Automatic, simultaneous control of polymer composition and molecular weight during free radical copolymer synthesis

McAfee, Terry; Montgomery, Rick; Zekoski, Thomas; Wu, Aide; Reed, Wayne F.

doi:10.1016/j.polymer.2017.12.005

Cited by 9 publications

(13 citation statements)

References 38 publications

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“…This is seen most clearly in Figure 4 , which shows the concentration of each monomer in the reactor versus time. The Ac dramatically slows the reaction compared to copolymer reactions of just Am and SS . Under similar reaction conditions these latter took 3 to 5 h, not the 27 obtained here .…”

Section: Resultssupporting

confidence: 52%

“…The Ac dramatically slows the reaction compared to copolymer reactions of just Am and SS . Under similar reaction conditions these latter took 3 to 5 h, not the 27 obtained here . No attempts were made in this work to speed the reaction up.…”

Section: Resultsmentioning

confidence: 61%

“…The means of connecting the flow rates of pumps feeding the reactor from separate comonomer reservoirs, using Equation , has been detailed in ref. .…”

Section: Methodsmentioning

confidence: 99%

“…Recently, this group achieved automatic control of molecular weight in free radical polymerization, automatic production of multi‐modal molecular weight distributions, and then simultaneous control of molecular weight and composition for free radical copolymerization . The latter was achieved for acrylamide (Am) and styrene sulfonate (SS) via continuous monitoring of their individual concentrations using an online UV spectrometer.…”

Section: Introductionmentioning

confidence: 99%

“…The controllers developed in refs. were essentially model‐free and involved only two constantly measurable proportionality constants for homopolymerizaton control and three constantly measurable proportionality constants for copolymerization control. Aside from these, a formal, model‐based nonlinear controller for homopolyerization molecular weight was also developed and demonstrated …”

Section: Introductionmentioning

confidence: 99%

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Coupling of NMR to ACOMP for Terpolymerization Monitoring and Control

McAfee

Jarand

Zekoski

et al. 2019

Macro Reaction Engineering

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Monitoring and control of free radical copolymerization using automatic continuous online monitoring of polymerization reactions (ACOMP) with UV detection has been recently achieved. It is difficult, however, to achieve spectral separation of similar monomers with UV alone. Here, nuclear magnetic resonance (NMR) is coupled to ACOMP for the first time and terpolymerization reactions involving acrylamide (Am), sodium acrylate (Ac), and styrene sulfonate (SS) are monitored, and a first attempt at active composition control is made. The NMR resolves the concentrations of Am and Ac, while the UV resolves SS and the sum of Am and Ac. NMR analysis is performed in water, using signal suppression, to eliminate the need for deuterated solvents. From this, instantaneous fractions of each comonomer in the terpolymer are continuously known, along with weight average molecular weight and intrinsic viscosity, IV. Am and Ac have similar reactivities, whereas the reactivity ratio of SS is much larger. Hence, there is high composition drift in batch polymerization and SS is rapidly consumed, leaving a final copolymer of Am and SS to form. Maintaining constant terpolymer composition is taken as a first step toward active control.

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Section: Resultssupporting

confidence: 52%

Section: Resultsmentioning

confidence: 61%

“…The means of connecting the flow rates of pumps feeding the reactor from separate comonomer reservoirs, using Equation , has been detailed in ref. .…”

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Coupling of NMR to ACOMP for Terpolymerization Monitoring and Control

McAfee

Jarand

Zekoski

et al. 2019

Macro Reaction Engineering

Self Cite

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Automatic Continuous Online Monitoring and Control of Polymerization Reactions and Related Methods

Reed

2019

Encyclopedia of Analytical Chemistry

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Automatic continuous online monitoring and control of polymerization (ACOMP) is a widely applicable platform for monitoring and controlling polymerization reactions. It relies on the continuous extraction, dilution, and conditioning of a small sample stream from the reactor on which measurements by various combinations of detectors are made. By combining simultaneous data from multiple detectors continuous monitoring of salient reaction characteristics can be made, such as kinetics, conversion of comonomers, composition drift, evolution of molecular mass and intrinsic viscosity, and detection of unusual phenomena, such as microgelation and runaway reactions. A growing area for ACOMP is its integration into predictive and closed‐loop reaction control with intriguing possibilities for enhancement by machine learning and artificial intelligence. Typical detectors include light scattering (LS), ultraviolet (UV)/visible spectrophotometry, viscometry, refractivity, and polarimetry, while NMR, dynamic light scattering (DLS), Mie scattering, conductivity, and near infrared (IR) and Fourier‐transform infrared (FTIR) are also used. Recent additions to ACOMP include the ability to use multiple similar sensors to detect the onset and evolution of polymer stimuli responsive behavior during synthesis; for example copolymer compositions at which a lower critical solution temperature (LCST) occurs. ACOMP has been applied to free radical, controlled free radical, and condensation reactions, to micellar, emulsion, and inverse emulsion polymerization, to post‐polymerization and derivatization reactions, and to batch, semi‐batch, and continuous reactors. While ACOMP is not inherently a chromatographic method, its continuous stream can be used in automatic conjunction with gel permeation and other separation chromatographies. Recently, ACOMP has been deployed in full‐scale industrial polymerization reactors to optimize efficiency and product quality.

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Future manufacturing and remanufacturing of polymeric materials

Schork

2019

J Adv Manuf & Process

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This paper will attempt to describe the future of manufacturing technology in polymeric products. While a wide range of literature references are cited to illustrate the technologies discussed, it is not meant to be a literature review of such a wide field, but rather as an educated guess about where polymer manufacturing (and remanufacturing) will evolve in the foreseeable future. K E Y W O R D Sdepolymerization, polymerization, polymer recycle, polymer remanufacture, pyrolysis, recycle

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Automatic, simultaneous control of polymer composition and molecular weight during free radical copolymer synthesis

Cited by 9 publications

References 38 publications

Coupling of NMR to ACOMP for Terpolymerization Monitoring and Control

Coupling of NMR to ACOMP for Terpolymerization Monitoring and Control

Automatic Continuous Online Monitoring and Control of Polymerization Reactions and Related Methods

Future manufacturing and remanufacturing of polymeric materials

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