Extrusion of pastes with a piston extruder for the determination of the local solid and fluid concentration, the local porosity and saturation and displacement profiles by means of NMR imaging

 Nuclear Magnetic Resonance (NMR) was used to investigate the extrusion behaviour of PTFE pastes in a ram extruder. By means of ¹H-NMR imaging (MRI) it is possible to determine the local proton density and therefore, the local fluid concentration. The ¹⁹F-MRI provides the local solid concentration. Thus the local saturation and the local porosity can be calculated with the information of the local fluid and solid concentration. Furthermore displacement profiles can be derived from NMR images by means of correlation techniques without any preparation or marking of the pastes. Received: 8 May 2000   Accepted: 1 May 2001     

Continuous peeling extrusion of SEBS block copolymers

During continuous peeling, a central polymer rod free of visible defects was continuously extruded while being peeled at the die exit. Continuous peeling can occur at flow rates orders of magnitude higher than those at which initial surface cracking is observed. Thus, if continuous peeling can be controlled it may have potential industrial applications. The aim of this work was to study how different extrusion parameters (temperature, flow rate, die length and diameter) affect the presence of continuous peeling. The melt exiting the die has been filmed to link physical measurements and observations and to determine whether or not continuous peeling is present. Different criteria have been considered to represent the extrusion conditions under which continuous peeling may occur. Surface tension criteria can be used to try to predict the appearance and disappearance of continuous peeling. A correlation formula is also proposed for the rod diameter in terms of surface tension. Our results show that the ratio of the rod diameter to the die diameter is approximately 25% greater in the case of short-orifice dies (L/D ≈ 0) than for long capillaries (L/D ≈ 10). The correlations obtained allow analysis and discussion of flow regimes for possible applications.     

Das Düsenschwellphänomen beim Austritt einer wandhaftenden anorganischen Glasschmelze aus Strangpreßwerkzeugen mit nichtkreisförmigem Öffnungsquerschnitt

Zusammenfassung Eine ausgeprägte Strangaufweitung tritt bei anorganischen Glasschmelzen dann auf, wenn bei schleichender Strömung eine Haftung zwischen der Wand des Matrizenkanals und dem strömenden Medium gegeben ist. Sie rührt dabei von der Umorientierung der Geschwindigkeitsverteilung von einem parabelförmigen zu einem kastenförmigen Profil her.In den experimentellen Untersuchungen konnte festgestellt werden, daß oberhalb einer bestimmten Kanallänge, d. h. bei ausgeprägten Strömungsverhältnissen im Preßwerkzeug die flächenbezogene Strangaufweitung konstant und dabei insbesondere unabhängig von der Profilform etwa 29% beträgt. Daraus wird gefolgert, daß dieser Betrag dem linearen Wert für den zweidimensionalen Fall des unendlich ausgedehnten Spaltes entsprechen muß.In einer theoretischen Analyse wurde die Berechnung dieses Falles ausgehend von der Stokes-Gleichung mit Hilfe der Methode der finiten Elemente durchgeführt. Aus der sich daraus ergebenden Druck- und Geschwindigkeitsverteilung konnte schließlich die Kontur des austretenden Stranges sowie dessen Endhöhe ermittelt werden.Ein Vergleich der experimentell und rechnerisch ermittelten Werte für die Strangaufweitung zeigt dabei eine recht gute Übereinstimmung und bestätigt dadurch auch die weitgehende Unabhängigkeit der flächenbezogenen Aufweitung von der Querschnittsform des Stranges.

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Inorganic glass melts are showing a characteristic die swell, when in the case of slow motion a strong adhesion between the streaming fluid and the wall of the die channel exists. The reason for this phenomenon is the rearrangement of the velocity profile from a parabolic to a box-type design form.The experimental investigations have demonstrated, that above a certain channel length, this means at distinct flow conditions inside the die channel, the value for the extension of the cross-sectional area is constant of about 29%. Particularly it is independent of the shape of the used die profiles. From this result, it is to deduce that this value must correspond to that of the two-dimensional case of the infinite extended slit.In a theoretical analysis the computation of this case was performed, starting from the Stokes-equation by the finite element method. By means of the resulting pressure and velocity distribution, the contour of the emerging rod and its final thickness could be determined.A comparison between experimental and computational results shows good agreement. So the appreciable independence of the magnitude of the die swell from the profile of the extruded rod is confirmed.

