聚合物特征和试验2005.ppt

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1、Polymer characterization and testing聚合物特征和试验Testing and characterization(generally 3 categories)试验和特征（通常可分为三类）Production lab testing for polymer QA release为发放聚合物质量保证书而进行的生产实验室试验 Mfr,solubles,additives,etc，熔体流动速率（MFR）、可溶性和添加剂等Non-routine polymer structure testing非常规的聚合物结构试验 MWD,tacticity,melting beha

2、vior，分子量分布（MWD）、立构规正度、熔融特性Application testing(how does it perform post processing)应用试验（在后加工过程中表现的特性）Tensiles,HDT,flex mod,impact,etc，拉伸强度、热变形温度（HDT）、弯曲模量、抗冲击强度等 Testing of molded parts(microscopy,gloss,etc)，对模塑零件进行的试验（显微镜试验、表面光泽等）Production testing生产试验Mfr，熔体流动速率（MFR)Additive content，添加剂含量Ethylene co

3、ntent，乙烯含量Hexane extractables，己烷可抽提物Decalin solubles，十氢化萘可溶物Xylene extractables，二甲苯可抽提物Volatiles，挥发份Yellowness index，黄度指数Pellet size，塑料粒子尺寸Powder particle size distribution，粉体颗粒度分布Powder metals analysis，粉体金属含量分析Dirt/contamination/pellet appearance test，杂质污染物以及粒子的外观试验Filter pressure rise/gel test，过滤器

4、压力升高凝胶试验Mfr熔体流动速率ASTM D1238美国材料实验协会ASTM D1238（试验方法的标准）Measures viscosity of PP melt(a function of Mw)测量聚丙烯熔体的粘度（是分子量的函数）Samples size from 2.5 to 6.0 grams(higher MFR requires more sample because more flows through machine during test)样品重量2.5-6克（MFR较高的样品，由于在试验中流经测试仪器的流量较大，所以需要更多试样量）Cylindrical chambe

5、r filled with resin and piston set in place将被测树脂填满圆筒形的测试管，将活塞安放就位After 4 minute preheat,2.16kg weight placed on piston and piston pushed to calibration mark(6 minutes)预热4分钟后，将2.16公斤的重锤安放在活塞的顶端，并将活塞推到校准的标记位置（6分钟）Cut extrudate start timer.At end of time period,cut extrudate切断熔体的挤出条，按动秒表计时，在定时周期结束时，再次切

6、断熔体的挤出条Mfr continued熔体流动速率（MFR)（续）Mfr(gms/10 minutes)=weight of extrudate/time intervalMFR（克10分钟）挤出条的重量时间间隔Generally an automated process通常是一个自动进行的测试过程Customers often have only 1 plastometer;may not agree with our lab客户通常只有一台塑性计，有可能和我们实验室仪器的型号不同Tinius Olsen MP600=右图为Tinius Olsen MP600 型Multiple extr

7、usions/MFR testing measures additive package effectiveness多次挤出熔体流动速率测试，测量添加剂配比的有效性Additive content添加剂含量Only one“key additive”is measured in the pellet 只测定塑料颗粒中“关键添加剂”的含量The key additive level is used as an indicator of total additive level and other additive levels.根据各项添加剂的添加比例，用这项关键添加剂的含量来表示总的添加剂含量

8、以及其它添加剂含量Method depends on the additive Masterbatch being correct!本方法取决于添加剂母料混合物的配方比例必须是正确的Some additives are easier to measure with precision than others(typical key additives are phenolics,phosphites,and CaSt or DHT).某些添加剂要比其它添加剂更容易精确测定（常用的关键添加剂有酚醛树脂、磷酸酯，和硬脂酸钙或二丁基羟甲苯（DHT）Specific tests used to det

9、ermine additive level include FTIR and XRF用于测定添加剂含量的特殊试验方法包括富利埃变换红外光谱法（FTIR)和X射线荧光分析法（XRF）FTIR富利埃变换红外光谱“Fourier Transform InfraRed”Spectroscopy“富利埃变换红外”光谱Good for Phenolics,Hindered Phenols(Primary stabilizers and UV Stabilizers),and similar molecules适合于酚醛树脂、受阻酚(主要的稳定剂和紫外光稳定剂)以及类似分子的检测Common Key add

