杀菌剂5—氯—2—甲基—3—异噻唑酮的合成

通过三步反应合成５－氯－２－甲基－３－异噻只酮。ａ）丙烯酸甲酯、多硫化钠、亚硫酸钠在０℃～５℃反应５ｈ得二硫代丙烯酸甲酯,收率９０％;ｂ）二硫代丙烯酸甲酯、甲苯、甲醇混合液在１５℃～２０℃下滴加甲胺反应１０ｈ得Ｎ,Ｎ－二甲基０－二硫代丙烯酰胺,收率１００％;ｃ）Ｎ,Ｎ－二甲基－二硫代丙烯酰胺、二氯乙烷混合液在２５℃滴加二氯砜升温反应１５ｈ,经过后处理得５－氯－２－甲基－３－异噻唑酮。     

N—乙酰基—S—Mang牛儿基—L—半胱氨酸及其类似物的合成

报道了3种聚异戊间二烯化合物－N－乙酰基－S－Mang牛儿基－L－半胱氨酸,N－乙酰基－S－法尼基－L－半胱氨酸及S－法尼基－巯基乙酸的合成,产品经薄层层析、元素分析、核磁共振氢谱证实。     

N—芳基—4—（N—苯甲酰基）亚胺基—5—异丙叉基恶唑烷—2—酮的合成及其波谱表征

由N－芳基－4－亚胺基－5－异丙叉基恶唑烷－2－酮苯甲酰化制得N－芳基－4－（N－苯甲酰基）亚胺基－5－异丙叉基恶唑烷－2－酮，其结构式得到了产共振波谱和质谱数据的确认，后者分子为刚性分子结构，相关质子分别处于苯甲酰基的屏蔽区和去屏蔽区，因而其^1HNMR波谱发生了不同程度的化学位移变化。     

3—二氯乙酰基—2—甲基—2—乙基—1，3—恶唑烷的合成研究

以w(NaOH)=33%水溶液为催化剂、乙醇胺、丁酮和二氯乙酰氯为原料，一步法合成了3－二氯乙酰基－2－甲基－2－乙基－1，3－恶唑烷。采用正交实验设计获得最佳反应条件；三氯甲烷做溶剂，反应温度－4－4℃，反应搅拌时间1h，产物收率78．6％。产品经红外光谱、核磁共振和元素分析确证。     

1—氧—乙酰基—2,3,5—三—氧—苯甲酰基—4—（1‘—胸腺嘧啶）—α—L—来苏糖 …

首次应用超声波新技术合成了１－氧－乙酰基－２,３,５－三－氧－苯甲酰基－４－（１’－胸腺嘧啶）－α－Ｌ－来苏糖,反应时间１．５ｈ,产率５５％,和通常的化学合成方法比较以应速度和产率有较大的提高。     

N，N—二甲基—N′—月酰基—1，3—丙二胺的合成

以月桂酸和N,N－二甲基－1,3－丙二受为原料,合成了N,N－二甲基－N′－月桂酰基－1,3－丙二胺,通过改变反应温度,酸胺的量比和投料方式,探索反应的优化条件。结果显示,当反应温度为160℃,n(月桂酸）：n（N,N－二基－1,3－丙二胺）＝1．00：1．10,N,N－二甲基－1,3丙二胺按40min连续滴加时,产物的游离酸值最低,为5．54mg/g。产品的红外光谱与标准样品的谱图相符。     

1—羟乙基—2—苯并咪唑氨基甲酸甲酯和1—乙基（2‘—丙烯酸酯—1’—基）—2—苯并咪唑氨基甲酸甲酯的合成及用薄层一紫外分光光度法测定其含量

1－乙基（2‘－丙烯酸酯－1‘－基）－2－苯并咪唑氨基甲酸甲酯是合成多菌灵高分子化学型缓释剂的重要单体。本文报道了1－乙基（2‘－丙烯酸酯－1‘－基）－2－苯并咪唑氨基甲酸甲酯及其制备过程中的中间体－1－羟乙基－2－苯并咪唑氨基甲酸甲酯的合成和分析方法。     

N、N—二甲基—α（1，3—二氧六环—5—）苄胺的合成

介绍了三种N,N－二甲基－α－（1,3－二氧六环－5－）苄胺的合成方法及其药用作用。并详细介绍了以苯甲醛为原料的合成方法。     

2—羟基—2—甲基—1—苯基丙酮的合成

以苯、正丁酰氯、溴、氢氧化钠等为主要原料，经三步反应合成了紫外光引发剂2－羟基－2－甲基－1－苯基丙酮，通过实验，确定了合成路线及较佳的工艺条件，总收率高于80％，具有较好的经济效益。     

