SYNTHESIS OF DBN AND ITS CATALYTIC PERFORMANCE FOR METHANOL CARBONYLATION TO METHYL FORMATE

1 , 5-diazabicyclo['1, 3, 0]non-5-ene(DBN) has been synthesized in our laboratory, and its catalytic activity and selectivity for methanol carbonylation to methyl formate (MF) have been studied. The experimental results have demonstrated that the synthetic processes of DBN used for the present work are reasonable and feasible. The total yield of three steps of DBN synthsis is approximate to 80%. The activity evaluation has shown that DBN can effectively catalyze the carbonylation reaction of methanol in the presence of propylene oxide (PO) promoter. PO-promoted DBN is a novel catalytic system superior to sodium methoxide.     

南瓜籽烘烤前后化学成分的分析

对烘烤前后南瓜籽中的化学成分进行分析并对比。采用同时蒸馏萃取装置萃取南瓜籽中的挥发性成分,采取超临界CO2萃取技术萃取南瓜籽油脂,并将其分为酸、碱、中性三个部分,用气相色谱-质谱联用方法分析其中化学成分并进行对比。结果表明,南瓜籽挥发性成分中含有多种醛类和酯类化合物,烘烤后产生了大量的烷基吡嗪,其在碱性部分中的相对含量比烘烤前提高14倍多,不饱和醛类化合物含量也有明显提高。南瓜籽油脂中的主要化学成分是油酸、亚油酸及其酯类。还含有生物活性功能成分如植物甾醇、角鲨烯和维生素E等。烘烤后除角鲨烯含量有所降低,维生素E、植物甾醇、亚麻酸等均有提高。     

水热法合成的MoVTeNbOx多组分氧化物催化剂上异丁烷的选择氧化

采用水热法合成了MoVTeNbOx多组分氧化物催化剂, 并用XRD, ICP, BET和SEM等方法对催化剂进行了表征, 考察了MoVTeNbOx多组分氧化物催化剂的组成、反应温度和空速对异丁烷选择氧化反应性能的影响. 其中组成为MoV0.3Te0.17Nb0.12Ox的催化剂显示出最好的催化活性和选择性, 在673 K下, 异丁烷的转化率为10.8%, 甲基丙烯醛(MAL)和甲基丙烯酸(MAA)的收率累积达到6.5%.     

通过三乙基铝促进的a-羟基环氧化合物的重排还原反应合成Madindoline母核片断——全取代环戊烯二酮单元

The fully substituted cyclopentenedione core of madindoline A （1） and B （2） as potent and selective inhibitor of IL-6 has been synthesized efficiently. The quaternary carbon center C-2＇ was constructed on the basis of a newly developed AIEt3-promoted tandem reductive rearrangement of α-hydroxy epoxides.     

超声波辐射下合成N-取代苯并噻唑-2-氨基-N'-取代吡唑-4-甲酰基硫脲

为实现多种活性成分的有效叠加和为药物筛选提供先导化合物, 以1-苯基-3-甲基-5-氯/苯氧基-4-吡唑甲酸为初始原料, 依次合成1-苯基-3-甲基-5-氯/苯氧基-4-吡唑甲酰氯、1-苯基-3-甲基-5-氯/苯氧基-4-吡唑甲酰基异硫氰酸酯, 再与取代苯并噻唑肼反应生成了8个未见报道的N-取代苯并噻唑-2-氨基-N'-取代吡唑-4-甲酰基硫脲. 采用超声波催化法合成了标题化合物, 并与加热回流的常规方法进行了对比. 超声波催化法具有操作简单、反应时间短、条件温和、产率高、副反应少等优点, 为此类化合物的合成提供了一种有效的新方法. 标题化合物经元素分析, IR, ¹H NMR确证结构.     

多步法制备纳米钛酸钡

采用醋酸钡、碳酸钾、钛酸丁酯等为初始反应物，通过多步反应的方法，制得了纳米钛酸钡。所得产品采用XRD、TEM和SEM等进行了表征，并对生长机理进行了分析。研究结果表明，得到的碳酸钡为直径约100 nm的纳米棒，再经室温下钛酸丁酯水解产生二氧化钛对碳酸钡纳米棒进行包覆，可得到一维核-壳结构的碳酸钡/二氧化钛，最后于700 ℃下经固相反应而得到钛酸钡的纳米颗粒。这种制备纳米钛酸钡的方法可以有效地控制产品形貌及粒径。     

Synthesis and X-ray crystal structure of oxamido-bridged heterobinuclear Ni(Ⅱ)-Cu(Ⅱ) complexes

The two complexes [Ni(oxen)Cu(L)2](ClO4)2.xH2O (L=2,2'-bipyridyl(bpy), 1,10-phenanthroline(phen)) have been synthesized, where oxen is N,N'-bis(2-aminoethyl)oxamido di-anion. The crystal structure of [Ni(oxen)Cu(bpy)2](ClO4)2.CH3OH has been determined by X-ray diffraction method. The crystal is triclinic system, space group P1 with a=12.179(1),b=12.298(2), c=11.476(2) A, a=97.57(1), B=97.52(1), 7=80.29(2), V=1669.04(67) A3, Z=2, Dcalcd=1.667 g/cm3. The structure has been refined to final R of 0.076 and Rw of 0.080, respectively. The complexes have an extended oxamido-bridged structure and consist of Ni(Ⅱ) ion in a square planar environment and Cu(Ⅱ) ion in a distorted octahedral environment.     

环氧化橡胶及其合金的研究与应用

综述了国内外环氧化橡胶及其合金的研究现状和应用趋势,重点介绍了环氧化天然橡胶、环氧化聚丁二烯、环氧化苯乙烯-丁二烯-苯乙烯三嵌段共聚物及其合金的优点,以及影响其物理机械性能的因素和环氧化橡胶的发展方向。     

GAS SORPTION AND TRANSPORT IN POLY (PHENYLENE OXIDE)(PPO)AND ARYL-BROMINATED PPO MEMBRANES

The apparent solubility (S), concentration-average diffusivity (D), and permeability (P), for C0_2, CH_4 and N_2 through PPO and aryl-brominated PPO at 35℃for pressure ranging from 1 to 26 atm are reported. It is found that P, D, and S of the membranes to all the three gases vary with the extent of bromination. S increases with the increase of the percent of bromine in each case, but D to CO_2 increases remarkably only at higher degree of brominafion, and therefore, P to CO_2 is increased by more than 100% over a wide range ofpressure in the case. The solubility data are well described by the dual mode sorption model. It is found that the gas molecules sorbed by the Langmuir mode are relatively more immobilized and the contribution of the nonequilibrinm character of the polymer to gas permeation increases obviously for CO_2 and is hardly changed for CH_4 with increasing bromine content. These observations are interpreted in terms of changes in specific free volume (SFV)and the cohesive energy density (CED) of the polymers.     

镁修饰丝光沸石对萘异丙基化选择性的影响

2，6-二异丙基萘是制备高级聚酯材料PEN和液晶聚合物的原料。用择形催化剂丝光沸石代替传统的Friedel—Crafts催化剂，在高压釜中以萘和丙烯为原料经异丙基化反应合成了2，6-DIPN。采用浸渍法用少量镁盐修饰水汽脱铝氢型丝光沸石（SDHM），减少了SDHM外表面的强B酸中心和非择形产物的生成，从而使2，6-DIPN的择形率提高到71％。2，6-DIPN／2，7-DIPN摩尔比达到2．89，有利于2，6-DIPN的分离提纯。