去甲氨噻肟酸乙酯合成研究

去甲氨噻肟酸乙酯是半合成头孢菌素药物的重要中间体之一.报道了在环合反应中,采用甲醇和水(体积比为1∶1)的混合溶剂代替二氯甲烷,甲醇等单一溶剂,反应温度在25℃左右下进行,收率明显提高,可达56.2%,结果令人满意.产品结构用1HNMR验证.     

氧化纤维素的制备研究

介绍了氧化纤维素 (DAC)的制备过程 ,用正交法探讨了以NaIO4 作氧化纤维素时反应温度、溶液pH值、氧化剂浓度、反应时间以及交互作用对DAC醛基含量的影响 ,找到了影响醛基含量的主要因素为反应温度、反应温度与NaIO4 的交互作用、反应温度与溶液 pH值的交互作用。初步确定了制备氧化纤维素的反应工艺 ,使醛基含量较高时的最佳反应条件为 :反应温度 3 5℃ ,反应时间 3h ,NaIO4 质量分数 6.78% ,pH值为 2时 ,醛基含量达 68.2 0 %。     

HPLC测定复方氯己定甲硝唑栓中醋酸氯己定、甲硝唑的含量

建立复方氯己定甲硝唑栓中主要成分醋酸氯己定、甲硝唑含量的高效液相色谱测定方法。色谱柱为大连依利特公司HypersilC18柱(20cm×4.6mm,10μm);醋酸盐缓冲溶液(取醋酸铵80g、辛烷磺酸钠2g加水800mL溶解后,用冰醋酸调节pH值至4.2,加水至1000mL)—甲醇(40∶60)为流动相;检测波长:甲硝唑315nm,醋酸氯己定260nm。醋酸氯己定、甲硝唑的回收率分别为99.27%、99.40%,RSD分别为0.57%、0.55%(n=9)。该方法简便,结果准确可靠。     

2,4-D/CMC接枝物纳米粒子的制备与缓释性能研究

以羧甲基纤维素钠（CMC）为基材，甲基丙烯酸甲酯（MMA）和二甲基二烯丙基氯化铵（DMDAAC）为改性单体，通过乳液聚合制备了CMC-g-P(MMA-DMDAAC)共聚物，采用自组装方法负载2,4-二氯苯氧乙酸（2,4-D）得到2,4-D/CMC-g-P(MMA-DMDAAC)纳米药物缓释体系。利用傅里叶红外光谱（FTIR）、差示扫描量热法（DSC）、热重分析（TGA）、扫描电镜（SEM）、粒度分析仪对其结构和形貌进行表征，并探究其载药性能和缓释性能。结果表明，2,4-D/CMC-g-P(MMA-DMDAAC)载药粒子呈笼状结构，粒度分布为160～425 nm；其载药率随着CMC∶MMA∶DMDAAC的摩尔比增大而提高，最高可达40.8%；其药物累计释放率随CMC∶MMA∶DMDAAC的摩尔比增大而降低，其释放行为符合Weibull模型，遵循Fick扩散机理。     

纤维素衍生物液晶相转变和织态结构

本文综述了纤维素衍生物液晶态相转变和织态结构。描述了纤维素衍生物从各向同性态向液晶态的转变过程和液晶态的织构特征。讨论了溶液浓度和温度对液晶相织构的影响。探讨了各种因素,如溶剂、取代基含量、外加力场和外加磁场等对液晶相的形成及织态结构的影响。     

铌酸催化合成乙酸苯乙酯

将铌酸用于催化合成乙酸苯乙酯 ,在醇酸摩尔比 1∶5 ,回流反应 2h ,催化剂用量 (以 1mol醇计 )为 5g的条件下 ,酯收率可达 84 .3%以上。催化剂不经处理 ,可多次循环使用 ,不污染环境 ,相对于一些其他催化剂 ,具有明显的优点。     

乙酸苄酯的合成新工艺研究

报道了合成乙酸苄酯的新工艺 ,以有机溶剂丙酸丁酯作为反应介质 ,三乙胺为催化剂 ,合成了乙酸苄酯。产品收率可达 99 1%,产品纯度 >99 5 %,溶剂可反复回收使用。     

Infrared study of salt free and salt treated cellulose pyrolysis under nitrogen atmosphere

The pyrolysis under nitrogen of salt free and salt treated cellulose was studied by infrared spectroscopy. The results confirm the unzipping mechanism suggested by DTA and TGA studies, and show this mechanism to apply to the untreated and salt treated samples. The results also show the unzipping to stop at the stage of char formation. The onset of this stage was found to occur after the volatilization of only 45–50% of the initial sample of the borax treated cellulose, compared with 65–70% of the KCl treated cellulose and 80–85% of the untreated cellulose.     

End-capped polystyrene with 8-hydroxyquinoline group by ATRP method

8-Hydroxyqunioline end-capped polystyrene was prepared through atom transfer free radical polymerization (ATRP) with 8-(5-chloromethyl) quinolyl acetate as initiator. The results indicated that this polymerization is a first order reaction with respect to monomer conversion. The molecular weight increased linearly with monomer consumption and very narrow distribution of molecular weight was obtained (polydispersity index less than 1.2). The FT-IR and NMR results show that the 8-hydroxyquinloine group was chemically bonded to the polymer end and there is nearly one 8-hydroxyquinoline group in per polymer chain. All those data show that polymerization of styrene at such conditions displayed living characters. The polymer with 8-hydroxyqquinoline end group reacted with triethylaluminum to form polymeric light-emitting complex and single layer LED was prepared by common spin-coating method. The peak wavelength of LED based on synthesized polymeric complex was around 570 nm.     

纤维素醚的特点、制备及在工业中的应用

综述了纤维素醚的种类、制备方法、性能和特点,以及纤维素醚在石油、建筑、造纸、纺织、医药、食品、光电材料及日化工业中的应用,介绍了一些具有发展前景的纤维素醚类衍生物的新品种并展望其应用前景。