阿折地平的合成及其结晶的研究

对阿折地平的合成工艺进行了研究,设计了一条适合于工业化生产的合成路线。以(1-二苯甲基-3-吖丁啶醇)脒基乙酸酯乙酸盐(Ⅲ)和2-(3-硝基苄叉)乙酰乙酸异丙酯(Ⅳ)为原料通过麦克加成得产品阿折地平(Ⅴ),产物收率86%,产品纯度大于99.5%。其中原料(Ⅲ)和(Ⅳ)可通过其它原料的合成得到,由乙酰乙酸异丙酯和间硝基苯甲醛可得原料(Ⅳ),产物收率76%;由3-氯-1,2-环氧丙烷和二苯甲胺制备1-二苯甲基-3-吖丁啶醇(Ⅰ),产物收率58%,化合物(Ⅰ)与氰基乙酸酯化得(1-二苯甲基-3-吖丁啶醇)氰基乙酸酯(Ⅱ),产物收率90%,化合物(Ⅱ)醇解胺化得原料(Ⅲ),产物收率85%。合成路线总收率达到30%,高于目前文献报道合成路线的收率。阿折地平粗品用苯-正己烷重结晶得α型阿折地平产品,用单一溶剂氯苯结晶得β型阿折地平产品。所有中间体和产品均采用HPLC和1H-NMR进行了定性及定量分析。     

基于α-β轴电流融合的液压系统状态监测与故障识别

针对由三相异步电动机拖动的液压系统提出了一种基于静止坐标系下α轴、β轴电流信号融合的图形化状态监测方法。通过测量三相异步电动机定子侧三相电流信号,经Clark坐标变换将三相电流转换到静止坐标系下,由静止坐标系下α、β轴的电流信号融合形成二维图形,根据所得二维图形特征实现液压系统运行状态及故障状况的实时在线监测。实验结果表明该方法简单、直观、可行。相对液压系统常用的油压、振动信号检测及其信号分析方法而言,文中提出的方法在设备运行状态、故障类型识别以及节能控制方面更简单、实用。     

Sustained release of Semaphorin 3A from α-tricalcium phosphate based cement composite contributes to osteoblastic differentiation of MC3T3-E1 cells

The reinforcement of calcium phosphate materials with silk fibroin (SF) has been one of the strategies to overcome the brittleness. However, the lack of osteoinductivity may still restrict their further use. This study aimed to investigate the biocompatibility and osteogenesis capacity of a novel Semaphorin 3A-loaded chitosan microspheres/SF/α-tricalcium phosphate composite (Sema3A CMs/SF/α-TCP) in vitro. Sema3A was first incorporated into CMs, and the Sema3A CMs/SF/α-TCP composite was then prepared. The morphology of the CMs was observed using SEM. The in vitro release kinetics, cytotoxicity, and cell compatibility were evaluated, and the real-time quantitative polymerase chain reaction (RT-qPCR) and activity of alkaline phosphatase (ALP) were used to evaluate the osteogenesis capacity of the composite. The in vitro release of Sema3A from the Sema3A CMs/SF/α-TCP composite showed a temporally controlled manner. The extract of the Sema3A CMs/SF/α-TCP composite presented no obvious side effect on the MC3T3-E1 cell proliferation, nor promote cell proliferation. The MC3T3-E1 cells were well-spread and presented an elongated shape on the Sema3A CMs/SF/α-TCP composite surface; the ALP activity and the osteogenic-related gene expression were higher than those seeded on the surface of the CMs/SF/α-TCP and SF/α-TCP composites. In conclusion, Sema3A CMs/SF/α-TCP has excellent biocompatibility and contributes to the osteoblastic differentiation of MC3T3-E1 cells.     

参麦注射液对单肺通气患者肺损伤的保护作用

目的: 探讨参麦注射液对单肺通气患者肺损伤的保护作用。方法: 择期拟全麻复合连硬下行肺叶切除术的患者40例,随机分为两组:对照组(C组,n=20)和参麦组(S组,n=20)。S组患者麻醉前 10 min 将参麦注射液 0.5 mL/kg 加入 100 mL 生理盐水静脉滴注完毕,C组则使用同等量的生理盐水。分别于麻醉前(T₀)、单肺通气后 30 min(T₁)、60 min(T₂)、90 min(T₃)、120 min(T₄)时抽取桡动脉血和混合静脉血做血气分析,并计算肺泡动脉氧压差(A-aDO₂)和肺分流率(Qs/Qt)。同时抽取桡动脉血 3 mL 迅速离心,测定血浆中超氧化物歧化酶(SOD)、丙二醛(MDA)、TNF-α、IL-6及IL-10浓度。结果: 与T₀比较,C组T_1-4 时Qs/Qt、A-aDO₂均升高(P<0.05),S组Qs/Qt、A-aDO₂仅T₄ 时升高(P<0.05)。与C组比较,S组T_1-4 时Qs/Qt、A-aDO₂均降低(P<0.05)。与T₀比较,C组T_1-4时TNF-α、IL-6和IL-10均升高(P<0.05),S组TNF-α、IL-6和IL-10仅T₄ 时升高(P<0.05)。与C组比较,S组T_1-4时Qs/Qt、A-aDO₂、TNF-α、IL-6和IL-10均降低(P<0.05)。结论: 参麦注射液预处理能有效抑制单肺通气后的氧化应激反应和TNF-α、IL-6、IL-10等炎症因子释放,改善肺换气功能,对单肺通气引起的肺损伤具有保护作用。     

