Continuous polymerization of ω‐lauryl lactam in an intermeshing corotating twin‐screw extruder

This article describes the synthesis of poly(ω‐lauryl lactam) by a reactive extrusion process. Anionic ring‐opening polymerization was performed in an intermeshing corotating twin‐screw extruder. We investigated the evolution of conversion of ω‐lauryl lactam as a function of reaction time, screw speeds, different feed rates, and different screw configurations along the screw axis in a twin‐screw extruder. For comparison with continuous polymerization in a twin‐screw extruder, we studied polymerization in an internal mixer, which was considered a batch reactor. We found the final conversion of ω‐lauryl lactam made in a twin‐screw extruder was higher than in an internal mixer. Higher molecular weights are found at lower screw speeds and feed rates. Melt viscosities and mechanical properties of the polymers were measured. Residence time, molecular weights, and shear mixing have the main effect on the mechanical properties of products. The twin‐screw extruder performance was interpreted in terms of commercial software. It was found that twin‐screw extruder reaction rate was higher than those in the batch reactor and increased locally with screw speed and feed rate. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 1605–1620, 2005     

Solvent‐free polymer emulsification inside a twin‐screw extruder

Solvent‐free extrusion emulsification (SFEE) is new technique for a twin‐screw extruder to prepare submicron‐sized particles (100–500 nm) without using hazardous solvents. The particle size is reliant upon the thickness of striated lamellae, which can be monitored rheologically based on the viscosity change occurring at the SFEE process. The lamellae coarsening rate is predominantly affected by the interfacial energy of the system when a surfactant is added but shows stronger dependency on viscosity change when interfacial growth between the polymer and water phases is solely determined by the end‐groups conversion into carboxylate species. For this latter case, the dissolution of the sodium hydroxide species and the kinetics of end‐groups conversion prove to be rate‐limiting phenomena to generating thinner striated lamellae. Additionally, the ionic strength of the system is notably important to the viscosity response and particle size produced, particularly when surfactant is not added. © 2018 American Institute of Chemical Engineers AIChE J, 64: 2113–2123, 2018     

Evolution of morphology and of chemical conversion along the screw in a corotating twin‐screw extruder

A new sampling device is used to perform near‐real‐time investigations of physical and chemical processes occurring inside a laboratory twin‐screw extruder. Polyamide‐6–ethylene propylene rubber (PA‐6–EPM) blending and styrene–maleic anhydride (SMA) imidation experiments are reported in terms of morphology development and evolution of the chemical conversion along the extruder, respectively. Comparison of the results obtained using this new technique with those of classical screw‐pulling experiments evidenced the potential erroneous conclusions than can be drawn from the latter. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 71: 135–141, 1999     

Experimental study of maleation of polypropylene in various twin‐screw extruder systems

A range of continuous mixing machines were used as continuous reactors for grafting maleic anhydride onto polypropylene. The machines used were (1) a nonintermeshing modular counterrotating twin‐screw extruder, (2) an intermeshing modular corotating twin‐screw extruder, (3) intermeshing modular counterrotating twin‐screw extruder, and (4) a Kobelco Nex‐T continuous mixer. The grafting reaction of maleic anhydride onto polypropylene and degradation of polypropylene during the grafting reaction were investigated as means for comparing these different machines for reactive extrusion. The influence of processing variables such as screw speed and processing temperature on polymer characteristics also was investigated. Generally, in a comparison of the different machines, the intermeshing counterrotating twin‐screw extruder had the lowest levels of grafted maleic anhydride, whereas the Kobelco Nex‐T continuous mixer under the conditions used had the highest levels of grafted maleic anhydride. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 1755–1764, 2003     

Improving mixing characteristics with a pitched tip in kneading elements in twin‐screw extrusion

In twin‐screw extrusion, the geometry of a mixing element mainly determines the basic flow pattern, which eventually affects the mixing ability as well as the dispersive ability of the mixing element. The effects of geometrical modification, with both forward and backward pitched tips, of a conventional forward kneading disks element (FKD) in the pitched‐tip kneading disks element on the flow pattern and mixing characteristics are discussed. Numerical simulations of fully filled, nonisothermal polymer melt flow in the melt‐mixing zone were performed, and the flow pattern structure and the tracer trajectories were investigated. The pitched tips largely affect the inter‐disk fluid transport, which is mainly responsible for mixing. These changes in the local flow pattern are analyzed by the distribution of the strain‐rate state. The distribution of the finite‐time Lyapunov exponent reveals a large inhomogeneity of the mixing in FKD is suppressed both by the forward and backward tips. By the forward tips on FKD, the mixing ability is relatively suppressed compared to FKD, whereas for the backward tips on FKD, the mixing ability is enhanced while maintaining the same level of dispersion efficiency as FKD. From these results, the pitched tips on the conventional KD turn out to be effective at reducing the inhomogeneity of the mixing and tuning the overall mixing performance. © 2017 American Institute of Chemical Engineers AIChE J, 64: 1424–1434, 2018     

