Aramid Yarn Neutralization via Multi-Stage Heating

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Solution Overview

Problem

Copolymers derived from 5(6)-amino-2-(p-aminophenyl)benzimidazole and para-phenylenediamine and terephthaloyl dichloride fibers retain sulfuric acid, making them difficult to neutralize effectively, which affects their long-term hydrolytic stability and increases manufacturing costs.

Innovation Solution

A method involving spinning the copolymer from an inorganic acid solvent, followed by washing with a basic aqueous solution for at least 5 seconds and heating in multiple steps, specifically at temperatures ranging from 200°C to 500°C, to achieve effective neutralization and enhance hydrolytic stability.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Strength

If copolymer fibers are spun from sulfuric acid solutions, then fiber strength and processability are improved, but sulfuric acid retention increases making neutralization difficult

Engineering Contradiction:
Improvefiber strengthVSAvoidsulfuric acid retention
Core Design Contradiction:
StrengthVSObject-generated harmful factors

Solution Approach 1:

The neutralization process is divided into multiple sequential stages: initial neutralization with basic aqueous solution, followed by extended washing with water, then a second neutralization stage with additional base, and finally prolonged water washing. This segmented approach allows progressive removal of sulfuric acid without compromising fiber strength.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The patent applies preliminary neutralization treatment during the washing process by introducing basic aqueous solutions before final drying. This preliminary action prevents sulfuric acid from causing hydrolytic degradation during subsequent processing and storage, addressing the neutralization difficulty before it becomes a critical problem.

Inventive Principle:
Principle #10Preliminary action

2Productivity

If copolymer fibers are not sufficiently neutralized, then processing time and cost are reduced, but long-term hydrolytic stability deteriorates

Engineering Contradiction:
Improveprocessing efficiencyVSAvoidhydrolytic stability
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

Basic aqueous solutions (neutralizing agents) serve as intermediaries between the sulfuric acid-containing fiber and the final product. These intermediaries facilitate the removal of harmful sulfuric acid through controlled chemical neutralization reactions, ensuring hydrolytic stability without requiring excessive processing time.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent implements continuous multi-stage washing and neutralization processes where basic solutions and water continuously act on the fiber to remove sulfuric acid. This continuous useful action ensures complete neutralization and maintains hydrolytic stability throughout the production process.

Inventive Principle:
Principle #20Continuity of useful action

3Device complexity

If traditional neutralization techniques are used for copolymer fibers, then process simplicity is maintained, but neutralization effectiveness is insufficient

Engineering Contradiction:
Improveprocess complexityVSAvoidneutralization effectiveness
Core Design Contradiction:
Device complexityVSManufacturing precision

Solution Approach 1:

The patent changes multiple process parameters including washing temperature, basic solution concentration, washing duration, and sequential treatment stages. These parameter changes transform the neutralization process from ineffective to highly effective, achieving thorough sulfuric acid removal while maintaining reasonable process complexity.

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 process results in high-tenacity aramid yarns with greater than 60% hydrolytic strength retention and improved economic viability by reducing sulfuric acid retention, leading to superior long-term physical properties.

Implementation Method 1

washing the yarn with a basic aqueous solution for at least 5 seconds

Methodology Applied
Scientific EffectNeutralization reaction: Chemical Bonding

Implementation Method 2

heating the yarn; wherein the yarn is heated in at least two process steps, characterized in that (i) in a first step the yarn is heated at a temperature of 200 to 360° C. at a tension of at least 0.2 cN/dtex, followed by (ii) a second step wherein the yarn is heated at a temperature of 370 to 500° C. at a tension of less than 1 cN/dtex

Methodology Applied
Scientific EffectThermal treatment: Heating

Data Source

PatentUS9790622B2Copolymer fibers and yarns and processes for making same
Publication Date: 2017.10.17 DUPONT SAFETY & CONSTRUCTION INC
  • US9790622B2 patent drawing
  • US9790622B2 patent drawing
  • US9790622B2 patent drawing

AI summary

The present invention concerns methods for obtaining high-tenacity aramid yarn, wherein the yarn is made of a copolymer obtained from a mixture of monomers comprising 5-(6)-amino-2-(p-aminophenyl)benzimidazole, an aromatic para-diamine, and an aromatic para-diacid; the method comprising: a) spinning said copolymer from an inorganic acid solvent to produce the aramid yarn; b) washing said yarn with a basic aqueous solution for at least 5 seconds; and c) heating said yarn; wherein the yarn is heated in at least two process steps, characterized in that (i) in a first step the yarn is heated at a temperature of 200 to 360° C. at a tension of at least 0.2 cN/dtex, followed by (ii) a second step wherein the yarn is heated at a temperature of 370 to 500° C. at a tension of less than 1 cN/dtex. In some embodiments, the yarn has an effective polymer cation to sulfur content molar ratio of at least 0.3. In some embodiments, the yarn has a hydrolytic strength retention of the yarn is greater than 60%.