Raman Spectroscopy for Real-Time 1,4-Butanediol Process Control

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Solution Overview

Problem

Current methods for monitoring reactor feeds and effluents in 1,4-butanediol production, such as gas chromatography, suffer from chemical changes during sample extraction and long analysis times, leading to inefficiencies and potential safety issues.

Innovation Solution

Implementing Raman spectroscopy to monitor feed and effluent streams in real-time, allowing for immediate data processing and adjustment of reaction conditions, thereby enhancing production efficiency and stability.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If gas chromatography is used to monitor reactor feeds and effluents, then analysis can be performed, but long testing times (up to 15 minutes or more) create lag time between system conditions and results

Engineering Contradiction:
Improveanalysis accuracyVSAvoidlag time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The patent replaces the mechanical gas chromatography system with a Raman spectroscopy system that uses light scattering to detect molecular vibrations. This substitution eliminates the need for physical sample extraction and chromatographic separation, enabling real-time monitoring without the 15+ minute lag inherent in GC methods while maintaining measurement accuracy through characteristic Raman spectral fingerprints of different compounds

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

Solution Approach 2:

The patent introduces Raman spectroscopy as an intermediary measurement technique that allows non-contact, in-situ analysis of reactor streams. The Raman probe acts as an intermediary device that can be inserted directly into the reactor to monitor composition changes in real-time, bridging the gap between process conditions and measurement data without requiring sample removal and laboratory analysis

Inventive Principle:
Principle #24Intermediary (Mediator)

2Measurement precision

If physical sample extraction is performed for gas chromatography analysis, then chemical composition can be measured, but chemical changes may occur during extraction and transfer

Engineering Contradiction:
Improvecomposition measurementVSAvoidsample integrity
Core Design Contradiction:
Measurement precisionVSReliability

Solution Approach 1:

The patent replaces the mechanical sample extraction and transfer process with optical Raman spectroscopy measurement. Instead of physically removing and transporting samples through complex extraction systems where contamination and chemical changes can occur, the Raman probe performs in-situ measurement directly in the reactor, eliminating sample integrity issues while maintaining accurate composition measurement

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

Solution Approach 2:

The Raman spectroscopy system performs self-contained measurement within the reactor environment. The probe collects Raman scattering signals directly from the reaction mixture in place, requiring no external sample handling infrastructure. This self-service approach eliminates the extraction and transfer steps that compromise sample integrity in traditional GC methods

Inventive Principle:
Principle #25Self-service

Data Source

PatentEP2920137B1Process control with raman spectroscopy
Publication Date: 2019.12.25 LYONDELL CHEMICAL TECHNOLOGY LP
  • EP2920137B1 patent drawingFigure 1
  • EP2920137B1 patent drawingFigure 2
  • EP2920137B1 patent drawing

AI summary

Embodiments of the present disclosure include methods of effecting process control in a reaction system for the production of 1,4-butanediol, the method including determining at least one property of a sample from the reaction system using Raman spectroscopy, and adjusting at least one parameter of the reaction system in response to the at least one determined property. Embodiments may also include methods of producing 1,4-butanediol, the method including reacting allyl alcohol with carbon monoxide and hydrogen in the presence of a solvent and a catalyst to produce a reactor fluid, sampling the reaction, determining at least one property of the sample using Raman spectroscopy, and adjusting the reaction in response to the at least one determined property.