Analysis of flow and mixing in screw elements of corotating twin‐screw extruders via SPH

Due to its meshless nature, the smoothed particle hydrodynamics method (SPH) provides high potential for the simulation of free‐surface flows and mixing in complex geometries. We used SPH to analyze the flow inside five typical screw elements of corotating twin‐screw extruders, two conveying elements, two kneading elements and a mixing element. Our results show conveying capabilities, pressure generation and power input for various operation states, completely and partially filled. We conducted a detailed mixing analysis based on tracer particles, which yielded the time evolution of the intensity of segregation for different tracers. From that, we determined exponential mixing rates, which describe the relative decrease of the intensity of segregation per screw revolution and characterize the mixing performance in different operation states. This provides valuable input information for simplified models of extruders, which are relevant to industrial applications and can significantly contribute to the efficient design, optimization and scale‐up of extruders. © 2017 American Institute of Chemical Engineers AIChE J, 63: 2451–2463, 2017     

Experimental investigation of the morphology development of polyblends in corotating twin‐screw extruders

Compounding extruders are still designed based on experience and time‐consuming experimental examinations. This work investigates the morphology development of incompatible polyblends along a mixing zone at the end of a corotating twin‐screw extruder. During the process, the samples are taken from the running extruder using special barrel plates. These samples are subsequently examined by means of scanning electron microscopy (SEM). This method allows sampling in less than 1 min and thus extremely fast and almost unaffected. The experimental investigation of the morphology development improves the knowledge about the factors essentially influencing the blending process. It also allows the verification as well as improvement of theoretical models. Polyblends of polypropylene (PP) and polyamide (PA) with 7.5, 15, and 30 wt % PA were examined. As well as the relevance of the mass percentage of the dispersed phase, the influence of the screw geometry, the screw speed, the melt temperature, the melt throughput, and the pressure profile was investigated. Apart from the melt throughput, all varied factors show an influence on the resulting blend morphology that may not be neglected. However, the changes of the mean particle sizes in the observed mixing zones are only gradual (mean particle size ≈ 1–4 μm), which can be attributed to the extremely fine blend morphology already existing during or after the melting. That means that the application of “classic melting zones” generally already produces finely dispersed blend morphologies, thus proving the essential importance of the melting zones regarding the development of the blend morphology. Consequently, the mean particle sizes, calculated by means of quantitative image analyses of SEM micrographs in the mixing zones following the homogenizing section only slightly depend on the compounding conditions (screw speed, melt throughput, screw geometry, melt temperature, and pressure profile). However, the direct visual analysis of the SEM images, especially in the first parts of the mixing zones, shows the simultaneous existence of large PA6 particles in the PP matrix. In addition, a downstream unification of the particle size distribution can be observed. Especially the number and size of the coarser particles decreases in the mixing zones. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 76: 708–721, 2000     

Effect of composition and processing conditions on the chemical and morphological evolution of PA‐6/EPM/ EPM‐g‐MA blends in a corotating twin‐screw extruder

This study investigated the effect of blend composition and processing conditions on the chemical conversion and morphological evolution of PA‐6/EPM/EPM‐g‐MA blends along a twin‐screw extruder. The maleic anhydride (MA) content of the modified rubber was found to decrease strongly, to a level of almost zero, and in the melting zone the particle size was dramatically reduced, from millimeters to submicrometers. Blend composition had a secondary effect on both chemical conversion and morphological development. The processing conditions, particularly the temperature profile and the screw speed, affected both the chemical conversion and the morphological evolution. Using low temperatures and low screw rotation it was possible to follow in detail the evolution of morphological development of a reactive blend in a twin‐screw extruder. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 1535–1546, 2001     

Experimental investigation of the morphology development and mechanical properties of waste ethylene propylene diene monomer/polypropylene blend in modular intermeshing corotating twin‐screw extruder

