正交法研究PE100管材料熔体强度测试的影响因素

温度、挤出速率、拉伸长度、拉伸加速度、测试轮对间的距离对测试PE100管材专用树脂的熔体强度有一定的影响,用正交试验考察了测试PE100管材专用树脂熔体强度时影响因子的显著性,确定测试PE100熔体强度主要影响因素是温度,次要影响因素是拉伸加速度,而测量轮对间距对测试结果的波动影响仅次于温度,最佳条件为A1(205℃),B1(0.1mm/s),C3(102mm),D3(24mm/s2),E1(0.3mm)。     

新型通用级苯酚-淀粉模塑料(PF2A1)的研制

研制的产品典型配方(质量份)是苯酚-淀粉树脂:六次甲基四胺:木粉:碳酸钙:氧化镁:硬脂酸锌:硬脂酸:油溶苯胺黑:群青=37.0:6.4:48.0:6.0:0.6:0.6:0.4:0.5:0.5;制备工艺参数是混合时间≥60min,工作辊温度85～95℃,空转辊温度145～155℃,辊距2.3～2.5mm,热炼时间4～5min,拼批时间≥45min;模塑工艺参数是预热温度100～110℃,预热时间10～15min,模塑压力≥25MPa,模塑温度175～180℃,模塑时间0.8～1.0min/mm,排气≥3次.产品性能达到酚醛模塑料(PF2A1)国家标准或优良,原料成本比苯酚-甲醛模塑料(PF2A1)低20.4%.     

三元乙丙基固体推进剂包覆层拉伸性能影响因素研究

采用静态单轴拉伸手段,研究了不同试验温度(-40℃、20℃、50℃)、相同拉伸速率(500mm/min)以及相同试验温度(-40℃)、不同拉伸速率(50mm/min、100mm/min、500mm/min)对三元乙丙橡胶类包覆层拉伸应力应变性能的影响。研究结果表明:同一拉伸速率(500mm/min),-40℃试验温度,材料发生脆性断裂,20℃、50℃试验温度,材料均发生屈服、高弹形变直至断裂;随着温度的升高,拉伸强度降低,拉断伸长率增加;同一试验温度(-40℃),拉伸速率为500mm/min时,材料发生脆性断裂,拉伸速率为50mm/min和100mm/min时,材料发生弹性形变。结合GJB770B-2005方法413.1,选用100mm/min的拉伸速率比较适合。     

增容剂SB对LDPE／PS共混物分散相尺寸的影响

用扫描电镜（SEM）研究了不同混合温芳和转速下增容剂苯乙烯－丁二烯二嵌段共聚物（SB）对低密度聚乙烯／聚苯乙烯（LDPE／PS）共混物分散相颗粒尺寸的影响,结果表明,混合温度为150℃时未增容共混物的分散相颗粒尺寸比200℃时粗大,而在150℃中入SB的共混物的分散相颗粒尺寸比200℃时更精细,在150℃时,转速从30r/min至100r/min至100r/min时,未增容共混物的分散相颗平均半径从3．1um降至0.8um,而增容共混物在30r/min时达到平衡颗粒尺寸0．8um,继续提高转速,颗粒尺寸无明显变化。     

盐析微萃取-气相色谱-质谱法测定实验室废水中7种苯系物

采用三氯甲烷作为萃取剂,氯化铵作为盐析剂,建立盐析微萃取-气相色谱-质谱法测定有机实验室废水中甲苯、乙苯、邻二甲苯、间二甲苯、对二甲苯、1,3,5-三甲苯、1,2,4-三甲苯的分析方法。当三氯甲烷用量为25μL,氯化铵用量为0.2 g,5 000 r/min下离心分离5 min时,1 m L水样中的苯系物能很好地被三氯甲烷萃取出来,富集倍数为40倍。色谱条件为:DB-5MS毛细管柱(30 m×0.25 mm×0.25μm),进样口温度220℃,载气为氦气,流量1 m L/min,分流比30∶1,进样量1μL,程序升温为:初始45℃保持3 min,3℃/min升温至70℃,再以30℃/min升至200℃保持2 min。质谱条件为:电子轰击离子源(EI),电子能量69.9e V,离子源温度240℃,四级杆温度150℃,电子倍增器电压1 741 V,采样深度1.5 mm,溶剂延迟3.5 min。在优化萃取和测定条件下,各组分的质量浓度在0.4~80μg/L内与峰面积线性关系良好,相关系数均大于0.992 5,各组分的检出限范围为0.01~0.5μg/L。对成都理工大学有机实验室中废水进行测定,能有效检出所含苯系物,同时做加标回收实验,回收率在92.92%~102.1%之间,相对标准偏差(n=5)在1.9%~4.5%之间,测定结果令人满意。     

