聚苯硫醚的硫化钠法常压合成实验研究及其结构表征

聚苯硫醚(PPS)是一种新型的特种工程塑料。在催化剂Na2CO3的作用下,用对二氯苯(p-DCB)和脱水后的硫化钠在N-甲基吡咯烷酮(NMP)溶剂中常压合成聚苯硫醚。实验中主要研究了硫化钠脱水率、反应温度、原料摩尔比和反应时间对该反应的影响,并提出了可能的缩聚反应机理。结果表明:合成反应条件是最佳反应温度为(195±5)℃,最佳n(Na2S)∶n(p-DCB)=1.1∶1,最佳反应时间为10 h,硫化钠脱水率在70%以上即可得到白色产品,采用的红外光谱、拉曼光谱、热失重及X-粉末衍射等现代仪器分析方法表征了其结构。     

硫化钠法合成聚苯硫醚工艺研究进展

综述了聚苯硫醚的性质、合成方法及目前供需情况.着重介绍了硫化钠法(SSM)工艺(如反应条件、溶剂回收、催化剂、脱水、产物分离、食盐去除等).指出SSM工艺存在产率低、溶剂成本昂贵、产品各项指标较差、纯度低等问题,认为溶剂回收、除盐等工艺还有待深入研究.     

聚苯硫醚合成失败废液中的溶剂回收

针对聚苯硫醚合成过程失败废液中的溶剂N-甲基吡咯烷酮回收方法研究,通过对减压蒸馏、加CuCl2处理后减压蒸馏以及减压精馏三种纯化方法进行对比,经过减压到0.098 MPa下精馏后的N-甲基吡咯烷酮纯度能达到99.35%,完全符合聚苯硫醚合成过程中对溶剂的纯度要求。     

聚苯硫醚的合成

对聚苯硫醚合成进行了研究。在催化剂Na2CO3的作用下,用对二氯苯（P—DCB）和脱水后的硫化钠在N-甲基吡咯烷酮（NMP）溶剂中常压合成聚苯硫醚。实验中主要研究了温度、原料配比和反应时间对该缩聚反应的影响。实验结果表明：适宜的反应温度为（192±3）℃,原料配比为1：1．1（Na3S：P—DCB）,反应时间为8h。     

二硫化钠法合成巯基乙酸的研究

概述了巯基乙酸的用途、合成方法 ,研究了二硫化钠法合成巯基乙酸的主要影响因素。实验从硫化钠、硫磺等基本原料出发 ,首先制得二硫化钠溶液 ,然后将二硫化钠同氯乙酸钠反应合成二硫代甘醇酸 ,最后用硫化钠溶液还原得到巯基乙酸。试验探讨了反应物料配比、反应温度、pH值、反应时间等因素对反应转化率的影响 ,实验结果表明该法的转化率可达 96 %左右 ,其具体反应条件如下 :硫化钠∶硫∶氯乙酸钠 (mol) =1.2∶1.4 4∶1.0 0 ,pH值 =7.5,合成二硫代甘醇酸的温度为 35℃ ,时间为 30min     

N-甲基吡咯烷酮溶剂萃取回收聚苯硫醚生产分析

聚苯硫醚具有较好的耐热性,不易被腐蚀,本身具有良好的力学性能,加工成本低,是特种工程塑料中性能最好的一种材料。采用萃取法在N-甲基吡咯烷酮溶剂中回收聚苯硫醚,并对其进行分析,通过分析萃取的类型以及N-甲基吡咯烷酮中的容量分析萃取的结果。     

聚苯硫醚生产用N-甲基吡咯烷酮溶剂萃取回收研究

采用萃取方法回收聚苯硫醚生产用N-甲基吡咯烷酮溶剂,研究了萃取剂类型、用量以及溶质浓度对N-甲基吡咯烷酮的分配比影响。结果表明,萃取剂选用三氯甲烷,V（O）／V（W）为1：1时,N-甲基吡咯烷酮的分配比可达到1．78。此外,溶液连续萃取实验结果表明,萃取后的溶剂可用精馏分离的方法实现N-甲基吡咯烷酮与三氯甲烷的回收,且二者均可重复使用。     

