FT-NIR Spectroscopy for Real-Time Polymer Particle Size Monitoring

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Solution Overview

Problem

Current methods for determining and controlling polymer properties in gas phase reactors, such as particle size and distribution, are slow and inefficient due to reliance on offline sampling and laboratory analysis, leading to production of 'off-spec' polymers and delayed adjustments in polymerization conditions.

Innovation Solution

The use of Fourier Transform Near-Infrared (FT-NIR) spectrophotometry for real-time, on-line measurement of polymer particle size and distribution, combined with regression models based on principal component analysis, allows for continuous monitoring and control of polymer properties in fluidized-bed reactors.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If offline sampling and laboratory analysis are used to determine polymer properties, then measurement precision can be achieved, but measurement time and productivity are severely reduced

Engineering Contradiction:
Improvepolymer property measurement accuracyVSAvoidproduction rate
Core Design Contradiction:
Measurement precisionVSProductivity

Solution Approach 1:

The patent replaces mechanical sampling and laboratory analysis systems with an optical measurement system. FT-NIR probes are inserted directly into the reactor to measure polymer properties optically, eliminating the need for physical sampling, transport, and manual laboratory analysis, thereby achieving both accuracy and real-time measurement

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

Solution Approach 2:

The patent introduces FT-NIR optical probes as intermediary measurement devices that can directly sense polymer properties within the reactor environment. These probes act as mediators between the polymerization process and the measurement system, enabling non-invasive, real-time monitoring without disrupting the process

Inventive Principle:
Principle #24Intermediary (Mediator)

2Measurement precision

If offline sampling methods are used, then measurement precision is maintained, but loss of time increases significantly

Engineering Contradiction:
Improvepolymer property measurement accuracyVSAvoidmeasurement time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The patent implements continuous measurement through FT-NIR probes that operate throughout the polymerization process without interruption. The system provides ongoing real-time data on polymer properties, eliminating the discontinuous nature of sampling and laboratory analysis, thereby reducing time loss while maintaining precision

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent substitutes the time-consuming mechanical sampling and laboratory analysis process with rapid optical measurement. FT-NIR spectroscopy provides instant results by directly analyzing polymer properties through light interaction, reducing measurement time from hours to seconds while preserving accuracy

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

3Device complexity

If reliance on manual sampling and analysis is maintained, then device complexity remains low, but manufacturing precision deteriorates due to delayed adjustments

Engineering Contradiction:
Improvemeasurement system complexityVSAvoidpolymer specification compliance
Core Design Contradiction:
Device complexityVSManufacturing precision

Solution Approach 1:

The patent implements a feedback control system where FT-NIR measurements of polymer properties are continuously monitored and fed back to the control system. This enables real-time detection of deviations from specification and automatic adjustment of polymerization parameters, significantly improving manufacturing precision despite increased system complexity

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The patent employs multi-functional FT-NIR probes that can measure multiple polymer properties (particle size, composition, morphology) simultaneously with a single device. This universal measurement capability improves manufacturing precision across multiple parameters while managing system complexity through integration rather than multiple separate systems

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

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 rapid, in-situ determination and control of polymer properties, reducing the production of 'off-spec' polymers and improving process efficiency by providing real-time data for adjusting reactor parameters.

Implementation Method 1

Fourier Transform Near-Infrared (FT-NIR) spectrophotometry

Methodology Applied
Scientific EffectNear-infrared radiation absorption: Absorption (EM radiation)

Implementation Method 2

measuring the average particle size and particle size distribution

Methodology Applied
Scientific EffectLight scattering: Scattering

Data Source

PatentUS9389161B2On-line FT-NIR method to determine particle size and distribution
Publication Date: 2016.07.12 EXXONMOBIL CHEMICAL PATENTS INC
  • US9389161B2 patent drawing
  • US9389161B2 patent drawing
  • US9389161B2 patent drawing

AI summary

This invention relates to a method for the determination of the average particle size or particle size distribution of a material in a gas phase reactor comprising: 1) analyzing the average particle size and particle size distribution of a baseline composition using the method described in ASTM D1921; 2) analyzing the average particle size and particle size distribution of said baseline composition using an FT-NIR analysis technique; 3) preparing a calibration matrix by comparing results from said reference analytical technique to the results from said FT-NIR analysis technique; 4) analyzing the material using an FT-NIR technique; and 5) identifying and quantifying the type and content of particles present in the material by comparing spectral data obtained from said FT-NIR technique of the material to said calibration matrix.This invention also relates to a process for determining polymer properties in a polymerization reactor system using such techniques.