非啮合双螺杆挤出过程停留时间分布实验研究

通过对非啮合双螺杆挤出过程常规螺纹纹元件螺杆组合及引入轴向循环段的螺杆组合下的停留时间的实验研究，分析了轴向循环段的引入对非啮合双螺杆过程中停留时间及其分布的影响。     

Production of controlled-rheology polypropylene resins by peroxide promoted degradation during extrusion

Results of experimental and modeling studies of the peroxide promoted degradation of polypropylene (PP) are presented. Experiments were carried out, in glass ampoules and in a plasticating extruder. The initiator, 2.5-dimethyl-2,5-bis(tert-butylperoxy)hexane was used as a radical generator. The extruder used had a 38 mm diameter and 24:1 L/D single-screw. In these experiments, the effect of peroxide concentration and screw speed on the molecular weight distribution (MWD) of the polypropylene resin was studied. Samples collected from the experimental runs were analyzed for melt flow index (MFI), flow curve, extrudate swell, and MWD. The measured data are presented and correlations among various parameters are considered. Generally, it can be concluded that controlled-rheology (CR) resins with lower molecular weight, narrower MWD, and reduced viscosity and elasticity, can be produced, A kinetic model for the peroxide Initiated degradation of PP is proposed. Simulations based on this model are compared with experimental data for the production of CR resins. The experimental data were obtained from three sources: (i) industry, (ii) literature, and (iii) present experimental work. The comparison was done in terms of average molecular weights of the resin. Agreement between model predictions and experimental results is quite satisfactory suggesting that this model should find use in commercial practice.     

同向双螺杆挤出机的停留时间分布及填充度

引 言 双螺杆挤出机在高分子材料加工中已被广泛地应用于聚合物共混改性、反应挤出及高分子可控降解等各个方面[1].但先前对挤出过程研究较少,一般仅停留在"黑箱"型经验操作的层面,主要以定性的机械设计为主.     

Measurements of residence time distribution for the peroxide degradation of polypropylene in a single-screw plasticating extruder

Measurements of the residence time distribution (RTD) in a single-screw plasticating extruder were carried out during experimental studies of the peroxide-initiated controlled chemical degradation of polypropylene (PP). A radioactive tracer method was employed, and the effect of screw speed, temperature, and reaction on the RTD was examined. An increase of the peroxide concentration resulted in a broader distribution whereas an increase of the extrusion temperature was found to result in a narrower distribution. Use of low screw speeds simply increased the time delay through the extruder without affecting considerably the breadth of distribution. Results obtained from the present experiments were compared with several theoretical models.     

发泡用高熔体强度聚丙烯的研究

以过氧化苯甲酰(BPO)为引发剂,在同向双螺杆挤出机上对聚丙烯(PP)进行硅烷交联,制备了高熔体强度聚丙烯(HMSPP),然后制得高发泡倍率的PP制品.实验对改性PP的熔体强度、力学性能、热性能和发泡性能进行了表征.结果表明:自制HMSPP的熔体强度是纯PP的5.01倍,力学性能和耐热性与纯PP相比均有较大提高,可用于成型高发泡倍率制品.     

茂金属聚乙烯交联反应挤出流动模型分析

在研究茂金属聚乙烯在双螺杆挤出机中进行的复合交联反应挤出过程流动模型时,在三参数关联流动模型中引入了第4个参数,获得了更好的停留时间分布曲线拟合效果。但是,其物理意义难以确定。为此,根据双螺杆挤出机的结构特点提出了RDBFC模型,获得了较好的拟合效果,物理意义更加合理。     

挤出加工方法对制备PP/PET原位微纤共混物微观形态的影响

分别使用双螺杆挤出机、配备不同结构螺杆或强剪切机头的单螺杆挤出机对聚丙烯(PP)/聚对苯二甲酸乙二醇酯(PET)进行熔融共混挤出,并用扫描电子显微镜观察了产物的微观形态。结果表明,使用双螺杆挤出机或使用配备三段式螺杆的单螺杆挤出机挤出PP/PET,只能制备出PET以球状形态均匀分散在PP连续相中的共混物,不含有任何微纤;使用配备有头部直槽混炼件的单螺杆挤出机挤出PP/PET,部分PET会形成短而粗的微纤;采用熔融挤出热拉伸淬冷法挤出PP/PET,可生产出微纤直径约为5 μm、长径比超过20的原位微纤共混物;采用强剪切机头及头部配备有直槽混炼件螺杆的单螺杆挤出机挤出PP/PET,可生产出微纤直径约为5~7 μm、长径比超过20的原位微纤共混物,且该方法操作简单、辅助设备少、具有工业可行性。     

