Application of Raman Spectroscopy to Characterization of Residence Time Distribution and Online Monitoring of a Pilot‐Scale Tubular Reactor for Acrylic Acid Solution Polymerization

Chevrel, Marie-Claire; Hoppe, Sandrine; Meimaroglou, Dimitrios; Chapron, D.; Bourson, P.; Wilson, James E.; Ferlin, Patrick; Laurent, Fabrice; Durand, Alain

doi:10.1002/mren.201500055

Cited by 13 publications

(6 citation statements)

References 28 publications

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“…Residence time distribution (RTD) of the reactor was studied in detail with nonreactive and reactive fl uids and with fl uid viscosities between 10 −3 and 1 Pa s. [ 42 ] It was demonstrated that RTD was very similar to that of a perfect plug-fl ow reactor. This assumption was made for all calculations.…”

Section: Mathematical Model Of Polymerization Reactormentioning

confidence: 98%

Continuous Pilot‐Scale Tubular Reactor for Acrylic Acid Polymerization in Solution Designed Using Lab‐Scale Rheo‐Raman data

Chevrel

Hoppe

Meimaroglou

et al. 2016

Macro Reaction Engineering

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A continuous pilot‐scale tubular reactor is designed for the polymerization of acrylic acid in aqueous solution. The reactor is equipped with CSE‐X static mixers from Fluitec which strongly increase heat and mass transfer despite laminar flow. A mathematical model of the reactor is proposed assuming that it is a perfect plug‐flow reactor and using kinetic and rheological equations previously established using a lab‐scale rheo‐Raman device. Calculated values of temperature and polymer concentration profile along the reactor as well as outlet average molar masses and viscosity are in good agreement with experimental results. Provided that the outlet viscosity of reaction medium does not exceed 0.5 Pa s, no reactor fouling occurred. On the contrary, fouling is detected after 6 to 8 h running with higher viscosities. This work is the first demonstration of applicability of CSE‐X static mixer elements in a continuous polymerization process producing high molar mass water‐soluble polymer. In addition, successful scale‐up of polymerization reactor is reported up to pilot‐scale as well as batch to continuous transposition, only on the basis of lab‐scale rheo‐Raman data. The interest of rheo‐Raman device for the acquisition of primary data is established.

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Section: Mathematical Model Of Polymerization Reactormentioning

confidence: 98%

Continuous Pilot‐Scale Tubular Reactor for Acrylic Acid Polymerization in Solution Designed Using Lab‐Scale Rheo‐Raman data

Chevrel

Hoppe

Meimaroglou

et al. 2016

Macro Reaction Engineering

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“…Moreover, this type of spectroscopies, like Fourier transformed infrared (FTIR) or Raman, can be of great interest to monitor in situ structural modifications with potential applications for implementation in real-time industrial diagnosis. 16,24,25 In this article, by means of FTIR and GIWAXS, we have accomplished a detailed description of the in situ isothermal crystallization of poly(trimethylene 2,5-furandicarboxylate) (PTF) in real time. From FTIR experiments, the evolution of hydrogen bonding with crystallization time can be monitored.…”

Section: Introductionmentioning

confidence: 99%

“…Vibrational spectroscopy is a powerful tool to identify at molecular-level conformations characteristic of amorphous and crystalline phases in polymers. Moreover, this type of spectroscopies, like Fourier transformed infrared (FTIR) or Raman, can be of great interest to monitor in situ structural modifications with potential applications for implementation in real-time industrial diagnosis. ,, …”

Section: Introductionmentioning

confidence: 99%

Study of the Crystal Structure and Hydrogen Bonding during Cold Crystallization of Poly(trimethylene 2,5-furandicarboxylate)

Toledano,

Gálvez,

Sanz

et al. 2024

Macromolecules

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Here, we present a detailed description of the in situ isothermal crystallization of poly(trimethylene 2,5-furandicarboxylate)(PTF) as revealed by realtime Fourier transform infrared spectroscopy (FTIR) and grazing incidence wideangle X-ray scattering (GIWAXS). From FTIR experiments, the evolution of hydrogen bonding with crystallization time can be monitored in real time, while from GIWAXS, crystal formation can be followed. Density functional theory (DFT) calculations have been used to simulate FTIR spectra for different theoretical structures, enabling a precise band assignment. In addition, based on DFT ab initio calculations, the influence of hydrogen bonding on the evolution with crystallization time can be understood. Moreover, from DFT calculations and comparison with both FTIR and GIWAXS experiments, a crystalline structure of poly(trimethylene 2,5furandicarboxylate) is proposed. Our results demonstrate that hydrogen bonding is present in both the crystalline and the amorphous phases and its rearrangement can be considered as a significant driving force for crystallization of poly(alkylene 2,5-furanoate)s.

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“…However, the technical requirements for conducting the widely used Fourier-transform infrared spectroscopy (FTIR) hamper the combination with other techniques and specific complex sample environments have to be designed to be coupled for each experiment requirement. By contrast, Raman spectroscopy has been widely used in combination with multiple techniques, in particular for polymer characterization in the industrial field [ 34 , 35 ] such as monitoring of in situ polymerization by Raman spectroscopy [ 36 , 37 , 38 ] as well as rheo-Raman [ 39 ] and Raman-DSC [ 40 ], due to its simple implementation, improvement of the time resolution and experimental advantages [ 41 ]. Furthermore, Raman spectroscopy is a non-destructive technique that can be applied to different media (bulk, fibres, solution, gels and films), specifically aqueous solution without special experimental preparations, and requires small quantities of sample to be studied [ 41 , 42 ].…”

Section: Introductionmentioning

confidence: 99%

Data Mining of Polymer Phase Transitions upon Temperature Changes by Small and Wide-Angle X-ray Scattering Combined with Raman Spectroscopy

et al. 2021

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The complex physical transformations of polymers upon external thermodynamic changes are related to the molecular length of the polymer and its associated multifaceted energetic balance. The understanding of subtle transitions or multistep phase transformation requires real-time phenomenological studies using a multi-technique approach that covers several length-scales and chemical states. A combination of X-ray scattering techniques with Raman spectroscopy and Differential Scanning Calorimetry was conducted to correlate the structural changes from the conformational chain to the polymer crystal and mesoscale organization. Current research applications and the experimental combination of Raman spectroscopy with simultaneous SAXS/WAXS measurements coupled to a DSC is discussed. In particular, we show that in order to obtain the maximum benefit from simultaneously obtained high-quality data sets from different techniques, one should look beyond traditional analysis techniques and instead apply multivariate analysis. Data mining strategies can be applied to develop methods to control polymer processing in an industrial context. Crystallization studies of a PVDF blend with a fluoroelastomer, known to feature complex phase transitions, were used to validate the combined approach and further analyzed by MVA.

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Application of Raman Spectroscopy to Characterization of Residence Time Distribution and Online Monitoring of a Pilot‐Scale Tubular Reactor for Acrylic Acid Solution Polymerization

Cited by 13 publications

References 28 publications

Continuous Pilot‐Scale Tubular Reactor for Acrylic Acid Polymerization in Solution Designed Using Lab‐Scale Rheo‐Raman data

Continuous Pilot‐Scale Tubular Reactor for Acrylic Acid Polymerization in Solution Designed Using Lab‐Scale Rheo‐Raman data

Study of the Crystal Structure and Hydrogen Bonding during Cold Crystallization of Poly(trimethylene 2,5-furandicarboxylate)

Data Mining of Polymer Phase Transitions upon Temperature Changes by Small and Wide-Angle X-ray Scattering Combined with Raman Spectroscopy

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