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研究了无水硫化钠与对二氯苯(以N-甲基吡咯烷酮为溶剂)合成聚苯硫醚反应的宏观动力学,该反应是一个小分子缩合串联自缩聚的过程,通过测定不同反应聚合体系中氯化钠的徨成率和硫化内的转化率,建立了该反应的宏观动力学方程:1/(1-PNaCl+PNa2s)=C0Kt+1;并计算得到220、250℃的表观反应速率为4.5×10^-4和3.0×10^-3kg/(mol.s),表观活化能为134kJ/mol。 相似文献
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魏秀萍 《分析测试技术与仪器》2014,(3):175-180
建立了一种用毛细管气相色谱法分析合成聚苯硫醚醇洗液组成的方法。其组成包括乙醇、水、对二氯苯和吡咯烷酮,采用DB-WAX毛细管气相色谱柱、TCD检测器。在优化的色谱条件下,4 种醇洗液组分在选择的浓度范围内线性关系良好,相关系数(r)均不小于0.998。在高、中、低3个加标水平下,平均回收率为95.72%~118.75%,相对标准偏差(RSD)均不大于4.91%。方法的检出限(LOD)为0.51~1.74 mg/kg。方法操作简单、准确、高效快捷,适用于硫化钠法合成聚苯硫醚醇洗液中4组分的同时检测。 相似文献
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采用热致相分离法,以己内酰胺为溶剂,制备得到了聚苯硫醚微孔膜并对薄膜性能表征.聚苯硫醚-己内酰胺体系制膜的优点之一是溶剂己内酰胺是水溶性的,可以采用纯水作为后处理的萃取剂.选择了合适的浓度,利用压制成型法制备聚苯硫醚平板膜;研究了体系冷却时的相行为,并考察了降温速率、聚合物浓度等因素对微孔形态与薄膜性能的影响.研究表明,聚苯硫醚-己内酰胺体系以固液分相为主,萃取后形成球晶状的微孔结构.降温速率对薄膜的微孔形态、孔径以及连通性有重要影响;当体系以较低降温速率冷却时,多孔形态为枝叶状,形成了更多的开孔结构并获得了更大的孔径,这是获得高通量微孔膜的主要原因.通过控制降温速率可以制备纯水通量大于100 L/m2h,孔径约4~5μm且连通性良好的聚苯硫醚微孔膜;研究了聚合物浓度的影响,薄膜的纯水通量随着聚合物浓度的增大而减小,并且当聚苯硫醚浓度>50 wt%时,由于大于临界浓度而失去渗透性. 相似文献
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硫化铵溶样催化极谱法快速测定硫磺中痕量硒 总被引:3,自引:0,他引:3
提出硫化铵溶解,氨性介质过氧化氢氧化分解硫磺试样,在0.48mol·L~(-1)HClO_4-4.76×10~(-3)mol·L~(-1)Na_2SO_3-2.96mol·L~(-1)NH_3·H_2O-6.81×10~(-3)mol·L~(-1)(NH_4)_2SO_4-8.41×10~(-4)mol·L~(-1)KIO_3-1.18×10~(-2)mol·L~(-1)硫脲-0.02g·L~(-1)动物胶体系中以催化极谱法测定痕量硒的方法.硒浓度在0.02~9.0ng·ml~(-1)范围内与极谱峰电流有良好的分段线性关系,检出限为0.01ng·ml~(-1).方法的RSD为3.4%~3.9%,加标回收率为91%~97%.此法仪器试剂简单,操作快速简便.用于硫磺样品的测定,结果满意. 相似文献
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聚对苯硫醚[poly(pphenylenesulfide),简称pPPS]的分子链是由对苯撑基和硫原子交替连接构成而使制品抗冲击能力差[1](有些研究者用共聚或共混的方法在pPPS中引入间位结构来达到减少其结晶度,增强韧性的目的)。余自力等[2]用硫磺溶液法合成了mPPS、pPPS及其共聚物,认为在pP... 相似文献
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Poly (phenylene sulfide amide) (PPSA) has been synthesized by using sulfur as Ssource which reacts with dichlorobenzamide (DCBA) and alkali in polar organic solvent atthe atmospheric pressure. The polymer structures were determined by elemental analysis,FT-IR and ~1H-NMR. It is shown that the yielded polymer has linear structure and itsstructure unit is -p-C_6H_4-CONH-p-C_6H_4-S-. The polymer morphology was studied byX-ray diffraction and polarized microscopy. The results show that PPSA is a crystallinepolymer and its spherulites are the aggregation of nontwisting lamella or micro-threadstructure. Under shearing force, these crystals are dispersed to form micro-fibrillarstructure. The decomposition kinetics of PPSA was also studied at different beating rates.The decomposition energy of PPSA is higher than that of PPS. 相似文献
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This is a method of producing crystal linear high molecular weight poly p-phenylene sulfide (HMWPPS) resins by mixing hydrogen sulfide which is produced from the acid gas of desulphurization factory of natural gas, sodium hydroxide, p-dichlorobenzene and additive sodium phosphate, and carrying out the polycondensation in hexamethyl phosphoryl triamide (HPTA) solvent for 4 to 6 h under normal pressure. This method has obvious advantages as simple equipment, easy operation, high activity, stable solvent, high product yield, low cost and it is suitable for large-scale industrial production. 相似文献