Controlled Degradation of Polypropylene: A Comprehensive Experimental and Theoretical Investigation

Experimental and modeling studies of the free-radical-induced degradation of polypropylene (PP) in the melt phase have been carried out. Experiments have been performed in a single-screw plasticating extruder using a peroxide as the free-radical source. Concentration of the peroxide was in the range 0.01–0.6 wt%. Results in the form of melt flow index (MFI) values, viscosity curves, and molecular weight distribution (MWD) of the produced resins are presented here. Based on these results, a constitutive equation describing the shear viscosity of the melt as a function of shear rate, temperature, and molecular weight has been derived. The extensional viscosity of these resins has been determined as a function of strain rate using Cogswell's analysis of converging flows. A previously developed kinetic model (plug flow) has been used to simulate the changes of the average molecular weights of the MWD, and a sensitivity analysis of this model has been carried out.     

高抗冲聚丙烯材料的制备

采用过氧化物引发剂与助交联剂组合对聚丙烯（PP）进行交联改性。研究了加工工艺、引发剂和助交联剂对改性效果的影响。结果表明，当选用交联剂A1和助交联剂B，且其用量分别为0.05%和1.0%时，在双螺杆挤出机上进行反应挤出，得到了高抗冲聚丙烯材料，在保持其它力学性能良好的前提下，它的悬臂梁制品冲击强度高达356J／m，为纯共聚聚丙烯的3倍多。     

Reactive extrusion of polyolefin ternary blends

Reactive extrusion of polypropylene (PP)/ethylene–propylene–diene terpolymer (EPDM)/high-density polyethylene (PE) (80/10/10 by weight) blends were carried out using a corotating twin-screw extruder. The effects of peroxide and coagent concentrations and extruder rpm were studied in terms of rheological, morphological, thermal, and mechanical properties of the blends. Melt viscosity of the peroxide-treated blend increased and decreased over the untreated one depending on the amount of a coagent. Morphologically, interfaces blur with only a peroxide treatment, and significant domain reduction was obtained when peroxide and a coagent were used together. Both T_m (crystalline melting temperature) and T_g (glass transition temperature) of PP increased in the blend, whereas those of PE slightly decreased. © 1996 John Wiley & Sons, Inc.     

RESIDENCE TIME DISTRIBUTION IN A SCREW EXTRUDER

It has been studied that the residence time distribution(RTD)function in a screw extruder in relation to that in thescrew and that in the die.For a complex flow field such as that between screw and die,it was supposed that the RTDfunction in the screw and that in the die were almost independent on each other.Therefore,a probabilistic method wasused to predict the RTD function in a complete extruder from that in the screw and that in the die.The experiments fordetermining the RTD were based on a stimulus-response technique.The results predicted,both in single-screw extruderand in twin-screw extruder,were in good agreement with those experimentally obtained.     

Experimental investigation on two-phase air/high-viscosity-oil flow in a horizontal pipe

The flow of very-viscous-oil and air through a horizontal pipe (inner diameter 22 mm) is experimentally studied. We first build and analyze the flow pattern map; a comparison between the air–water and the air–oil flow pattern maps shows a strong influence of the fluid properties. The experimental flow maps are compared with empirical and theoretical ones – Baker (1954), Mandhane et al. (1974), and Petalas and Aziz (1998) – showing a poor agreement. Experimental pressure gradients are also reported and compared with theoretical model, but also in this case the agreement is not very satisfactory. Finally, the elongated bubble velocity and length are measured and compared to model present in the literature. We conclude that the high viscosity of the liquid phase has a strong influence on the results and that the current models are not able to predict the flow features satisfactorily.     

