正交回归多元标准加入光度法同时测定UF_4中杂质镍,镉,锌

采用正交回归多组分标准加入光度法 ,在二甲酚橙 -CTMAB -硼砂显色体系中 ,同时测定了核燃料UF4中微量杂质镍、镉和锌 ,实验工作量少 ,结果可靠 ,三种组分的测定误差不大于 4% ,回收率为97%～ 1 0 3%。     

高温固硫添加剂的选择研究

根据煤中硫在不同温度下的释放特性,通过室内试验对不同固剂、添加剂进行选择性研究,重点研究了添加剂在高温下的固疏情况,并对其合成工艺、适应性、稳定性进行了研究,介绍了工业性试验及工业推广应用情况,并对固硫原理作了初步分析。     

活性添加剂对硫酸钙结晶过程的影响

研究反应温度、酸浓度、溶剂浓度及搅拌速度对硫酸钙结晶过程的影响;在溶剂中加入活性添加剂后,硫酸钙的溶解度增大,晶形由细长瓦楞状变成了粗大棱柱状.     

N-苯基马来酰亚胺改性酚醛树脂的合成及其结构性能

采用滴加苯酚的方式合成了N-苯基马来酰亚胺改性酚醛树脂（PPMF）, 考察了N-苯基马来酰亚胺（PMI）参与酚醛缩聚反应的转化程度和树脂黏度特性的变化规律.发现延长苯酚滴加时间能提高PMI参与共缩聚反应的竞争能力和转化率;随着回流反应时间的增加,PMI转化率增加,树脂的黏度也随之增大;较高的反应温度或较大的PMI用量均会导致PMI转化率的显著下降.利用核磁、红外和元素分析等表征了改性酚醛树脂的结构及组成,确定N-苯基马来酰亚胺已共缩合于酚醛树脂中,其中PMI含量可达33％左右.利用DSC和TGA研究了N-苯基马来酰亚胺改性酚醛树脂的固化特性和耐热性能,发现PPMF树脂经历了两个固化阶段, 第一阶段是少量羟甲基的缩合, 第二阶段为马来酰亚胺的双键打开自交联形成. PPMF树脂固化产物的耐热性能优于传统的热塑性酚醛树脂.     

Highly Stereoselective Synthesis of Novel Multistereogenic Bis‐Bifunctional Ligands Based on [2.2]Paracyclophane‐ 4,7‐quinone,their Structure Elucidation and Application in Asymmetric Catalysis

Bis‐bifunctional cis‐4,7‐diarylsubstituted‐4,7‐dihydroxy‐4,7‐dihydro[2.2]paracyclophanes 3–6 were synthesized by a highly diastereoselective reaction of ortho‐substituted aryllithium reagents with [2.2]paracyclophane‐4,7‐quinone ( 1 ). Enantiomerically pure diols 3–5 were tested as chiral inductors in the enantioselective addition of diethylzinc to benzaldehyde (up to 93.5% ee). Acid dehydration of cis‐4,7‐di(2‐methoxyphenyl)‐4,7‐dihydroxy‐4,7‐dihydro[2.2]paracyclophane ( 3 ) results in 4,7‐dihydro‐7,8‐di(2‐methoxyphenyl)[2.2]paracyclophane‐4‐one ( 8 ) – a planar chiral cyclohexadienone of the [2.2]paracyclophane series with a para‐semiquinoid substructure. X‐Ray investigations of compounds 3, 4 and 8 were performed.     

Asymmetric 1,4‐Addition of Diethylzinc to Cyclic Enones Catalyzed by Cu(I)‐Chiral Sulfonamide‐Thiophosphoramide Ligands and Lithium Salts

The chiral sulfonamide‐thiophosphoramide ligand L1 , prepared from the reaction of (1R,2R)‐(−)‐1,2‐cyclohexanediamine with diphenylthiophosphoryl chloride and p‐toluenesulfonyl chloride, was used as a chiral ligand in Cu(MeCN)₄ClO₄‐promoted catalytic asymmetric addition of diethylzinc to cyclic enones using LiCl as an additive in which up to 90% ee can be realized under mild conditions within 0.5 h. This chiral ligand is stable and recoverable after usual work‐up and can be reused in the same catalytic asymmetric reaction. Moreover, it was found that this series of chiral ligands represents a type of S,O‐bidentate ligands on the basis of ¹H NMR, ³¹P NMR and ¹³C NMR spectroscopic investigations. The linear effect of ligand ee and product ee further revealed that the active species is a monomeric Cu(I) complex bearing a single ligand.     

A Convenient Synthesis of β‐Phenylselenocarbonyl Compounds by In‐TMSCl Promoted Cleavage of Diphenyl Diselenide and Subsequent Michael Addition

A simple and convenient procedure has been developed for the synthesis of β‐phenylselenocarbonyl compounds by a one‐pot reaction of diphenyl diselenide and α,β‐unsaturated ketones, aldehydes, esters and nitriles in the presence of indium metal‐trimethylsilyl chloride under sonication. Presumably, the In‐TMSCl reagent system reacts with diphenyl diselenide to form an intermediate, PhSeSiMe₃, which then undergoes Michael addition with the α,β‐unsaturated carbonyl compounds to produce the products.     

Cyanation of N‐Acylhydrazones with Trimethylsilyl Cyanide Promoted by a Brønsted Base and a Lewis Acid

Cyanation of N‐acylhydrazones using trimethylsilyl cyanide (TMSCN) proceeded well in the presence of an amine to afford the corresponding α‐hydrazinonitriles in high yields. For less reactive substrates, the combined use of an amine and a catalytic amount of scandium triflate [Sc(OTf)₃] was effective to promote the reactions. The mechanistic study suggested that the amine worked as a Brønsted base.     

引气剂的应用技术研究

虽然应用引气剂的技术经济效益重大,由于施工技术员对应用技术掌握不够,影响了引气剂的广泛应用,本文对引气剂的作用机理、应用范围、使用方法作了较详细的论述。     

Al2O3掺杂ZnO压敏陶瓷的晶粒生长研究

研究了Al2O3掺杂对ZnO压敏陶瓷晶粒生长规律的影响,应用晶粒生长动力学方程确定了晶粒生长的动力学指数和激活能.实验结果表明,对于Al2O3掺杂ZnO压敏陶瓷,其晶粒生长的动力学指数n等于4,激活能Q等于(400±26)kJ/mol.Al2O3掺杂ZnO压敏瓷的晶粒生长机理是ZnAl2O3尖晶石颗粒在ZnO压敏瓷晶粒边界钉扎过程中Al3+和O2-通过ZnAl2O4尖晶石的扩散.