聚苯硫醚的合成、结构与性能研究

本文论述了聚苯硫醚（PPS）的合成及结构与性能研究的现状，全面阐述了PPS的共混改性及结构改性的途径，并对其应用发展做了进一步的探讨。     

聚苯硫醚的合成与应用

聚苯硫醚（PPS）是迄今为止世界上性价比最高的特种工程塑料，由于在电绝缘材料、导电材料、阻燃材料、摩擦材料、耐热材料和聚合物合金等领域有着广泛的应用而逐渐成为国内外研究热点。笔者综述了聚苯硫醚的结构、性能、合成与应用研究进展，并对今后聚苯硫醚的发展进行了预测。     

Non-Isothermal Crystallization of High-Impact Polystyrene/Poly(Phenylene Sulfide) Blends

The morphology of isothermally crystallized poly(phenylene sulfide) (PPS) and a blend combining it with high-impact polystyrene (HIPS) were observed through a polarized optical microscope equipped with a CSS450 hot-stage. The crystalline superstructure of PPS is mainly spherulite, and it was found that the presence of HIPS has little influence on the morphology of PPS, but decreases the nucleation rate of PPS. The effect of HIPS on the non-isothermal crystallization of PPS was investigated by differential scanning calorimetry (DSC). The maximum and onset crystallization temperatures for the HIPS/PPS blend were about 10°C lower than those of neat PPS, which indicates that the crystallization of PPS was retarded by HIPS. The Ozawa model was used to analyze the non-isothermal crystallization kinetics of PPS and its blends. The Avrami exponent values of neat PPS were higher than those of its blend, which shows that the presence of HIPS changed both the nucleation rate and the crystallization rate of PPS.     

Study on Polymerization Conditions and Structure of Poly(phenylene Sulfide Sulfone)

High molecular weight linear poly(phenylene sulfide sulfone)s (PPSS) were prepared by aromatic nucleophilic substitution reaction at atmospheric pressure. Influences of various polymerization conditions, such as solvent, catalyst, molar ratio, reaction temperature and time, on the molecular weight of PPSS were examined. The intrinsic viscosity of PPSS obtained under optimum synthesis conditions according to orthogonal experiments was 0.55 dl/g. The results of FT-IR, ¹H-NMR, UV spectrum and Raman spectrum confirmed the linear chain nature of product. The maximum UV absorption of PPSS increased with the increase of its intrinsic viscosity. X-ray diffraction and SALS studies indicated that some local ordered structures formed in the samples annealed between 220 ^○C∼240 ^○C for 4 h. The improvement in thermal performance of PPSS of high molecular weight was confirmed by DSC and TGA experiments.     

聚苯醚结构的官能化

对官能化的聚苯醚（PPO）树脂的种类、合成方法及性能进行了综述,并对各类树脂的应用前景进行了展望。     

Overall Investigation of Poly (Phenylene Sulfide) from Synthesis and Process to Applications—A Review

Poly (phenylene sulfide) (PPS) is one kind of high‐performance polymer with high thermal stability that can be used widely in different industrial domains. However, according to an investigation of the literature, few reviews have comprehensively focused on the continuous development of PPS applications in the past decade. To meet this demand, this paper provides an overall investigation of PPS polymer and PPS‐based composites from synthesis and process to applications. Briefly, this paper introduces PPS materials according to the following topics. First, the molecular weight distribution and morphology of PPS, as well as their reinforced parts, are introduced. Afterward, the topic is focused on the synthesis, process, and blending of PPS. In the next part, this paper investigates the key points regarding PPS as a high‐performance polymer, focusing on the aspect of thermal behavior and mechanical properties. Finally, PPS composite applications are emphasized and overviewed from a wide range of aspects.     

New Coupling Agents as Adhesion Promoters at the Poly(Phenylene Sulfide)/Glass Interface-Studies with Micro and Macro Composites

Carboxy-functionalized poly(phenylene sulfide) having different molar masses and amount of the functional group were prepared in order to be used with γ-aminopropyltriethoxysilane as surface treatment of E-glass fibers. These grafted polymer chains act as connecting chains in order to improve the interfacial shear strength of the PPS-glass interface. According to their chemical nature, which is the same as the PPS matrix, and their ability to crystallize in the same crystalline form as the pure PPS, a continuum of bonding from the fiber surface to the bulk matrix is achieved. A chemical linkage is established at the glass surface by means of hydrolyzed ethoxysilane groups of the γ-APS and from the formation of amide units resulting from the reaction of amine functions of the silane and the carboxylic groups of the modified PPS. A “physical” linkage is expected between the grafted PPS and the PPS chains by means of entanglements and co-crystallization. A large improvement of the interfacial shear strength measured from the microdroplet test is observed when a modified-PPS having a medium molar mass and a low amount of functional groups is used in comparison with untreated or silane-treated glass fibers. This improvement is also observed for short glass fibers/PPS composite materials. In fact, a large improvement is obtained on mechanical properties such as the tensile, flexural, and impact strengths.     

