A Combined NMR Relaxometry and Surface Instability Detection System for Polymer Melt Extrusion

A combined system for solidification and instability detection during the forced extrusion of polymers is constructed and first investigations are presented. The system comprises a home built Halbach-type NMR magnet, monitoring the NMR relaxation at different positions along the extrudate length, and a highly sensitive transducer in the die recording mechanical pressure fluctuations. The system is complemented by an optical extrudate visualization setup. First results are shown for low density and high density polyethylene (LDPE and HDPE), which have different branching structures. Three relevant processing parameters were varied during the investigations, i.e., extruder rotation speed, draw ratio and extrusion temperature. Overall, the characteristics of NMR relaxation show a clear dependence on the magnet position along the extrudate length, which can be related to the cooling, onset and propagation of crystallization, and solidification of the polymer melt. The coupling of a low-field NMR with a high sensitivity instability detection system shows the potential of creating a versatile tool for a unique online control method in polymer processing. In the future, this combination could provide insight into the influence of branching structures on polymer processing of polyethylene, for example.

[1]  M. Dees,et al.  Pressure oscillations and periodic extrudate distortions of long-chain branched polyolefins , 2005 .

[2]  D I Hoult,et al.  The principle of reciprocity. , 2011, Journal of magnetic resonance.

[3]  Andreas Maus,et al.  A Robust Proton NMR Method to Investigate Hard/Soft Ratios, Crystallinity, and Component Mobility in Polymers , 2006 .

[4]  M. Maiwald,et al.  Process and reaction monitoring by low-field NMR spectroscopy. , 2012, Progress in nuclear magnetic resonance spectroscopy.

[5]  M. Wilhelm,et al.  Online Coupling of Size‐Exclusion Chromatography and Low‐Field 1H NMR Spectroscopy , 2012 .

[6]  H. Pasch,et al.  Online coupling of two-dimensional liquid chromatography and NMR for the analysis of complex polymers , 2012 .

[7]  P. Blümler,et al.  Dipolar Halbach magnet stacks made from identically shaped permanent magnets for magnetic resonance , 2010 .

[8]  Hans-Peter Raich,et al.  Design and construction of a dipolar Halbach array with a homogeneous field from identical bar magnets: NMR Mandhalas , 2004 .

[9]  J. Shoolery Nuclear Magnetic Resonance Spectroscopy , 1954 .

[10]  S. Vleeshouwers,et al.  A rheological study of shear induced crystallization , 1996 .

[11]  Dagmar van Dusschoten,et al.  Increased torque transducer sensitivity via oversampling , 2001 .

[12]  B. Hills,et al.  Motional relativity and industrial NMR sensors. , 2006, Journal of magnetic resonance.

[13]  M S Conradi,et al.  Remote tuning of NMR probe circuits. , 2000, Journal of magnetic resonance.

[14]  T. McLeish Tube theory of entangled polymer dynamics , 2002 .

[15]  Morton M. Denn,et al.  Polymer Melt Processing: Foundations in Fluid Mechanics and Heat Transfer , 2008 .

[16]  M. Wilhelm,et al.  Synthesis and Linear and Nonlinear Melt Rheology of Well-Defined Comb Architectures of PS and PpMS with a Low and Controlled Degree of Long-Chain Branching , 2013 .

[17]  U. Scheler,et al.  Extrusion Monitoring of Polymer Melts Using a High‐Temperature Surface‐NMR Probe , 2005 .

[18]  Christoph Clauser,et al.  Improved Halbach sensor for NMR scanning of drill cores. , 2007, Magnetic resonance imaging.

[19]  S. Meiboom,et al.  Modified Spin‐Echo Method for Measuring Nuclear Relaxation Times , 1958 .

[20]  M. Wilhelm,et al.  Correlation between polyethylene topology and melt flow instabilities by determining in-situ pressure fluctuations and applying advanced data analysis , 2010 .

[21]  M. Wilhelm,et al.  In situ Pressure Fluctuations of Polymer Melt Flow Instabilities: Experimental Evidence about their Origin and Dynamics. , 2009, Macromolecular rapid communications.

[22]  H. Münstedt,et al.  Strain hardening of various polyolefins in uniaxial elongational flow , 2003 .

[23]  Morton M. Denn Polymer Melt Processing: Subject Index , 2008 .

[24]  Walter Michaeli,et al.  Determining object boundaries from MR images with sub-pixel resolution: towards in-line inspection with a mobile tomograph. , 2010, Journal of magnetic resonance.

[25]  J. Penning,et al.  Phase Composition and Molecular Mobility in Nylon 6 Fibers as Studied by Proton NMR Transverse Magnetization Relaxation , 2004 .

[26]  E. Purcell,et al.  Effects of Diffusion on Free Precession in Nuclear Magnetic Resonance Experiments , 1954 .