Anionic copolymerization of [60]fullerene with styrene initiated by sodium naphthalene

The novel C₆₀–styrene copolymers with different C₆₀ contents were prepared in sodium naphthalene-initiated anionic polymerization reactions. Like the pure polystyrene, these copolymers exhibited the high solvency in many common organic solvents, even for the copolymer with high C₆₀ content. In the polymerization process of C₆₀ with styrene an important side reaction, i.e., reaction of C₆₀ with sodium naphthalene, would occur simultaneously, whereas crosslinking reaction may be negligible. ¹³C-NMR results provided an evidence that C₆₀ was incorporated covalently into the polystyrene backbone. In contrast to pure polystyrene, the TGA spectrum of copolymer containing ∼ 13% of C₆₀ shows two plateaus. The polystyrene chain segment in copolymer decomposed first at 300–400°C. Then the fullerene units reptured from the corresponding polystyrene fragments attached directly to the C₆₀ cores at 500–638°C. XRD evidence indicates that the degree of order of polymers increases with the fullerene content increased in terms of crystallography. Incorporation of C₆₀ into polystyrene results in the formation of new crystal gratings or crystallization phases. In addition, it was also found that [60]fullerene and its polyanion salts [C₆₀ⁿ⁻(M⁺)_n, M = Li, Na] cannot be used to initiate the anionic polymerization of some monomers such as acrylonitrile and styrene, etc.© 1998 John Wiley & Sons, Inc. J. Polym. Sci. B Polym. Phys. 36: 2653–2663, 1998     

半导体凝固点测定仪的研制及其应用

为了配合物理化学实验“凝固点降级法测定萘的摩尔质量”,研制出半导体制冷凝固点测定仪,实现了凝固点测定和摩尔质量计算的自动化,解决了老式实验装置存在的问题。通过对环己烷凝固点和萘摩尔质量的测定,验证了该仪器的可靠性,同时还探讨了搅拌速率和冷阱的温度变化对凝固点测定值的影响。     

2,6-萘二甲酸二甲酯与一些二甲基萘所形成的激基复合物

2,6-萘二甲酸二甲酯与一些二甲基萘可以形成激基复合物。本文通过稳态和动态荧光光谱研究了这类激基复合物的形成与分子结构的关系。结果表明,尽管这些二甲基萘的电离能基本相同,但因取代基位置不同使分子中电荷分布不同,从而影响了激基复合物的形成能力。     

Synthesis and properties of aromatic polyamides derived from 1,7-bis(4-aminophenoxy)naphthalene and various aromatic dicarboxylic acids

A series of novel bis(phenoxy)naphthalene-containing polyamides having inherent viscosity up to 2.02 dL/g were synthesized by the direct polycondensation of the diamine 1,7-bis(4-aminophenoxy)naphthalene with various aromatic dicarboxylic acids in N-methyl-2-pyrrolidone (NMP) using triphenyl phosphite and pyridine as condensing agents. Most of the polyamides could be readily dissolved in polar aprotic solvents such as N,N-dimethylacetamide and NMP, and could be solution-cast into transparent, flexible, and tough films. These polymers had glass transition temperatures in the range of 139–263°C, and 10% weight loss temperatures in nitrogen and air were above 499 and 484°C, respectively. © 1996 John Wiley & Sons, Inc.     

沸石分子筛催化剂上萘的择形异丙基化反应性能

 研究了HY,Hβ,HM和HZSM－5沸石分子筛对萘择形异丙基化反应的催化性能．结果发现,这些沸石分子筛的活性顺序为HY＞Hβ＞HM＞HZSM－5,对2,6－二异丙基萘的选择性顺序为HM＞Hβ＞HY．除沸石分子筛的酸量与酸分布外,其孔道结构与大小是影响萘异丙基化反应的主要因素．脱铝能选择性地降低沸石外表面的酸性,且对沸石的催化性能有较大影响．常压水蒸气脱铝结合强酸再处理有利于催化剂催化性能的提高．提高反应温度有利于萘的转化,但温度过高会引发许多副反应,适宜的反应温度约为523K．反应时间对产物分布的影响不明显．异丙醇／萘摩尔比应小于2．     