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A Fläche - a ^p ,a ^u Knotenpunktsvariablen für Druck bzw. Geschwindigkeit - a, b Seitenlängen des Rechteckprofils - B =L · N ^u Matrix - D Viskositätsmatrix - f Kräftematrix - K Schwerkraftvektor - K ^p ,K ^u Elementdruckmatrix, Elementgeschwindigkeitsmatrix - L Transformationsmatrix für den ebenen Fall - m Kronecker-Symbol für den zweidimensionalen Strömungszustand - N ^p ,N ^u Ansatzfunktionsmatrizen für Druck bzw. Geschwindigkeit - p Preßdruck - R Radius - T Preßtemperatur - t Lastvektor - u = (w, v) Geschwindigkeitsvektor - _A flächenbezogene Strangaufweitung - _R Aufweitung einer linearen QuerschnittsabmessungR - dynamische Viskosität - Dichte - D u/Dt Substantielle Ableitung der Geschwindigkeit nach der Zeit - T Transponierte einer Matrix (oberer Index) Vorgetragen auf der Jahrestagung der Deutschen Rheologischen Gesellschaft in Berlin vom 13.–15. Mai 1985     

Planar and tubular perovskite-type membrane reactors for the partial oxidation of methane to syngas

Dense planar and tubular oxygen separation membranes of La_0.6Ca_0.4Fe_0.75Co_0.25O_3– were investigated as reactors for the partial oxidation (POX) of methane to syngas. Their permeation properties were measured in an air/argon pO₂ gradient as a function of temperature. At 900 °C, the oxygen flux through a 1.26-mm-thick membrane was 0.075 mol/cm²·s and through a 0.25-mm-thick tube, 0.24 mol/cm²·s.For the POX measurements, a catalyst was added to the membrane and methane was introduced on the argon side. This resulted in a gradual increase of the oxygen flux with increasing concentration of methane, reaching 2 mol/cm²·s at 900 °C with pure methane. For the planar reactor, the CO selectivity reached 99% and the CH₄ conversion 75% at 918 °C with pure methane. For the tubular reactor, the CO selectivity and CH₄ conversion were 83 and 99%, respectively, under the same conditions. After 1,400 h of operation in a tubular POX reactor, the membrane was examined revealing phase demixing and local decomposition.Presented at the OSSEP Workshop Ionic and Mixed Conductors: Methods and Processes, Aveiro, Portugal, 10–12 April 2003     

The melt elastic behavior of polypropylene/glass bead composites in capillary flow

The melt extrudate swell and entry pressure losses are important characteristics of elastic properties during die extrusion of polymeric fluids. They are usually expressed with die-swell ratio (B) and entry pressure drop (ΔP_o). In the present paper, the die-swell behavior and entrance pressure drop of a polypropylene (PP) filled with A-glass beads were investigated by using a Rosand capillary rheometer to identify the effects of the filler contents and extrusion rate on the elastic behavior of the sample melts. The experiments were carried out under the conditions with an apparent shear rate range of 50–10⁴ s⁻¹ and a temperature of 190 °C. The results showed that B increased nonlinearly with increasing shear rate at the wall (γ_w), and increased linearly with the increase of shear stress at the wall (τ_w). With the increase of the volume fraction of the fillers B decreased nonlinearly. Similarly, the entry pressure drop increased linearly with the increase of τ_w, whereas the influence of the filler concentration on ΔP_o was insignificant in this case. Furthermore, B increased as a linear function of ΔP_o, and extension stress (σ_e) increased nonlinearly with increasing γ_w.     