Quantifying sub-grid scale (SGS) turbulent dispersion force and its effect using one-equation SGS large eddy simulation (LES) model in a gas–liquid and a liquid–liquid system

The one-equation SGS LES model has shown promise in revealing flow details as compared to the Dynamic model, with the additional benefit of providing information on the modelled SGS-turbulent kinetic energy (Niceno et al., 2008). This information on SGS-turbulent kinetic energy (SGS-TKE) offers the possibility to more accurately model the physical phenomena at the sub-grid level, especially the modelling of the SGS-turbulent dispersion force (SGS-TDF). The use of SGS-TDF force has the potential to account for the dispersion of particles by sub-grid scale eddies in an LES framework, and through its use, one expects to overcome the conceptual drawback faced by Eulerian–Eulerian LES models. But, no work has ever been carried out to study this aspect. Niceno et al. (2008) could not study the impact of SGS-TDF effect as their grid size was comparable to the dispersed bubble diameter. A proper extension of research ahead would be to quantify the effect of sub-grid scale turbulent dispersion force for different particle systems, where the particle sizes would be smaller than filter-size. This work attempts to apply the concept developed by Lopez de Bertodano (1991) to approximate the turbulent diffusion of the particles by the sub-grid scale liquid eddies. This numerical experimentation has been done for a gas–liquid bubble column system (Tabib et al., 2008) and a liquid–liquid solvent extraction pump-mixer system ( [Tabib et al., 2010] and [28] ). In liquid–liquid extraction system, the organic droplet size is around 0.5 mm, and in bubble columns, the bubble size is around 3–5 mm. The simulations were run with mesh size coarser than droplet size in pump-mixer, and for bubble column, two simulations were run with mesh size finer and coarser than bubble diameter. The magnitude of SGS-TDF values in all the cases were compared with magnitude of other interfacial forces (like drag force, lift force, resolved turbulent dispersion force, force due to momentum advection and pressure). The results show that the relative magnitude of SGS-TDF as compared to other forces were higher for the pump-mixer than for the coarser and finer mesh bubble column simulations. This was because in the pump-mixer, the ratio of “dispersed phase particle diameter to the grid-size” was smaller than that for the bubble column runs. Also, the inclusion of SGS-TDF affected the radial hold-up, even though the magnitudes of these SGS-TDF forces appeared to be small. These results confirms that (a) the inclusion of SGS-TDF will have more pronounced effect for those Eulerian–Eulerian LES simulation where grid-size happens to be more than the particle size, and (b) that the SGS-TDF in combination with one-equation-SGS-TKE LES model serves as a tool to overcome a conceptual drawback of Eulerian–Eulerian LES model.     

双螺杆挤出机螺杆组合对聚丙烯/纳米CaCO3复合材料在线流变性能的影响

采用啮合型同向旋转双螺杆挤出机制备聚丙烯(PP)/纳米碳酸钙(nano-CaCO3)复合材料,制备过程中在双螺杆挤出机末端连接Haake在线流变仪进行在线流变性能测试。研究了两种螺杆组合结构、纳米CaCO3含量对PP/纳米CaCO3复合材料在线剪切黏度的影响,比较了在不同聚合物加工流场下PP/纳米CaCO3复合材料的在线流变性能。结果表明,引入分布混炼有利于降低复合材料的剪切黏度,复合材料剪切黏度随纳米粒子的加入先呈下降趋势,当达到某一含量后,再提高纳米粒子含量会使黏度提高。     

A one dimensional model for the prediction of extraction yields in a two phases modified twin-screw extruder

Solid/liquid extraction is performed on raw plant substrate with a modified twin-screw extruder (TSE) used as a thermo-mecano-chemical reactor. Visual observations and experimental residence time distributions (RTD) are used to develop a solid transport model based on classical chemical engineering method. Modeled and experimental residence times are compared. The transport model is then coupled with a reactive extraction model in order to predict extraction yields.     

Analysis of residence time distribution in the extrusion process including the effect of 3-D circulatory flow

It is of great importance to accurately measure or predict the Residence Time Distribution (RTD) in designing extruders and/or in setting up a proper operating condition, because chemical reactions depend significantly on the RTD and temperature when chemical reactions take place during the extrusion process. A previous method to predict the RTD can analytically determine RTD, Residence Time Distribution Function f(t) and Cumulative Residence Time Distribution Function F(t), based on a simplified two-dimensional velocity field in an extruder. However, this previous method cannot accurately take into account the three-dimensional circulatory flow inside the extruder. The present paper suggests a new method to accurately determine the RTD taking into account the three-dimensional circulatory flow and presents a new formula derived to calculate f(t). In order to demonstrate the applicability of the new method including the circulatory flow effect, RTD, f(t) and F(t) were calculated based on a three-dimensional velocity field obtained via a quasi-three-dimensional finite element analysis. It was found that the previous method has a tendency to underestimate the RTD, owing to the neglect of the three-dimensional circulatory flow in comparison with the new method.     