氯化铜对6-甲氧基-2-酰基萘选择性氯化反应

甲氧基酰基萘;甲氧基萘;氯化铜对6-甲氧基-2-酰基萘选择性氯化反应     

以工业萘和粗甲基萘为主要原料合成萘系高效减水剂

工业萘、粗萘、甲基萘或萘残油等均可作为制取萘高效减水剂的原料。目前 ,其主要原料工业萘出现全球性紧缺 ,价格不断上扬[1] 。而攀枝花粗甲基萘比工业萘便宜许多 ,如果能用粗甲基萘代替工业萘生产萘系高效减水剂 ,可降低成本 ,使之具有更大的市场竞争力。前期实验表明单独使用粗甲基萘制备的减水剂 ,其减水率虽然较高 ,但产品含气量较大且引气不均匀 ,使混凝土抗压强度达不到要求。为了将工业萘和粗甲基萘混合物作为原料制备高效减水剂 ,并尽量用粗甲基萘替代工业萘 ,我们做了大量的实验 ,寻求到了工业萘和粗甲基萘混合物作为原料制备高效…     

1,4-双(4′-N,N-二甲基氨基苯乙烯基)萘的合成及荧光性质

利用Wittig反应合成了一个以萘为π-Center的对称型“D-π-D”有机绿色发光化合物1,4 双(4′-N,N-二甲基氨基苯乙烯基)萘(BDASN),并测试了其在不同环境中的光谱性质.在378nm激发波长的激发下,BDASN显示出很强的荧光发射峰,峰位在521nm(CH₂Cl₂).随着溶剂极性增大,最大发射波长红移且荧光强度降低,与“D-π-A”分子具有相似的分子内电荷转移(TICT)行为.在β-环糊精(β-CD)中BDASN的绿色发光带被猝灭,同时在450nm附近蓝发光带的荧光强度骤增.     

气相色谱法检测大孔吸附树脂中的有机残留物

建立了同时检测大孔吸附树脂中苯、甲苯、二甲苯、苯乙烯、二乙苯、二乙烯苯、萘、癸烷、十一烷和十二烷等10种有机残留物的测定方法。以二氯甲烷为提取溶剂,采用超声提取法对样品进行前处理。采用气相色谱法检测,色谱柱为DB-624毛细管柱,检测器为氢火焰离子化检测器。上述10种有机残留物在12 min内能很好地分离,样品的加标回收率(n=3)为73.8%～107.9%,相对标准偏差为1.3%～4.4%,最低检测限为0.007～0.03 mg/L。本方法具有灵敏、准确、快速等特点。对9种商品树脂及其预处理品的有机残留物进行了测定,结果表明树脂预处理前后有机残留物的含量相差很大,经过预处理的树脂可以安全地应用于中药的生产。     

超分子体系强的分子识别研究 23: 多胺修饰β-环糊精及其铜 配合物与萘衍生 物的包结配位作用

用荧光光谱滴定法测定了单-[6-(二乙烯三胺)-6-脱氧]-β-环糊精(1)、单-[6-(三乙烯四胺)-6-脱氧]-β-环糊精(2)及其铜配合物(3,4)与一系列萘衍生物在磷酸缓冲溶液(pH7.2,0.1mol.dm^-^3)中,25℃时形成超分子体系的稳定常数,并与母体β-环糊精的配位能力进行了比较。化学计量法表明,四种化学修饰β-环糊精与萘衍生物形成了1:1的超分子配合物。从尺寸适合、几何互补及多点识别等方面讨论了主体化合物对模型底物的分子选择性键合能力。结果表明,疏水相互作用、范德华力、静电相互作用及氢键等多种非共价键弱相互作用协同贡献于超分子配合物的形成,主-客体间的结构匹配在分子受体选择性键合底物形成超分子配合物中起重要作用。