New Coupling Agents as Adhesion Promoters at the Poly(Phenylene Sulfide)/Glass Interface-Studies with Micro and Macro Composites

Carboxy-functionalized poly(phenylene sulfide) having different molar masses and amount of the functional group were prepared in order to be used with γ-aminopropyltriethoxysilane as surface treatment of E-glass fibers. These grafted polymer chains act as connecting chains in order to improve the interfacial shear strength of the PPS-glass interface. According to their chemical nature, which is the same as the PPS matrix, and their ability to crystallize in the same crystalline form as the pure PPS, a continuum of bonding from the fiber surface to the bulk matrix is achieved. A chemical linkage is established at the glass surface by means of hydrolyzed ethoxysilane groups of the γ-APS and from the formation of amide units resulting from the reaction of amine functions of the silane and the carboxylic groups of the modified PPS. A “physical” linkage is expected between the grafted PPS and the PPS chains by means of entanglements and co-crystallization. A large improvement of the interfacial shear strength measured from the microdroplet test is observed when a modified-PPS having a medium molar mass and a low amount of functional groups is used in comparison with untreated or silane-treated glass fibers. This improvement is also observed for short glass fibers/PPS composite materials. In fact, a large improvement is obtained on mechanical properties such as the tensile, flexural, and impact strengths.     

3，3’-二乙基-4，4’-二苯甲烷型多马来酰亚胺／聚苯醚树脂的固化反应研究

热固性聚苯醚(PPO)已成为高性能印制电路板用树脂(PCB)发展的主流。本课题组的前期研究表明,3,3,-二乙基-4,4,-二苯甲烷型多马来酰亚胺(PEDM)/烯丙基化PPO是一种新型高性能PCB用树脂。文章采用红外光谱和裂解气相色谱,对PEDM的含量为PPO 10%的PEDM/烯丙基化PPO树脂的固化反应进行研究,结果表明,PEDM分子的不饱和双键与PPO的烯丙基和羟基在加热过程中发生了反应。     

聚（2,5—二甲基）对苯硫醚合成的初步研究

介绍以硫磺、氯和对二甲苯为原料,无水三氯化铁（ＦｅＣｌ３）作催化剂,三氯甲烷（ＣＨ３Ｃｌ３）作溶剂,合成聚（２,５－二甲基）对苯硫醚（ＤＭＰＰＳ）。最佳反应条件为：最佳投料摩尔比：对二甲苯／ＳＣｌ２／ＦｅＣｌ３＝１．０／１．０２／０．１０,反应温度２０～８０℃,反应时间５～６ｈ。收率为６２．５％。产品经红外光谱、Ｘ射线衍射光谱、激光拉曼光谱和差热分析验证,为线型结晶性,无双硫键,熔点Ｔｍ为３０６℃（美国ＲｙｔｏｎＶ－１型ＰＰＳ熔点为２７５～２８５℃的工程高聚物。所述合成方法原料和催化剂价廉易得、合成工艺简化、无副产物ＮａＣｌ产生、操作易、周期短、成本比ＰＰＳ低。其不足之处是产品收率不够高,有待在溶剂和催化剂选择方面作进一步研究。     

玻纤增强聚苯硫醚复合材料的增韧研究

针对玻纤增强聚苯硫醚材料韧性差的问题，对聚苯硫醚傲璃纤维复合体系的增韧进行了研究，考察了玻纤、改性聚合物、有机超细粒子对复合材料力学性能的影响。采用基体增韧（预增韧）与有机超细粒子增韧技术，在保持复合材料拉伸强度和模量的同时，较大地提高了冲击强度，获得了综合力学性能优异的纤维增强聚苯硫醚材料。