1—苯基—3—甲基—4—苯甲酰基吡唑酮—5从醋酸中萃取镍的研究

研究了1－苯基－3－甲基－4－苯甲酰基吡唑酮－5从醋酸盐介质中对镍的萃取，发现体系中同时存在三个萃取平衡。文中给出了三种萃合物可能的结构，给出了这些平行反应中各独立反应的平衡常数及热力学函数并提出了它们的求算和数据处理方法。     

维生素对聚乙烯醇溶液静电纺丝性能的影响

将维生素(VC)溶解在质量分数8%的聚乙烯醇(PVA)水溶液中,通过静电纺丝制得PVA/VC共混纳米纤维。分析了VC含量对溶液性能及静电纺丝速度的影响;测试了纤维的形貌结构及力学性能。结果表明:PVA/VC共混溶液属于切力变稀流体;当PVA/VC质量比为100/10或100/20时,共混溶液的电导率和静电纺丝速度较纯PVA溶液明显提高,制得的纳米纤维表面光滑,粗细均匀;与纯PVA纳米纤维比较,其平均直径和拉伸强度降低,断裂伸长率提高。     

Structure and Performance of Poly(vinylidene chloride‐co‐vinyl chloride) Porous Membranes with Different Additives

Poly(vinylidene chloride‐co‐vinyl chloride) (P(VDC‐co‐VC) membranes were prepared by non‐solvent‐induced phase separation and adjusted by adding water‐soluble polyethylene glycol (PEG) and water‐insoluble silicon dioxide (SiO₂) hydrophilic nanoparticles. The structure of pores and antifouling performance were investigated to illustrate the effect of these nanoparticles. The cross section of the P(VDC‐co‐VC) membrane exhibited more macropores and the typical finger‐like pores turned into more vertically interconnected ones with increasing PEG content, while the number and size of finger‐like pores became less with increasing SiO₂ content. Considering the filtration and antifouling experiments, the presence of hydrophilic PEG and SiO2 nanoparticles in the P(VDC‐co‐VC) polymer matrix improved the membrane performance in terms of high flux, high BSA rejection ratio, and fouling resistance.     

Strain-induced crystallization kinetics of vinylidene chloride/vinyl chloride (VDC/VC) copolymers

The strain-induced crystallization (SIC) behavior of VDC/VC copolymers has a significant effect on processibility on the blown film process. However, data on SIC of VCD/VC copolymers has been very limited due to the difficulty of measuring the rapid crystallization rates induced by strain; whereas, crystallization under quiescent conditions has been studied extensively. In this work, SIC of VDC/VC copolymers has been calculated from measurements of the adiabatic temperature rise upon stretching of amorphous specimens. The effect of stretching conditions such as strain rate, total strain, and initial temperature and the effect of polymer variables such as copolymer composition, molecular weight, and plasticizer content are determined. It is found that the performance of different VDC/VC copolymers on the film-blowing process correlates much better with measurements of SIC than with quiescent crystallization behavior.     

Stabilization of polymers of vinylchloride with sulfur

The high stabilizing efficiency of element sulfur was revealed by the thermooxidative destruction of polymers of vinylchloride (VC). It was shown that the stabilizing efficiency of sulfur in compositions of polymers of VC is comparable with the efficiency of phenolic antioxidants. Element sulfur inhibits process of autooxidation of esters‐plastifiers of polymers of VC, apparently, because of destruction of formed hydroperoxides. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 4538–4542, 2006     

VC／BA共混物增容PVC／HDPE共混体系的研究

采用氯乙烯—丙烯酸丁酯(VC/BA)共混物作为聚氯乙烯(PVC)/高密度聚乙烯(HDPE)共混物的增容剂,通过冲击实验、拉仲实验、动态力学分析,系统地研究了共混体系性能与其结构之间的关系。通过Brabender流变仪测定了VC/BA共混物增容PVC/HDPE共混体系的流变性能。结果表明,VC/BA共混物是PVC/HDPE共混体系的良好增容剂。在一定范围内,VC/BA共混物与HDPE对PVC有协同增韧效应。vC/BA和HDPE的加入改善了PVC的塑化和流变性能     