Nowadays, with the increase in the number of automobiles, waste EPDM (ethylene propylene diene monomer) is causing a significant environmental problem. From environmental and economical perspectives, recycling is one of the popular methods to solve environmental problems. This study, which involved waste EPDM/PP (polypropylene) blends with the ratio range of 70/30 and 75/25, set out to ascertain the relevance of the mass percentage of the dispersed phase, the influence of the screw geometry, the screw rpm, and the melting temperature of PP materials on the morphology and mechanical properties of the waste rubber blend. The purpose of this study is to develop a high‐value thermoplastic elastomer from waste EPDM. This investigation concentrated on determining the optimum conditions for producing a blend by extrusion, relative to screw geometry, screw rational speed, and operating temperature. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 2276–2282, 2002     

Modeling of industrial nylon‐6,6 polymerization process in a twin‐screw extruder reactor. II. Neural networks and hybrid models

This article describes the application of neural networks and hybrid models to the finishing stage of nylon‐6,6 polycondensation in a twin‐screw extruder reactor. A planned experiment in the industrial and in the pilot plant was employed to build the neural network and the hybrid model. The hybrid model combines information calculated from the phenomenological model with the neural network model. The comparison of experimental with calculated data shows good agreement. During two years, industrial data were collected. The comparisons of the models' prediction with these data were performed and reasonable results are achieved from the industrial point of view. These models help an increase of industrial production of about 20%. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 72: 905–912, 1999     

Residence time in a single screw free helix extruder using a new solution to the biharmonic equation

A new analytical solution for the biharmonic equation was developed for single screw extrusion cross-channel fluid mechanical flow. This analysis led to a quantitative model for residence time distribution when combined with the historic solutions of the drag and pressure flow in the rectangular channel in the single-screw extruder. The focus of the theoretical and experimental investigation here was to examine how closely the new analytical solution correlated with experimental residence time data for a free-helix extruder. This new extrusion device was operated as both a conventional extruder and a more positive displacement device by using only helix rotation as the pump. The Moffatt eddies that occur in the quiescent corners of the rectangular channel with screw rotation were found to have a strong effect on the residence time of the extruder. Because there were no quiescent corners for the free-helix flow there was essentially no residence time tail for this mode of extruder displacement. The theoretical results for a sheet of dye spanning the screw channel width and dye “blobs” were compared with experimental results for both modes of operation. In all cases, the experiments and the theory predictions were essentially consistent.     

Experimental characterization and modeling of twin‐screw extruder elements for pharmaceutical hot melt extrusion

In this study we characterized various screw elements of a co‐rotating twin‐screw extruder used for pharmaceutical hot melt extrusion (HME) and measured the pressure characteristic, i.e., the correlation between the axial pressure gradient and the material throughput in a completely filled screw section at different screw speeds. A typical HME matrix material, Soluplus, was used for the experiments and its required rheological properties were determined. A three‐parameter model based on a dimensionless formulation of the measured quantities was used. These parameters could not be determined uniquely by fitting to experimental data. Therefore we developed an approach to approximate one empirical parameter based on the mechanistic consideration of a pressure‐driven channel flow. The model was extended to account for the variable melt temperature. The results confirmed the expected tendencies and established an essential input parameter set for one‐dimensional simulations of co‐rotating twin‐screw extruders. © 2013 American Institute of Chemical Engineers AIChE J, 59: 4440–4450, 2013     

挤出过程停留时间分布影响因素之间的交互作用

应用全析因设计方法,研究了捏合块角度、比产率(喂料速率/螺杆转速)和螺杆转速对双螺杆挤出机机筒不同位置的延迟时间和平均停留时间的影响,考察了各因素之间的交互作用。结果表明,在所选取的操作条件下,螺杆转速对延迟时间和平均停留时间的影响最大,捏合块角度与比产率的影响程度相近。3因素两两交互作用对延迟时间的影响程度由大到小依次为捏合块角度与比产率、螺杆转速与比产率、捏合块角度与螺杆转速;对平均停留时间的影响由大到小依次为比产率与螺杆转速、捏合块角度与比产率、捏合块角度与螺杆转速。3因素3阶交互作用对平均停留时间的影响比较显著。     

Morphological evolution of polypropylene/polystyrene blends in a twin‐screw extruder

