十六醇磷酸酯合成工艺研究

研究了十六醇磷酸酯的合成工艺,采用加水反应和水解工艺制取单烷基磷酸酯,考察了十六醇与五氧化二磷(P2O5)的摩尔比、反应时间、反应温度、水解等因素对转化率和单烷基磷酸酯质量分数的影响。得到的优化工艺条件为:酯化反应阶段,十六醇、P2O5及水的摩尔比为1.70∶1.00∶1.13,85℃下反应10 h;水解反应阶段,加水量为磷酸酯质量的4%,85℃,水解2 h。结果表明,所得的十六醇磷酸酯白度较好,产物单酯的质量分数>78%、酯化率>85%、单酯率>90%。     

固体酸SO4(2-)/Nb2O5催化合成尼龙酸二异丁酯

研究了SO4^2-／Nb2O5作为催化剂催化合成尼龙酸二异丁酯的反应。通过正交试验确定了最佳反应条件：酸醇物质的量比为1：2．5，催化剂为反应物总量的0.35％，反应回流2．0h，在此条件下酯化率可达97．8％。     

苯乙酸合成新工艺

应用氯化钴和低价含硫化合物低压合成四羰基钴盐的技术于氯苄羰化合成苯乙酸的生产工艺中。结果表明甲醇水溶剂系统有利于低压合成四羰基钴盐；氢氧化钙作中和剂使用，要求羰化产物后处理的温度提高，以保证苯乙酸的产率；碱的用量和浓度是影响苯乙酸产率的重要因素。     

Aphid deterrence by glucose esters in glandular trichome exudate of the wild tomato,Lycopersicon pennellii

Settling of the potato aphid,Macrosiphum euphorbiae, on feeding membranes was deterred by methanolic leaf rinses ofLycopersicon pennellii, or of its F₁ with tomato,L. esculentum. The active compounds in theL. pennellii rinsates were identified as 2,3,4-tri-O-acylglucoses bearing short to medium chain length fatty acids. These compounds are localized in the glandular exudate of the type IV trichomes and may accumulate to levels in excess of 400 g/cm². In choice assays, purified glucose esters fromL. pennellii reduced aphid settling at concentrations as low as 25 g/cm²; at concentrations of 150 g/cm² or more, all aphids avoided treated areas. Glucose esters were also active in deterring aphid settling in no-choice assays. At 100 g/ cm², these esters resulted in increased levels of mortality after 48 hr.     

负载型磷钨酸催化杂醇油合成混合酯的研究

本实验以杂醇油和乙酸为原料，杂多酸HPW／MxOy为催化剂。在相同条件下将几种工艺进行比较，从而选出适合该酯化反应的工艺。同时考察了催化剂的用量、醇酸酯比、反应时间等对酯化反应的影响。并研究了杂多酸的重复使用性。确定了酯化率和酯含量最佳时的酯合成反应的工艺条件。     

氰酸酯树脂的性能与应用

氰酸酯树脂具有较低的介质损耗因数和低而稳定的介电常数，使用频带宽，力学性能好，吸水率低，是新一代航空航天雷达天线罩理想的基体材料。介绍了该树脂的制备途径、性能和应用，并指出合成中应注意的问题。     

Effects of reaction and cure temperatures on morphology and properties of poly(ester‐urethane)

Poly(ester‐urethane) was synthesized from poly(ethylene glycol adipate) (PEG) and 2,4‐toluene diisocyanate (TDI) to study the effects of reaction temperature and cure temperature on the crystallization behavior, morphology, and mechanical properties of the semicrystalline polyurethane (PU). PEG as soft segment was first reacted with TDI as hard segment at 90, 100, and 110°C, respectively, to obtain three kinds of PU prepolymers, coded as PEPU‐90, PEPU‐100, and PEPU‐110. Then the PU prepolymers were crosslinked by 1,1,1‐tris (hydroxylmethyl) propane (TMP) and were cured at 18, 25, 40, 60, and 80°C. Their structure and properties were characterized by attenuated total reflection Fourier transform infrared, wide‐angle X‐ray diffraction, scanning electron microscopy, dynamic mechanical analysis, and tensile testing. With an increase of the reaction temperature from 90 to 100°C, the crystallinity degree of soft segment decreased, but interaction between soft and hard segments enhanced, leading to the increase of the glass transition temperature (T_g) of soft domain and tensile strength. When the cure temperature was above 60°C, miscibility between soft and hard segments of the PEPU films was improved, resulting in relatively low crystallinity and elongation at break, but high soft segment T_g and tensile strength. On the whole, all of the PEPU‐90, PEPU‐100, and PEPU‐110 films cured above 60°C possessed higher tensile strength and elongation at break than that of the films cured at other temperatures. The results revealed that the reaction temperature and cure temperature play an important role in the improvement of the crosslinking structure and mechanical properties of the semicrystalline PU. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 708–714, 2006     

2-氯甲基-4-甲氧基-3,5-二甲基吡啶盐酸盐的合成

2,3,5 三甲基吡啶用双氧水/冰醋酸氧化制得2,3,5 三甲基吡啶 N 氧化物,收率91%;该氧化吡啶与发烟硝酸/浓硫酸反应得4 硝基 2,3,5 三甲基吡啶 N 氧化物,收率80 4%;将其与甲醇钠反应得到4 甲氧基 2,3,5 三甲基吡啶 N 氧化物,收率91%;4 甲氧基 2,3,5 三甲基吡啶 N 氧化物与乙酸酐反应得到2 乙酰基氧甲基 4 甲氧基 3,5 二甲基吡啶,收率66 6%;2 乙酰基氧甲基 4 甲氧基 3,5 二甲基吡啶在碱性条件下水解得2 羟甲基 4 甲氧基 3,5 二甲基吡啶,收率93%;再用氯化亚砜氯代制得2 氯甲基 4 甲氧基 3,5 二甲基吡啶盐酸盐,收率90 6%。通过TLC、IR、1HNMR对产物进行了表征。     

N－氰基乙亚胺酸乙酯含量的气相色谱分析

采用GC-900气相色谱仪、3%PEG-12000/Chromosorb880AWDMCS填充柱和FID检测器,以水杨酸甲酯为内标物测定N-氰基乙亚胺酸乙酯含量,回收率在98.5%—101.8%之间,标准偏差为0.27%,变异系数为0.27%。     

盐酸小檗碱-环糊精包合物的体外溶出度研究

目的探讨包合技术对中药制剂体外溶出度以及缓释作用的影响。方法选用饱和溶液法生成包合物 ,用DSC证明包合物的生成 ;采用分光光度法 ,考察盐酸小檗碱包合物的体外溶出度和缓释作用。结果 β CD·BH、RM β CD·BH和BH的T50 、Td分别为 5 69.8,740 .2min ;73 .7,10 7.0min和 19.6,2 5 .5min ,包合物的释药数据与t作线性回归方程为 :Y =0 .0 63 9t -0 .473 8,Y =0 .5 5 64t+5 .65 8。结论RM β CD·BH和 β CD·BH的溶出速率明显慢于BH ,具有一定的缓释作用 ,同时RM β CD·BH较β CD·BH具有更好的生物利用度 ;β CD·BH和β CD·BH的体外溶出度与t为一相关性良好的线性方程 ,符合零级释药方程。