硅烷交联聚氯乙烯的制备和性能

对由悬浮共聚合成的氯乙烯／乙烯基三乙氧基硅烷共聚树脂的水解交联行为和交联聚氯乙烯的性能进行了研究。结果发现，通过聚合过程添加pH调节剂可得到凝胶含量很低的氯乙烯／乙烯基三乙氧基硅烷共聚树脂；该类共聚树脂加工后有一定程度交联发生，凝胶含量随共聚树脂中乙烯基三乙氧基硅烷含量增加而增加；当加工样品在水中浸渍后凝胶含量又有较大幅度提高，说明水解交联的发生；交联后PVC高温力学性能和耐热变形性提高。     

Effects of electrolytes on the electrochemical performance of Si/graphite/disordered carbon composite anode for lithium-ion batteries

The influences of LiBF₄, LiClO₄, lithium bis(oxalato) borate (LiBOB), LiPF₆ with VC and without VC, and the mixed electrolytes composed of different ratios of LiBOB and LiPF₆ or LiClO₄ on the electrochemical properties of Si/graphite/disordered carbon (Si/G/DC) composite electrode were systematically investigated by constant current charge-discharge and electrochemical impedance spectra (EIS) techniques. Scanning electron microscopy (SEM) was used to observe the change of electrodes in morphology after given cycle numbers. X-ray photoelectron spectroscopy (XPS) was employed to understand the influences of different mixed electrolytes on the composition of SEI layers. The results showed that Si/G/DC composite electrode in the mixed electrolytes presented better electrochemical performance than in single electrolyte. The compactness and compositions of SEI layers intensively influenced the cycle performance of Si/G/DC composite materials. LiBOB and additive VC had a good synergistic effect on the formation of the dense SEI layers. In particular, Si/G/DC in 0.5 M LiBOB + 0.38 M LiPF₆ electrolytes containing VC exhibited a high reversible capacity and excellent cycle performance.     

Synthesis of random and block copolymers of vinyl chloride and vinyl acetate by RAFT miniemulsion polymerizations mediated by a fluorinated xanthate

Reversible addition–fragmentation chain transfer miniemulsion (co)polymerizations of vinyl acetate (VAc) and vinyl chloride (VC) are conducted in the presence of a fluorinated xthanate (X1). VAc miniemulsion polymerization can be well controlled by X1, and PVAc with small polydispersity index (PDI, <1.20) are obtained. X1 also shows well mediative effect to VC‐VAc miniemulsion copolymerization, while the PDI of VC‐VAc copolymer is greater than that of PVAc since a chain transfer rate to VC is greater than that to VAc. PVAc‐b‐PVC copolymers are synthesized by VC miniemulsion polymerizations mediated by X1‐terminated PVAc. PDIs of PVAc‐b‐PVC copolymers are greater than that of PVAc and VC‐VAc random copolymers with close monomer compositions, and increase with the increase of VC conversion. This is caused by the increased chain transfer to monomer and the formation of monomer‐rich and polymer‐rich phases during the VC polymerization stage. As‐prepared PVAc‐b‐PVC copolymers exhibit a micro‐phase separated morphology. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45074.     

Recent research advances in the chemistry of poly(vinyl chloride)

Summarized briefly here are some new observations that relate to the polymerization chemistry of vinyl chloride (VC) and to the thermal degradation, thermal stabilization, fire retardance, and smoke suppression of poly(vinyl chloride) (PVC). During polymerization, head-to-head VC emplacement leads to β-chloroalkyl radicals that can transfer chlorine atoms directly to VC. Another mechanism for transfer to monomer is responsible, however, for the polymer molecular-weight reductions that occur at high VC conversions. This transfer process involves the abstraction of methylene hydrogen from the polymer by an ordinary macroradical and the subsequent bimolecular donation of a chlorine atom to VC. The propagation steps of the polymerization do not become diffusion-controlled at VC conversions near 90%, and hydrogen abstraction from the polymer by ordinary macroradicals leads to the structural defects that cause thermal instability. The thermal dehydrochlorination of PVC involves ion pairs or four-center concerted transition states that are highly polarized. Reversible thermal stabilization of the polymer by organic metal salts occurs by the Frye-Horst process, and the reductive coupling of PVC chains may suppress both smoke and flame. This coupling can result from reactions of the polymer with zero- or low-valent transition-metal species that are formed in situ from appropriate additives.