玻璃微珠改性PP和LLDPE力学性能的比较研究

采用玻璃微珠(GB)改性聚丙烯(PP)和线性低密度聚乙烯(LLDPE)，对玻璃微珠的用量、粒径和复合材料加工方法对材料的力学性能的影响进行了比较研究。结果表明：随着GB用量的增加，单、双螺杆挤出GB／PP复合材料的拉伸模量、弯曲强度和弯曲模量均呈线性增长的趋势，而屈服强度则有小幅下降；断裂应变在低含量时有所提高，然后迅速下降；单双螺杆挤出材料的冲击强度均有所提高，并在一定范围内随GB用量的提高而增大，且单螺杆挤出材料的冲击强度略高于双螺杆挤出材料。而GB／LLDPE中，随着GB用量的增加，单螺杆挤出复合材料的拉伸模量、弯曲模量均呈线性增长趋势，而屈服强度和弯曲强度在含量较高时略有上升；双螺杆挤出复合材料的拉伸模量、屈服应力、弯曲强度和弯曲模量均呈线性增长的趋势，两者的断裂应变都有所降低，但没有严重劣化LLDPE复合材料的冲击特性。GB的粒径对两种复合材料的力学性能影响不大，但对GB／PP复合材料的韧性有较大影响。单、双螺杆挤出GB／PP复合材料的冲击强度在一定范围内较纯料有一定提高；同样的，双螺杆挤出复合材料的冲击强度低于单螺杆挤出材料。     

同向双螺杆不同螺纹元件混炼效果的数值研究

采用Polyflow软件数值模拟了啮合同向双螺杆挤出机流道内聚丙烯(PP)熔体的流动,数值计算了常规螺纹元件和开槽螺纹元件流道内PP熔体的三维等温流场,采用粒子示踪分析法(PTA)分析了不同螺纹元件流道内粒子的拉伸度自然对数、分离尺度和停留时间,比较了常规螺纹元件和开槽螺纹元件的混炼效果。研究表明,与常规螺纹元件相比,由于熔体在沟槽内产生漏流,开槽螺纹元件的建压输送能力较低,分散混合性能较弱;开槽螺纹元件流道内因粒子的停留时间较长,其分布混合性能优于常规螺纹元件。     

Dynamical modelling of a reactive extrusion process: Focus on residence time distribution in a fully intermeshing co-rotating twin-screw extruder and application to an alginate extraction process

The context of this study is the modelling of reactive extrusion process based on an alginate extraction protocol. Residence Time Distribution (RTD) is one important part to predict the kinetics of reactive compounds. A simple model is proposed to predict RTD in fully intermeshing co-rotating twin-screw extruders without reaction. This model, which can be easily extended to reactive case in a future work, is based on the extension of an axial dispersion model, including control parameters (screw speed and flow rate) and geometrical parameters (screw profile and die design). Simulations were performed for various operating and geometrical conditions so as to illustrate possibilities offered by the proposed model. Validation was conducted for two different extrusion applications, seaweed extrusion and polymer extrusion. This highlighted the model ability to predict RTD for various kinds of materials after adjusting only one parameter thanks to a unique experimental RTD curve.     

Mixing characteristics of different tracers in extrusion of polystyrene and polypropylene

To characterize the actual flow behavior of polymer, polystyrene (PS) and polypropylene (PP) macromolecular tracers were synthesized by copolymerization and graft routes. The two tracers were then used to obtain the residence time distribution (RTD) functions of PS and PP in a twin‐screw extruder. The effect of temperature on RTD is discussed using different tracers. The mixing characteristics of different tracers in the extrusion of PS and PP were compared by measuring the overall and partial RTDs. The dependence of the overall and partial RTDs on the tracer types was investigated. The effects of mixing intensity, miscibility, and melting difference on the measured distribution were also discussed. POLYM. ENG. SCI., 54:310–316, 2014. © 2013 Society of Plastics Engineers