聚醚酮酮（PEKK）／4，4′-二苯氧基二苯砜（DPODPS）多嵌段共聚物的合成与性能

采用溶液缩聚法由酰氯端基聚醚酮酮(PEKK)齐聚物和4，4′-二苯氧基二苯砜(DPODPS)制备了PEKK／DPODPS多嵌段共聚物，用DSC、TGA等方法对共聚物进行了表征和性能测试。结果表明，随着共聚物中DPODPS含量的增加，共聚物的熔融温度逐渐降低，而其玻璃化转变温度则逐渐升高。当DPODPS质量分数在32．63％～40．73％范围内时，所得共聚物的Tg为185～193℃，比纯PEKK的Tg高出20～28℃；其Tm为322～346℃，比纯PEKK的Tm降低35～59℃，这既保持了纯PEKK的耐热性，又改善了熔融加工性能。该组成范围内的共聚物的拉伸强度(σi)为86．6～84．2MPa，拉伸模量(M)为3．1～3．4GPa，断裂伸长率(ε)为18．5％～20．3％。     

小分子胺直接有效催化合成α-苯硒基酮

用有机小分子胺, 如辛可尼啶, L-脯胺酸和N-取代的手性1,2-环己二胺等直接催化酮与苯硒基氯反应, 通过这一简单有效的方法, 高收率合成了一些α-苯硒基酮.     

磁场对含稀土铝锂合金断裂特征的影响

以含铈铝锂合金为研究对象，研究了磁场对含稀土铝锂合金时效过程的影响，从断裂特征及微观组织两方面分析了磁场作用规律。实验结果表明：未加磁场时，合金的断裂特征以理断裂为主；扁平晶粒厚度不匀，在磁场作用下，此合金的断裂特征与微观组织发生明显改观，随磁感应强度增强，合金主断裂面上准解理断裂特征减弱，同时二次裂纹增多，分层比较升高；扁平晶粒厚度变薄，尺寸趋于均匀。用少体物理理论，探讨了磁场对含稀土合金原子扩散过程的影响，为进一步研究稀土元素在磁场中的行为及其局域效应提供了一定的实验依据。     

Brnsted酸性离子液体催化醛(酮)与二元醇的缩合反应

研究了以Bro¨nsted酸性离子液体1-正丁基-3-甲基咪唑磷酸二氢盐(BMImH2PO4)为催化剂,在不使用其它有机溶剂且无需脱水的条件下,于室温下进行醛(酮)与二元醇的缩合反应,得到了由中至高的转化率和高选择性.产物1,3-二口恶戊烷可以和反应物自动分层,后处理操作简单.过量的醇与离子液体可以多次重复使用,且醛(酮)的转化率无明显降低.     

Synthesis and Characterization of Novel Organosoluble Methyl Substituted Poly(aryl Ether Ketone)s Containing Sulfone Linkage

Several new methyl substituted poly(aryl ether ketone)s containing sulfone linkage with inherent viscosities of 0.62–0.84 dL/g have been prepared from 4,4′‐bis(2‐methylphenoxy)diphenylsulfone and 4,4′‐bis(3‐methylphenoxy)diphenylsulfone with terephthaloyl chloride and isophthaloyl chloride by electrophilic Friedel‐Crafts acylation in the presence of DMF with anhydrous AlCl₃ as a catalyst in 1,2‐dichloroethane, respectively. These polymers having weight‐average molecular weight in the range of 71,000–49,000 are all amorphous and show high glass transition temperatures ranging from 167 °C to 191 °C, excellent thermal stability at temperatures over 400 °C in air or nitrogen, high char yields of 51–58% in nitrogen and good solubility in CHCl₃ and polar solvents such as DMF, DMSO and NMP at room temperature.     

Arsenic Speciation in Urine and Blood Reference Materials

Acute and chronic exposure to arsenic is a growing problem in the industrialized world. Arsenic is a potent carcinogen and toxin in humans. In the body, arsenic is metabolized to produce several species, including inorganic forms, such as trivalent (As^III) and pentavalent (As^V), and the methylated metabolites such as monomethylarsonic acid, (MMA^V), and dimethylarsinic acid (DMA^V), in addition to arsenobetaine (AsB) which is ingested and excreted from the body in the same form. Each of these species has been reported to possess a specific but different degree of toxicity. Thus, not only is the measurement of total As required, but also quantification of the individual metabolites is necessary to evaluate the toxicity and risk assessment of this element. There are a large number of reference materials that are used to validate methodology for the analysis of As in blood and urine, but they are limited to total As concentrations. In this study, the speciation of five arsenic metabolites is reported in blood and urine from commercial available control materials certified for total arsenic levels. The separation was performed with an anion exchange column using inductively coupled plasma mass spectrometry as a detector. Baseline separation was achieved for As^III, As^V, MMA^V, DMA^V, and AsB, allowing us to quantify all five species. Excellent agreement between the total arsenic levels and the sum of the speciated As levels was obtained.     

哺乳妇女血、乳中三种元素含量检测

研究了哺乳期母体内血、乳中锌、铁、钙三种元素含量的检测。探讨了用一定量的基体释放剂，取少量血液、乳液经大倍数稀释，直接于原子吸收仪上进行测定。此法快速、准确、实用。     

铜催化下格氏试剂与酰卤的选择性偶合: 直链酮化合物的合成

在一般情况下,格氏试剂与酰卤偶合反应难以控制在酮阶段,往往得到叔醇。在较低温度下有机铜试剂与酰卤偶合可高产率地得到酮,所以用固体铜盐CuX(X=Cl、Br、I)作为格氏试剂与酰卤偶合的催化剂,可以提高反应的选择性,从而提高酮的产率。但固体铜盐的催化反应仅适合于空间位阻较大的脂肪酮和某些芳香酮的制备,对于直链脂肪酮的制备则产率很低。我们采用可溶性铜络合物Li_2Cucl_4(四氯合铜酸锂)等作催化剂,在均相溶液中反应,有效地提高了催化效果及反应的选择性,从而使格氏试剂与酰卤的偶合反应成功地用于直链脂肪酮的制备,产率良好。     

二苄基二茂钛的羰基化反应

用取代的二苄基二茂钛与一氧化碳在正庚烷中反应,生成二羰基二茂钛和二苄基甲酮。通过光谱监测,发现1摩尔一氧化碳插入碳钛键,得到取代的苯乙酰基苄基二茂钛。反应随着取代基给电子能力的增加而加快(Me>t-Bu≈H>F>Cl)。中间体Cp_2Ti[C(O)CH_2Ph]CH_2Ph很活泼,迅速发生分子内消除,消除的苄基和苯乙酰基生成二苄基酮。