PAN Spinning Solution Preparation for Homogeneous Salification

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Solution Overview

Problem

Existing processes for producing carbon fibers from acrylic fiber precursors (PAN) face challenges in achieving homogeneous salification of carboxylic groups, leading to uneven heat treatment and unsatisfactory quality, with additional steps and hazardous reagents like gaseous ammonia required for improved performance.

Innovation Solution

A process involving a homogeneous suspension of acrylonitrile copolymer with a solvent mixture of DMSO and aqueous ammonia or amines at controlled temperatures, followed by rapid heating, ensures complete salification of acid groups, forming a gel-free spinning solution suitable for high-quality carbon fibers.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Strength

If gaseous ammonia is used for salification to improve fiber performance, then elastic modulus and tenacity are enhanced, but process complexity and safety hazards increase

Engineering Contradiction:
Improvefiber strengthVSAvoidprocess complexity
Core Design Contradiction:
StrengthVSDevice complexity

Solution Approach 1:

The patent changes the physical state parameter of the ammonia reagent from gaseous to aqueous solution form. This parameter change maintains the chemical salification function while eliminating the need for specialized gas handling equipment and safety systems, thus reducing process complexity while preserving fiber strength enhancement

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses readily available aqueous ammonia solution instead of requiring complex gas delivery systems. The aqueous solution can be easily handled, applied, and disposed of, replacing the need for sophisticated gaseous ammonia infrastructure while achieving the same salification effect for improved fiber mechanical properties

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

2Manufacturing precision

If traditional discontinuous two-step process is used, then polymer isolation is achieved, but production efficiency and energy consumption worsen

Engineering Contradiction:
Improvepolymer isolation qualityVSAvoidproduction efficiency
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent merges the polymer isolation step with the spinning solution preparation step by directly using the polymerization solvent as the spinning solvent. This eliminates the need for separate isolation and dissolution operations, maintaining polymer purity while significantly improving production efficiency and reducing energy consumption

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent makes the polymerization solvent serve multiple functions: it acts as both the reaction medium for polymerization and the spinning solvent for fiber formation. This multi-functionality eliminates intermediate processing steps while ensuring the solvent is already optimized for the polymer structure, thereby improving both isolation quality and production efficiency

Inventive Principle:
Principle #6Universality (Multi-functionality)

3Loss of time

If salification is performed only on fiber surface, then treatment time is reduced, but homogeneity and fiber quality deteriorate

Engineering Contradiction:
Improvetreatment timeVSAvoidsalification homogeneity
Core Design Contradiction:
Loss of timeVSManufacturing precision

Solution Approach 1:

The patent performs salification during the spinning process itself rather than as a separate post-treatment step. The aqueous ammonia solution is introduced into the spinning bath where fibers are formed, allowing salification to occur simultaneously with fiber solidification. This preliminary action ensures homogeneous penetration of ammonia throughout the fiber structure while maintaining efficient production timing

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The spinning bath acts as an intermediary medium that facilitates uniform distribution of ammonia throughout the forming fibers. The aqueous environment of the spinning bath allows ammonia to diffuse evenly into the fiber matrix during the formation process, ensuring homogeneous salification without requiring extended treatment times or additional processing steps

Inventive Principle:
Principle #24Intermediary (Mediator)

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 production of carbon fibers with enhanced tenacity and elastic modulus by ensuring uniform treatment of carboxylic groups, reducing production costs and energy consumption, and eliminating the need for hazardous reagents.

Implementation Method 1

the use of nitrogen compounds in the production process of the PAN precursor, in particular the use of primary and secondary low-molecular-weight amines and, above all, ammonia... the PAN precursor containing itaconic acid is treated with amines or ammonia during the spinning phase... the salification process of the carboxylic groups with ammonia or amines

Methodology Applied
Scientific EffectChemical reaction (salification): Chemical Bonding

Implementation Method 2

heating the homogeneous suspension coming from step i) to a temperature ranging from 70 to 150°C in a time ranging from 0.5 to 30 minutes, until the complete dissolution of the copolymer and the formation of a homogeneous solution

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 3

dissolved in a suitable solvent to be spun and transformed into a fiber precursor of carbon fiber. The solvents most commonly used for the preparation of the spinning solution are: dimethylacetamide (DMAC), dimethylformamide (DMF)... dimethylsulfoxide (DMSO)

Methodology Applied
Scientific EffectSolvation: Solvation

Implementation Method 4

the heat treatment of a suitable acrylic precursor (PAN), having a chemical composition suitable for allowing a controlled gradual elimination of heteroatoms... the heat developed during the oxidation/stabilization treatment

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 5

These ammonium salts after heat treatment turn into amides and eventually cause the cross-linking of the PAN fiber by attacking the nitrile groups present in the polymer chain

Methodology Applied
Scientific EffectCross-linking: Chemical Bonding

Data Source

PatentEP3783132B1Process for the preparation of a spinning solution for the production of acrylic fiber precursors of carbon fibers, and the relative carbon fibers
Publication Date: 2026.03.11 MONTEFIBRE MAE TECH SRL

AI summary

An optimized process for the preparation of a spinning solution for the production of acrylic fiber precursors (PAN) of carbon fibers and an optimized process for the production of carbon fibers from said acrylic precursor (PAN), are described.