Fused Deposition Modelling of high temperature polymers: Exploring CNT PEEK composites

The Fused Deposition Modelling (FDM™) process owes its popularity to its hardware versatility, low cost and wide range of materials (and colours) available. In this study, PEEK was produced with 1% and 5% carbon nanotubes (CNTs) and processed in a modified FDM system able to operate with high temperature polymers. The tensile strength, layer bonding and microstructure of the plain and CNT loaded PEEK samples were investigated throughout the three steps of manufacturing: compounded composite feedstock filaments, single FDM deposited layers and fabricated test specimens. Interestingly, every step of processing seems to fabricate structures of lower performance. As part of the characterisation of the FDM structures, short shear beam tests were used as a new method to assess layer-to-layer bonding.     

New low-cost tubular ceramic microfiltration membrane based on natural sand for tangential urban wastewater treatment

In wastewater treatment, the development of low-cost separation methods is of significant importance. Low-cost membranes based on natural materials have become a highly active research topic in recent years. Herein, using low-cost natural Moroccan sand, new ceramic supports have been developed and characterized using different techniques such as X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), differential thermal analysis (DTA), along with scanning electron microscope (SEM). Plastic paste (average particle size ≤125 µm) was blended with organic additives and water, then the obtained paste was extruded into porous tubular supports. The support had a porosity of 43%, water permeability of 1928 L/h m² bar, excellent chemical and mechanical properties and an average pore diameter in the range of 8–15 µm after firing at 950 °C/2 h. As per SEM analysis, the tubular supports had a smooth and crack-free surface. The slip casting process was used to create a microfiltration layer from the same natural sand powder (average particle size ≤63 µm) using a mixture of powder sand, water, and polyvinyl alcohol solution. The water permeability of the microfiltration membrane sintered at 950 °C/2 h was 1052 L/h m² bar, the average pore size diameter was about 0.90 µm and 82% of pores had a diameter ≤1.00 µm. The obtained microfiltration membrane was tested for the treatment of urban wastewater. The membrane showed excellent separation performance in turbidity removal and chemical oxygen demand.     

Stick-slip flow of high density polyethylene in a transparent slit die investigated by laser Doppler velocimetry

The oscillating flow instability of a molten linear high-density polyethylene is carefully studied using a single screw extruder equipped with a transparent slit die. Experiments are performed using laser Doppler velocimetry in order to obtain the local velocities field across the entire die width. At low flow rate, the extrusion is stable and steady state velocity profiles are obtained. During the instability, the velocity oscillates between two steady state limits, suggesting a periodic stick-slip transition mechanism. At high flow rate, the flow is mainly characterized by a pronounced wall slip. We show that wall slip occurs all along the die land. An investigation of the slip flow conditions shows that wall slip is not homogeneous in a cross section of the slit die, and that pure plug flow occurs only for very high flow rates. A numerical computation of the profile assuming wall slip boundary conditions is done to obtain the true local wall slip velocity. It confirms that slip velocities are of the same order of magnitude as those measured with a capillary rheometer.     

In-line monitoring flow in an extruder die by rheo-optics

A new modular slit die with optical windows in two different positions and three pressure transducers flush-mounted along the wall was built and coupled to the exit of a twin-screw extruder. Thus, the birefringence and the pressure drop of polystyrene were monitored inline during extrusion. Two experimental procedures were tested: steady-state and cessation of extruder feeding. The latter proved to be very useful in the case of polystyrene since the ratio between the birefringence and the pressure drop can be quantified for a wide range of steady-state conditions with a single experiment. In fact, down to relatively lower values of pressure drop, the birefringence proved to be a function of shear stress at the wall only, depending neither on the initial feeding rate nor on the aspect ratio of the slit die, for W/h down to 5, at least.     

A new device for in-line colorimetric quantification of polypropylene degradation under multiple extrusions

An in-line colorimeter that is able to quantify color changes in real time during extrusion was developed and validated. It is composed of LEDs emitting at three different wavelengths and a photocell that measures the intensity of the light transmitted through the polymer melt flow. The colorimeter was validated at the bench by employing colored aqueous solutions and in-line during the extrusion of a colored polypropylene. Furthermore, it was used to in-line quantify the color changes in a polypropylene as generated over multiple extrusions due to thermo-mechanical degradation. The technique was proved to be fast and suitable to measure color changes in real time during extrusion.