10、itives include Irganox 1010/3114,DGMS,and Tinuvin 622,and Sodium Benzoate常用的关键添加剂包括 Irganox 1010/3114、DGMS 以及 Tinuvin 622 和苯甲酸钠Pellets are compression molded into sheet,which is inserted into machine先将样品塑料粒子压制成薄片，然后将样片插入到检测仪器中Calibration curve needed to calculate additive level需要用校正曲线来计算添加剂的含量XRF:X-

11、Ray Fluorescence SpectrometerXRF:X-射线荧光光谱仪Good for additives containing Calcium,Phosphorus,Sodium,Sulfur,Zinc适合于检测含有钙、磷、钠、硫、锌的添加剂Pellets pressed into plaque and inserted into machine先将试样塑料粒子压制成型为样板，然后将样板插入检测仪器Need to have a calibration curve for additive必须先建立一条添加剂含量的校正曲线 添加剂硬脂酸钙DHT柠檬酸二氢钾苯甲酸钠DSTDP，硫代

12、二丙酸二硬脂醇酯 DMTDP，硫代二丙酸二甲酯BZ，二丁基二硫代氨基甲酸锌 元素钙，Ca镁，Mg磷，P磷，P磷，P磷，P磷，P磷，P钾，K钠，Na钠，Na硫，S硫，S锌，ZnEthylene Content乙烯含量Uses FTIR(pressed plaques,etc)采用富利埃变换红外光谱（试样压片等）Calculates计算 Total weight percent ethylene 乙烯的总重量百分比含量 Weight Percent ethylene in the random copolymer segment 无规共聚物片断中的乙烯重量百分比含量 Calculates the

13、percentage of the impact copolymer composed of ethylene-propylene random copolymer 计算由乙烯-丙烯无规共聚物组成的高抗冲共聚物的百分比含量Used for QC control and product release用于QC控制以及发放产品质量证书Hexane Extractables己烷可抽提物Pellets are ground into a powder 先将塑料粒子磨成粉末Refluxed in boiling hexane for 3 hours in a thimble放在套管内用沸腾的己烷回流三小

14、时Weight lost in extraction is reported as%hexane extractables称重计算抽提失重，计作己烷可抽提物百分比 In plant environment,%HE is also measured by NMR在工厂环境中，己烷可抽提物百分比也可以用核磁共振法（NMR）进行测定 Same sample prep 准备相同的样品 NMR must be calibrated based on numerous known samples NMR必须用各种已知的样品进行校正Decalin and Xylene Solubles十氢萘和二甲苯可溶物X

15、ylene extracts more from the resin than hexane二甲苯可以比己烷从树脂中抽提出更多的提取物Decalin extracts more from the resin that Xylene十氢化萘可以比二甲苯从树脂中抽提出更多的提取物Decalin test procedure:十氢化萘试验步骤：powder sample is dissolved in heated decalin 将粉状样品溶解在加热的十氢化萘中 the solution is chilled at 0C,and then filtered 将溶液在0C下冷冻，然后进行过滤 The

16、 resulting solution is placed in a weighed pan,and heated at 120C for 2 hours.Material in pan is decalin solubles.将过滤所得的溶液放置在一个称量盘中，在120C下加热两小时，称重盘中的剩余物料计作十氢化萘可溶物Xylene typically not used by BP NA,though other suppliers use itBP 北美通常不采用二甲苯可溶物指标，虽然其它供应商采用这个指标NMR is also used to test DS and XS也可以用核磁共振法(NMR)进行十氢化萘可溶物(DS)和二甲苯可溶物(XS)试验Oven Volatiles烘箱挥发份试验Sample is sealed in metal container when taken from unit 将从生产装置上取来的样品放置在密封的金属容器中For powder,20 g is placed into a pre-weighed disposable aluminum di