FeCuNbSiB非晶粉体/丁基橡胶复合薄膜的力敏特性

以粒径为45μm的Fe73.5Cu1Nb3Si13.5B9非晶粉体为复合相,丁基橡胶为基体相,利用模压成型法制备了粉体含量为85%、厚度为150和200μm的复合薄膜。采用LYYL-500N高档型微机控制压力试验机对薄膜试样进行连续加载/卸载实验(速度分别为0.1,0.5和1.0mm/min),用TH2816LCR数字电桥测试频率1和50kHz下薄膜的阻抗Z值。研究了加载/卸载速度、测试频率、薄膜厚度和环境温度对FeCuNbSiB粉体/丁基橡胶力敏特性的影响。研究表明,复合薄膜在v=0.1mm/min时,其重复性最好,在加载过程中,应力灵敏度|k|值随着应力的增大呈现先增大后减小的变化趋势,卸载过程中,|k|值随着应力的逐渐减小而增大。在1kHz测试频率下复合薄膜的力敏灵敏度高于50kHz。相同测试条件下,厚度为200μm的复合薄膜的力敏灵敏性略优于150μm的。在39.5~80℃温度范围内,随着温度的升高复合薄膜的灵敏度越高。     

橡胶防老剂RD不同分析方法的比较

为比较橡胶防老剂RD(TMQ 2,2,4-三甲基-1,2-二氢化喹啉聚合体(C12H15N)n(n=2～4))高效液相色溶剂梯度洗脱的方法和GC-Ms高温裂解方法测定聚合物的含量,采用高效液相色谱法,以水-甲醇作为流动相,检测波长254nm,流速为1mL/min,C18 4.6mm×150mm/5μm色谱柱;GC-Ms法的热分解温度590℃,分解时间6s,热分解室温度为320℃,注射温度250℃,色谱柱DB-1 30mm×0.32mm×0.25μm,升温速度10℃/min,终温为120℃。载气N2流速为1mL/min,FID检测温度280℃,H2流速为30mL/min,空气流速为300mL/min;面积归一法计算含量。结果表明,高效液相色谱法比气相色谱法稳定、可靠,高效液相色谱法测定橡胶防老剂RD的含量优于气相色谱法。     

超声辅助-乳化液液微萃取-气相色谱法测定水体中7种苯系物

采用正己烷为萃取剂,乙腈为乳化剂,建立超声辅助-乳化液液微萃取-气相色谱法(USA-ELLME-GC)检测水中甲苯、乙苯、对二甲苯、间二甲苯、邻二甲苯、1,3,5-三甲苯,1,2,4-三甲苯的分析方法。当萃取剂正己烷为150μL,乳化剂乙腈为400μL,超声时间为12 min时,50 m L水溶液中苯系物被成功萃取到正己烷中,富集倍数达到333倍。色谱条件为:DB-5MS(30 m×0.25 mm,0.25μm)毛细管柱,进样口温度220℃,检测器(FID)温度250℃,程序升温(初始45℃保持3 min,3°C/min升温至70℃,再以30℃/min升至200℃保持2 min),氢气流量10m L/min,尾吹气流量30 m L/min,分流比30∶1。在优化的萃取和色谱条件下,7种苯系物在0.08~1.00 mg/L浓度范围内与峰面积呈线性关系,相关系数均0.9980,方法检出限为0.005~0.01 mg/L,质量浓度均为0.10 mg/L的苯系物的7次前处理及测定结果相对标准偏差RSD为1.5%~4.7%。建立的方法应用于学校内湖水和实验室废水中7种苯系物的测定,平均回收率为86.5%~110.4%,测定结果满足分析化学痕量分析要求。     

TC4钛合金板材电子束焊接疲劳性能

研究了不同工艺电子束焊接TC4钛合金板材的疲劳性能及断口金相组织。结果表明:工艺为V=150kV、If=366mA、v=600mm/min、Ib=69mA的试样焊缝的疲劳性能最好;气孔和冷隔作为应力集中源起作用而易成为裂纹源;焊缝及母材断口均由小断块组成,断块上有典型的疲劳辉纹;工艺为V=90kV、If=1654mA、v=600mm/min、Ib=51.1mA和V=150kV、If=342mA、v=200mm/min、Ib=29mA的试样焊缝疲劳辉纹间距较母材大,即扩展速率较母材快,疲劳性能不如母材;焊缝柱状晶内的网篮状马氏体组织越粗大,裂纹扩展性能越差;裂纹的扩展方式主要是穿晶断裂,相邻柱状晶内的网篮状组织取向差别太大,穿晶扩展受阻,裂纹便改沿晶扩展。     