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聚苯硫醚纤维的抗张强度与工艺和结构的关系 总被引:1,自引:0,他引:1
以熔融纺丝法制备出不同结晶度的各向同性聚苯硫醚纤维作为样品,根据密度和声速测定值确定出PPS晶相和无定形相的本征横向声模量E0⊥,c(4.40 GPa)和E0⊥,am(1.99 GPa).利用密度梯度法测定出的结晶度Xc和X-衍射法测定的晶区取向因子fc,按照Samules模型计算出不同牵伸和定型工艺下制备的PPS纤维样品的非晶区取向因子(fam),在此基础上分析PPS纤维抗张强度与牵伸定型工艺参数、结构之间的关系.结果表明,PPS纤维的最佳牵伸温度及紧张热定型温度分别在90℃和190℃附近;提高PPS纤维的牵伸温度及紧张热定型温度可以增加纤维的结晶度,在一定范围内对纤维抗张强度的增加有促进作用;但较高的牵伸温度及紧张热定型温度不利于纤维非晶区取向的提高,造成PPS纤维抗张强度降低.牵伸倍数的增加可以有效提高PPS纤维的非晶区取向程度,抗张强度也随着增加. 相似文献
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支化反应型高分子量聚苯硫醚合成研究 总被引:3,自引:0,他引:3
本文以硫磺和对二氯苯为原料,在极性有机溶剂中合成聚苯硫醚(PPS),加入含活性基团的二卤代苯作为共聚第三单体。研究表明,2,5-二氯硝基苯是一种较好的扩链剂,-NO2在反应中将被还原为-NH2,且-NH2在高温下与芳环进一步发生支化反应。当2,5-三氯硝基苯含量低于2%时,控制反应条件,能制得性能优良的支化反应型高分子量PPS树脂。由于共聚第三单体量少,共聚物与中等分子量PPS树脂具有相近的结构。 相似文献
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聚对苯二甲酰对苯二胺/尼龙6复合物 总被引:7,自引:0,他引:7
随着材料科学的发展,纤维增强塑料已由纤维与树脂的复合,扩展到以刚性链高分子与柔性链高聚物在分子水平上的微观复合.棒状、刚性的液晶高分子是一种超高强度和超高模量的高分子材料,同时还具有在某种条件下易于自发取向形成微纤的特性.基于这些性能,液晶高分子自然成为代替无机纤维作增强剂,与柔性链高聚物进行微观复合最理想的材料.在与柔性链高聚物复合时,如何使之在基体中形成有很高的长径比(L/D)的液晶纤维,并在基体中又能起到强的增强效果,来获得高强度、高模量的复合材料.多年来一直是国际上研究的热点,有关这方面… 相似文献
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In this study, we report the melting behavior of poly(phenylene sulfide), PPS, which has been cold-crystallized from the rubbery amorphous state. We find that the crystallization kinetics are faster for cold-crystallized PPS than for melt-crystallized material, due to formation during quenching of a short-range ordered, but noncrystalline, structure. We observe that the endothermic response of cold-crystallized PPS at a large undercooling consists of a low temperature endotherm, followed by an exothermic region, and by the main higher melting endotherm. The lower melting peak temperature of cold-crystallized PPS increases as the crystallization temperature increases, but the main upper melting peak temperature remains almost the same. The size of the exothermic region is strongly related to the degree of undercooling, and must be taken into account in order properly to determine the degree of crystallinity of the material prior to the scan. When the crystallization time is varied, we see a systematic decrease in the size of the main endotherm, and an increase in size of the lower melting endotherm. This suggests that a portion of the main endothermic response is due to reorganization during the scan. Annealing will not only increase the degree of crystallinity but also improve the crystal perfection; therefore the ability of an annealed sample to reorganize decreases as the annealing time increases. However, an additional third melting peak is seen when a cold-crystallized sample is annealed at high temperature for a sufficiently long residence time. The existence of the third melting peak suggests that more than one kind of distribution of crystal perfection may occur when PPS has been cold-crystallized and subsequently annealed. 相似文献