
Adaptability or versatilityVSLoss of time

Solution Approach 1:

The patent combines multiple sequential functionalization reactions into a single simultaneous reaction step. Multiple functional groups are grafted onto cellulose in one-pot conditions, eliminating the need for separate reaction steps, intermediate isolations, and multiple purification cycles, thereby dramatically reducing reaction time and operational complexity

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent employs preliminary activation of cellulose hydroxyl groups under alkaline conditions before introducing multiple functionalizing agents. This preliminary action creates reactive cellulose alkoxide species that can simultaneously react with different functionalizing agents, enabling concurrent multi-functionalization in a single reaction step

Inventive Principle:
Principle #10Preliminary action

2Adaptability or versatility

If conventional sequential functionalization methods are used to prepare multi-functionalized cellulose, then multiple functional groups can be grafted onto cellulose, but the cost increases

Engineering Contradiction:
Improvemulti-functionality of celluloseVSAvoidmanufacturing cost
Core Design Contradiction:
Adaptability or versatilityVSEase of manufacture

Solution Approach 1:

The patent merges multiple functionalization reactions and purification steps into a single integrated process. By performing simultaneous functionalization in one-pot conditions and using a single filtration step for purification, the patent eliminates repeated use of solvents, reagents for intermediate treatments, and multiple purification operations, thereby significantly reducing manufacturing costs

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent employs water as the reaction medium and uses the cellulose fibers themselves as the support matrix throughout the process. The reaction mixture can be directly filtered and washed with water, eliminating the need for organic solvents and complex purification protocols, thereby reducing both material costs and processing costs

Inventive Principle:
Principle #25Self-service

3Adaptability or versatility

If conventional functionalization methods are used, then functional groups can be grafted onto cellulose, but the yield is low

Engineering Contradiction:
Improvemulti-functionality of celluloseVSAvoidfunctionalization yield
Core Design Contradiction:
Adaptability or versatilityVSProductivity

Solution Approach 1:

The patent optimizes reaction parameters including pH (maintained alkaline), temperature, and the concentration and ratio of multiple functionalizing agents to maximize grafting efficiency. By carefully controlling these parameters, the patent achieves high degrees of substitution for multiple functional groups simultaneously, thereby maximizing functionalization yield

Inventive Principle:
Principle #35Parameter changes

4Shape

If mechanical treatment methods are used to prepare nanofibrillated cellulose, then nanofibrils can be obtained, but high energy consumption is required

Engineering Contradiction:
Improvenanofibril structureVSAvoidenergy consumption
Core Design Contradiction:
ShapeVSUse of energy by moving object

Solution Approach 1:

The patent performs preliminary chemical functionalization of cellulose fibers before mechanical nanofibrillation. The introduced functional groups create electrostatic repulsion between fibers, which pre-weakens inter-fiber bonding and reduces the mechanical energy required for subsequent nanofibrillation, thereby lowering overall energy consumption

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent modifies the chemical properties of cellulose by introducing charged functional groups, which changes the physical interactions between fibers. This chemical modification reduces the strength of fiber-fiber bonding, allowing mechanical disintegration into nanofibrils to occur with lower energy input compared to treating native cellulose

Inventive Principle:
Principle #35Parameter changes

5Shape

If mechanical treatment methods are used to prepare nanofibrillated cellulose, then nanofibrils can be obtained, but the nanofiber structure is damaged

Engineering Contradiction:
Improvenanofibril structureVSAvoidnanofiber integrity
Core Design Contradiction:
ShapeVSStrength

Solution Approach 1:

The patent introduces functional groups that create electrostatic repulsion between nanofibrils during mechanical treatment. This repulsive force counteracts the compressive and shear stresses experienced by nanofibrils during homogenization, preventing structural collapse and maintaining nanofiber integrity and crystallinity in the final product

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

This method enables the rapid preparation of multi-functionalized cellulose fibers with high yields and low costs, maintaining the integrity of the carboxyl charge and facilitating subsequent nanofibrillation without increasing energy requirements.

Implementation Method 1

subjecting cellulose fibers to: a first functionalization step for grafting a first organic functional group on the cellulose polymer, by reacting the cellulose with a first reactant... and a second functionalization step for grafting on the cellulose polymer a second organic functional group...

Methodology Applied
Scientific EffectChemical Bonding: Chemical Bonding

Implementation Method 2

One of these methods, comprising providing cellulose fibers with a carboxymethyl function and an aldehyde function... The TEMPO-catalyzed oxidation was proposed as one of the most promising methods for the production of cellulose nanofibers. Indeed, TEMPO transforms the primary hydroxyl at C6 in the cellulose chain into a carboxylate group, thereby creating electrostatic repulsions and facilitating the separation of cellulose nanofibers

Methodology Applied
Scientific EffectElectrostatic Repulsion: Ion Repulsion/Attraction

Data Source

PatentUS20250146186A1A method of preparing multi-functionalized cellulose and use thereof for preparing multi-functionalized nanofibrillated cellulose
Publication Date: 2025.05.08 INST NAT DE RECH POUR LAGRICULTURE
  • US20250146186A1 patent drawing
  • US20250146186A1 patent drawing
  • US20250146186A1 patent drawing

AI summary

A method of preparing multi-functionalized cellulose, including subjecting cellulose fibers concomitantly, in one-pot in an alkaline reaction medium, to a first functionalization step for grafting a first organic functional group on the cellulose and a second functionalization step for grafting a second organic functional group on the cellulose. The multi-functionalized cellulose fibers thus obtained, and containing at least a carboxyl function, are particularly suitable for being subjected to a nanofibrillation step to prepare multi-functionalized nanofibrillated cellulose.