对聚氯乙烯/氯化聚乙烯/聚乙烯共混体系的研究

从动态粘弹谱和力学性能的测试证实氯化聚乙烯(CPE)与聚氯乙烯(PVC)不相容,但可以作为PVC/聚乙烯(PE)的增容剂。对共混物的形态研究发现,在PVC/CPE中加入少量低密度聚乙烯(LDPE)有利于CPE连续网状结构的形成。通过双辊混炼机和Brabender流变仪研究了CPE和PE对PVC的抗冲击性能和加工性能的影响。结果表明,CPE能促进PVC的塑化,LDPE能延缓PVC的塑化。在PVC/CPE(100/10)中加入少量PE可使抗冲击强度大大提高。PVC/CPE/LDPE(100/12/2.5)在20℃的抗冲击强度比PVC/CPE(100/12)高30千焦/米~2以上。采用示差扫描量热计研究了共混物分散状态,实验结果表明混炼时间、混炼温度和混料顺序对共混物抗冲击强度有明显影响。     

IN690合金管热挤压温升与挤压力的研究

温升和挤压力是影响钢管挤压过程的重要指标,利用热模拟实验获得了IN690合金的热加工本构关系,建立了IN690合金钢管热挤压过程的有限元模型.采用正交实验设计的仿真实验系统分析了坯料温度（T b=1000～1200℃）、挤压速度（v=20～200 mm/s）和模具预热温度（T d=300～500℃）对管材成形过程中温升...     

丁香罗勒油气相色谱与气质联用分析

目的:建立丁香罗勒油中丁香酚的含量测定方法和鉴定挥发性化学成分。方法:气相色谱法,4mm×2m不锈钢柱,10％SE—30为固定液,Chromosorb WAW 60～80目担体,FID检测器,柱温110℃,水杨酸甲酯为内标物;气质联用,以HP—5毛细管柱,柱温起始120℃保持5min后以5℃/min升温至150℃保持7min,检测质荷比范围10～425。结果:丁香酚在2～10mg/ml范围内具良好线性关系,平均回收率为100.08％,RSD为0.95％;气质联用鉴定了39个化合物。结论:方法简便,快速,准确,可排除其它成分的干扰。     

Hydrostatic extrusion of solid polymers

Hydrostatic extrusion of a high density polyethylene rod was carried out. Both the process of plastic deformation during hydrostatic extrusion and the changes of properties of the polyethylene with extrusion were studied. Particular attention was paid to the process of molecular orientation and the destruction of the original lamellae. To obtain a better understanding of the deformation process, the lateral dimension of crystallite and the long period were obtained from the X-ray diffraction data. Furthermore, the influence of extrusion conditions on the structure and properties of the extrudate were investigated. The Vickers hardness number and thermal shrinkage of the extrudates were affected considerably by the extrusion conditions, i.e. extrusion temperature and extrusion ratio. In order to determine the relationship between the properties and extrusion conditions, it is necessary to consider not only the molecular orientation but also the crystallinity, fibrosity and the fine-structure of the extrudates.     

ZK60镁合金型材挤压过程有限元数值模拟

本文运用DEFORM-3D平台对ZK60变形镁合金型材挤压过程进行了数值模拟.分析了变形温度(T=300℃/350℃)、变形速度(V=2、5mm/s)对合金等效应变、等效应力、温度场以及变形载荷的影响规律.结果表明:温度对等效应力影响显著,变形温度从300℃升高到350℃,合金最大等效应力从75MPa降低到55MPa;变形速度对温升影响显著,挤压速度由2mm/s升高到5mm/s,合金最大温升由81℃升高到118℃.确定了ZK60合金在挤压比为25时,适宜的挤压温度为350℃,挤压速度应在5mm/s以下.     

Elemental speciation analysis by multicapillary gas chromatography with microwave-induced plasma atomic spectrometric detection

Multicapillary column gas chromatography (MC-GC)/microwave-induced plasma atomic emission spectrometry (MIP AES) was developed for fast speciation analysis of organotin compounds in the environment. Ethylated butyltin compounds could be separated isothermally within less than 30 s (instead of ～5-10 min) without sacrificing either the resolution or the sample capacity of conventional capillary GC with oven temperature gradient programming. Careful optimization of the pressure and temperature GC program allowed a comprehensive organotin speciation analysis including phenyltin compounds within less than 2.5 min, increasing the sample throughput 6-fold. Compatibility of MC-GC with an MIP atomic emission detector (MIP-AED) was discussed. MC-GC/MIP-AES was validated for the analysis of sediment (PACS-1 and BCR 462) and biological (NIES11) certified reference materials.     