The effects of the blend composition and rotation speed on the morphological evolution of polypropylene (PP)/polystyrene (PS) blends were investigated in a twin‐screw extruder. When PS was the major component, the rate of melt and the rate of dispersion played final roles in the morphological development of the polymer melts. However, when PP was the major component, the rate of dispersion and the rate of coalescence played key roles. A high tendency to coalesce occurred at a high rotation speed and/or a high content of the dispersed phase. When the PP/PS blend composition was close to 1, a cocontinuous morphology was observed to transmute into a coarse one with increasing rotation speed. Attempts were made to correlate the morphology and mechanical properties. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Continuous polymerization of ε‐caprolactone initiated by titanium phenoxide in a twin‐screw extruder

The continuous polymerization of ε‐caprolactone initiated by titanium phenoxide was carried out in both an internal mixer and a twin‐screw extruder. The polymerization was performed under different processing conditions, including various temperatures and screw speeds. To perform a kinetic study, samples were collected along the time axis (internal mixer) and along the screw axis (extruder). Size exclusion chromatography and proton nuclear magnetic resonance were used to study the evolution of the conversion degree with mixing time and with the extruder. The rheological behavior was also characterized. Temperature had a strong effect on conversion in the internal mixer, whereas in the twin‐screw extruder, both temperature and screw speed played major roles. The specificity of the titanium phenoxide to lead to high‐molar‐mass poly(ε‐caprolactone) under these processing conditions was also confirmed. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Continuous polymerization of lactam–lactone block copolymers in a twin‐screw extruder

Continuous copolymerizations of ?‐caprolactone with ?‐caprolactam and ω‐lauryl lactam were carried out in a modular intermeshing corotating twin‐screw extruder. Sodium hydride (initiator) and N‐acetyl caprolactam (coinitiator) were used to synthesize lactam–lactone copolymers in a twin‐screw extruder. We consider the variables of feeding order and feed rate of comonomers on the reactive extrusion of lactam–lactone copolymers. It was observed that simultaneous feeding of both monomers with initiator and coinitiator in the first hopper produced a mixture of homopolymers. When we fed the lactam into the first hopper and caprolactone sequentially into the second hopper, we obtained the lactam–caprolactone block copolymers. However, when we fed caprolactone first into the first hopper and the lactam into the second hopper, the extruded product was a mixture of poly(?‐caprolactone) and lactam monomer. We synthesized high molecular weight copolymers of poly(caprolactam‐b‐caprolactone) and poly(lauryl lactam‐b‐caprolactone) with different block lengths by sequential feeding of monomers. The block length of the block copolymer could be adjusted by controlling the feed rate of each monomer during reactive extrusion. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 1429–1437, 2003     

Investigation on the uniformity of high‐density polyethylene/wood fiber composites in a twin‐screw extruder

Uniform dispersion of wood fiber in high‐density polyethylene can improve the mechanical properties and surface finish of the wood plastic composites. However, it is difficult to achieve uniform dispersion when the wood content is high, due to its low thermal stability, incompatibility with polymer, and affinity for agglomeration. This work was undertaken to improve the uniformity of high‐density polyethylene/wood composites by designing screw configurations, optimizing screw speed, and altering material compositions. The rheological properties and scanning electron microscope micrograph were used to characterize the uniformity. The results showed that the medium dispersive and distributive mixing, medium screw speed, and lubricant were all beneficial in improving uniformity. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

A study of foam granulation and wet granulation in a twin screw extruder

This research investigated a new technique known as foam granulation for the continuous manufacturing of pharmaceuticals by a twin screw extruder. Six grades of hypromellose were compared as binders in the trials, using two addition methods: foam injection by auxiliary side stuffer feeder and liquid injection directly into the extruder. The produced granules were tested for particle size, Carr compressibility index and characteristic fracture strength. It was found that granulation using foam injection improved powder lubrication inside the extruder and wetting uniformity of the lactose, as well as produced granules having lower Carr indices. © 2012 Canadian Society for Chemical Engineering     

利用往复扰动螺棱强化单螺杆挤出机内混合模拟表征

提出了采用副螺棱轴向往复运动提高单螺杆挤出机混合的结构并建立了相应的数学模型。对挤出机内牛顿流体三维周期性流动和混合过程进行了数值模拟。采用有限体积方法,变量分布采用交错网格,副螺棱的周期性运动边界通过叠加网格方式实现。采用4阶Runge-Kutta方法实现流体追踪计算,得到了示踪剂界面增长及累积停留时间分布。采用Poincaré 截面揭示混沌混合存在的区域,证实了副螺棱往复运动能够产生混沌混合效应提高螺槽内的混合效果,与其位置固定时相比,缩短了平均停留时间,停留时间分布变窄。作为对比,同时分析了常规的副螺棱位置固定的单螺杆挤出机内的相应混合行为。