Gel Detection in Solution Polymerization via Spectral Analysis

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Solution Overview

Problem

Current methods for detecting gel particles in solution polymerization processes are not suitable for real-time, in-line monitoring, leading to difficulties in identifying optical imperfections in films, such as 'fish eyes', as they are typically offline and time-consuming, or do not effectively measure gel flurries.

Innovation Solution

The use of infrared, near-infrared, or Raman spectrometers to monitor the spectrum of the reactant and solvent stream at various locations in the polymerization process, applying mathematical methods to extract noise features and quantify gel presence, allowing for real-time detection of gel flurries.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If laser light scattering measurements are used to detect particles in polymer, then particle size distribution can be determined, but the measurement cannot be performed in real-time during polymerization

Engineering Contradiction:
Improveparticle size distribution measurementVSAvoidmeasurement time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The patent replaces the mechanical/optical scattering measurement system with a spectroscopic measurement system (FTIR, FTNIR, or Raman). Instead of using laser light scattering that requires offline sampling and dilution, the invention uses infrared or Raman spectroscopy to detect gel flurries through their characteristic absorption or scattering signatures in the reactant stream, enabling real-time monitoring without mechanical intervention.

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

Solution Approach 2:

The patent introduces spectral analysis as an intermediary measurement approach. Rather than directly measuring particle size through scattering, the system uses spectroscopic signals (infrared or Raman) that interact with the gel flurries in the polymerization stream. The spectral data serves as an intermediary indicator that correlates with gel presence, allowing indirect but real-time detection.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Measurement precision

If gel detection is performed offline using particle size determination equipment, then accurate particle characterization is achieved, but the detection is not suitable for in-line real-time measurement

Engineering Contradiction:
Improveparticle characterization accuracyVSAvoidin-line measurement capability
Core Design Contradiction:
Measurement precisionVSEase of operation

Solution Approach 1:

The patent makes the spectroscopic measurement system universal by designing it to handle multiple functions: it can monitor the polymerization process, detect gel flurries, and provide real-time feedback for process control. The same FTIR, FTNIR, or Raman spectrometer that can characterize chemical composition now also detects gel particles, eliminating the need for separate specialized equipment and enabling in-line operation.

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

Solution Approach 2:

The invention replaces the complex mechanical sampling and measurement system with a non-intrusive spectroscopic probe that can be positioned directly in the polymerization stream. This substitution eliminates the need for offline sampling, dilution, and manual measurement steps, making the system suitable for in-line real-time operation while maintaining detection accuracy.

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

3Quantity of substance

If standard spectroscopic methods are used to monitor polymerization, then monomer and co monomer concentration can be measured, but gel flurries cannot be detected

Engineering Contradiction:
Improvemonomer concentration measurementVSAvoidgel flurry detection
Core Design Contradiction:
Quantity of substanceVSDifficulty of detecting and measuring

Solution Approach 1:

The patent changes the measurement parameters by analyzing different regions of the spectral data. Instead of focusing only on the standard monomer/co-monomer absorption peaks, the system examines additional spectral regions and patterns that are sensitive to gel flurry presence. By changing which spectral parameters are monitored and how they are processed, the system can detect both chemical composition and gel particles using the same spectrometer.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention applies local quality analysis by examining specific regions within the spectral data that are characteristic of gel flurries. Rather than treating the spectrum as a uniform signal, the system identifies and analyzes local spectral features (specific wavenumber regions, peak shapes, or patterns) that indicate gel presence, while other regions continue to provide monomer concentration information.

Inventive Principle:
Principle #3Local quality

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

Enables in-line, real-time detection of gel content, reducing the occurrence of optical imperfections in films by identifying gel flurries promptly, thereby improving the quality of the polymerization process.

Implementation Method 1

Fourier transform infrared spectroscopy (FTIR)

Methodology Applied
Scientific EffectAbsorption Spectroscopy: Absorption Spectroscopy

Implementation Method 2

laser light scattering measurements

Methodology Applied
Scientific EffectLight Scattering: Scattering

Data Source

PatentUS7566571B2Detection of gels in a solution polymerization
Publication Date: 2009.07.28 NOVA CHEM (INT) SA
  • US7566571B2 patent drawing
  • US7566571B2 patent drawing

AI summary

In a solution polymerization process the increase in gel content in the solution at one or more locations may be detected by monitoring the structure of a spectrum obtained by analyzing the reaction at said one or more locations using a spectrometer selected from the group consisting of infrared spectrometers, near infrared spectrometers and Raman spectrometers.