Hydrostatic extrusion behaviour of high density polyethylene

The solid state processing of a high density polyethylene by hydrostatic extrusion at room temperature has been investigated. The extrusion pressure for a given extrusion ratio is found to depend on the pressure fluid used, the die angle and the velocity of extrusion. The strain hardening behaviour of the resulting extrudates is found to be independent of the extrusion ratio. An effective flow stress equation which accounts for the dependence of the flow stress of high density polyethylene on strain, strain rate and hydrostatic pressure is developed and used in an analysis of the extrusion process based on the upper bound approach. The calculated values of the extrusion pressure as a function of the various extrusion variables are in reasonable agreement with the experimental results.     

12 vol%SiCP/2024Al基复合材料热挤压过程有限元模拟与分析

基于MSC.Marc软件平台,建立了含SiC_P体积分数为12%的SiC_P/2024Al复合材料热挤压轴对称刚-塑性热力耦合有限元分析模型。利用该模型对复合材料的热挤压过程进行模拟,分析了热挤压过程中的载荷-行程曲线和材料流动状态,讨论了模具温度及挤压速度对挤压载荷的影响。模拟结果表明,该坯料在挤压比为30∶1、挤压温度为400～450℃、挤压速度为0.1～1.0 mm/s、挤压载荷为4.0 ×106～5.0 ×106N之间能够顺利挤出表面无缺陷的复合材料棒材。最后通过在 700 t水压机上采用相同工艺挤出高质量的复合材料棒材验证该工艺的可行性。     

HPLC-ELSD法测定普瑞巴林的光学纯度

目的:建立高效液相色谱-蒸发光散射检测法(HPLC-ELSD)检测普瑞巴林的光学纯度。方法:选择ChiralcelOD-H色谱柱(250mm×4.6mm);以正己烷-异丙醇-三氟乙酸(965:32:3)为流动相;流速为0.5mL/min;采用蒸发光散射检测器,漂移管温度为80℃,载气流速为1.6L/min。结果:普瑞巴林的两种光学异构体(S/R)达到良好分离,R-异构体在1.013～10.13μg/mL范围内线性良好,r=0.99902,平均回收率为99.6%(n=15),检测限为12.3ng。结论:本文建立方法简单、快速、灵敏、准确、可靠,适用于普瑞巴林及制剂的光学纯度检测。     

Study on the morphology,rheology and surface of dynamically vulcanized chlorinated butyl rubber/polyethylacrylate extrudates: effect of extrusion temperature and times

A high-damping thermoplastic vulcanizate (TPV) composed of chlorinated butyl rubber (CIIR) and polyethylacrylate (PEA) was prepared by using a twin-screw extruder. The effect of extrusion temperature and times on the morphology, rheology and surface of the extrudates was examined and attempts were made to correlate the extrudate surface with the evolution of two-phase morphology and the rheological behavior. CIIR gel content of each extrudate was also analyzed. The result shows that CIIR gel content increases with increasing extrusion temperature or times; furthermore, extrusion at high temperature can produce numerous PEA and CIIR macromolecular radicals, thus chemical links take place between PEA and CIIR molecules. Morphological analysis indicates that phase inversion occurs at a gel content of around 68%, and with increasing extrusion times at high temperature the dispersed particles become larger and the particle edges become blurrier. All CIIR/PEA extrudates show pseudoplastic flow behavior. The extrusion temperature or extrusion times have a significant effect on melt viscosity of the extrudates. Surface analysis exhibits that co-continuous nature of the two-phase morphology results in melt fracture and periodic distortions on the extrudate surface, but with the increasing extrusion temperature or times the surfaces of the extrudates become gradually smooth.     

Shrinkage as a measure of the deformation efficiency of ultra-oriented high density polyethylene

A simple test is described that allows the evaluation of the molecular extension in solid state extruded high density polyethylene at maximum extrusion draw ratio 36. The samples, which were prepared by shaving the extrudates to films of average thickness 0.4 mm, were melted very rapidly and shrunk at 160° C. Experimental evidence shows that at high heating rates (800° C min⁻¹) all the molecular extension is recovered elastically. The variation of shrinkage with molecular weight indicates a difference in the molecular extension produced during the extrusion, and a simple relationship between molecular draw ratio and modulus is considered.