锦州油田无碱二元复合驱实验研究

针对锦州油田的条件及开采现状,进行了α-烯烃磺酸盐类表面活性剂HDS及SNF聚合物组成的二元复合体系(SP)提高采收率的室内研究。考查了HDS表面活性剂的界面张力特性以及吸附特征;进行了二元复合体系的界面张力、表观黏度及岩心驱替等实验。结果表明:HDS表面活性剂油水平衡界面张力可以降低到超低数量级(10-3mN/m),吸附损失小(0.2%浓度HDS≤2.0 mg/g);二元复合体系油水平衡界面张力也能达到超低;黏度保持率高(≥90%),配伍性好,相对水驱提高采收率20%以上。故HDS表面活性剂是性能优良的表面活性剂,HDS与SNF聚合物组成的无碱二元复合体系能大大提高锦州油田的采收率,无碱二元复合驱是适合锦州油田开发的新技术。     

超声熔体处理Al-7%Si合金坯料的半固态铸造

由于从循环利用的废料中不断累积增加Fe元素等杂质元素,所以铸造铝合金零部件高性能的要求往往很难实现。要求合金中粗大板条状的含铁化合物β-Al5FeSi在不使用变质剂和昂贵的纯铝锭条件下转变成无害的形貌结构。在凝固过程中通过利用超声振动来检测分析其对具有不同铁含量的Al-7%Si合金坯料的显微组织的变质效果。在感应加热至半固态温度583℃后,立即对超声熔体处理的坯料进行触变铸造,然后对触变铸造的铸件进行微观组织和拉伸性能检测分析。在触变铸造时,要求球形的初生α-Al相充填合金组织中的微小孔洞中,以便首先确定在坯料中通过超声熔体处理使合金显微组织产生变质效果。在605~630℃温度范围内进行超声熔体处理时,初生α-Al相从树枝状晶转变为细小的圆球形形貌。与未进行超声熔体处理的坯料相比,坯料超声熔体处理后合金中的粗大板条状β-Al5FeSi化合物相变得明显细小。升至583℃后进行半固态铸造不会明显改变β-Al5FeSi化合物的尺寸大小,可是却会使初生α-Al相的形貌变得更圆整,这有利于触变铸造。经预先加热的坯料进行触变铸造后,由于低的铸造温度,产生了快速凝固效果,使得合金中的共晶硅层片变得特别细小。在对超声熔体处理的坯料进行触变铸造时,具有不同铁含量的触变试样的抗拉强度变化并不大,即使合金含铁量达到2%。然而,用未处理的Al-7%Si-2%Fe合金坯料进行触变铸造时,其强度较差,仅为80 MPa,而用超声熔体处理的同种合金坯料,其抗拉强度达180 MPa。用超声熔体处理的不同含铁量的Al-7%Si合金坯料进行触变铸造时,其伸长率也提高了约一倍,例如触变铸造超声熔体处理的Al-7%Si-0.5%Fe合金坯料时,试样的伸长率为11%,而未进行超声熔体处理的同种合金触变铸造试件,其伸长率只有5%。     

Introduction of two polyvinyl alcohol resins for efficient solid support Cu-catalyzed N-arylation of α-aminoacids with aryl halides in aqueous media

In this article, two polyvinyl alcohol (PVA)-based resins were prepared by crosslinking of epoxidized PVA-chains using of 4-(4-aminobenzyl)benzenamine as a crosslinker and polymerization of acrylated PVA chains in the another approach. The prepared PVA resins showed well hydrophilic and swelling properties in various organic solvents, which are used in solid-phase organic synthesis (SPOS). Swelling properties of these resins were examined in dimethylformamide, tetrahydrofuran, water, ethanol, methanol, dichloromethane, and dioxane. Furthermore, the both resins were characterized by FTIR and ¹H-NMR and their properties such as epoxy equivalent weight (EEW) of epoxidized PVA and density of the resins were determined by analytical methods. Then, α-amino acids such as L-aspartic acid, L-leucine, L-alanine, L-serine, L-valine, L-threonine, and L-tyrosine were immobilized on both resins through esterification reaction between these α-amino acids with the present hydroxyl groups on PVA resines, to carry out their solid-phase N-arylation reaction in the presence of CuI as a catalyst in milder and greener conditions than free resin protocols. Hydrolysis of the correponding N-arylated α-amino acids immobilized on the resins gave the N-arylated α-amino acids in high to excellent yields. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47597.     

碟状α-磷酸锆在聚酯粉末涂料中的防腐蚀作用研究

利用水热法合成了碟状 α-磷酸锆（ α-ZrP）并以此为功能填料制备了新型防腐聚酯粉末涂料,采用 SEM、FT-IR和 XRD对磷酸锆的物理形貌和化,学结构进行了表征,分别运用 TGA-DTG和 SEM分析了防腐涂料涂层的热稳定性与微观形貌。以 3.5%NaCl水溶液模仿海洋环境,测试了不同 α-ZrP含量的聚酯粉末涂层在浸泡过程中的交流阻抗谱（ EIS）和极化曲线（ LSV）分析了 α-ZrP对涂料防腐性能的影响。结果表明：添加碟状 α-ZrP能够大幅增强聚酯涂层的耐腐蚀能力,腐,蚀电压显著正移,腐蚀电流密度下降 1~3个数量级。当 α-ZrP的含量占总组分的 3%时,涂层的防腐性能达到最佳。     

Ni-P/TiO2非晶态催化剂对α-蒎烯加氢的性能

采用化学还原法制备Ni-P/TiO₂非晶态催化剂,以α-蒎烯加氢反应为探针反应,考察了催化剂制备条件对其催化性能的影响,得到适宜的制备条件为载体与NiCl₂?6H₂O质量比为3∶1,P/Ni摩尔比为2.5∶1,反应温度为25℃,pH为11。结果表明：该条件下制备的催化剂对α-蒎烯加氢具有较高的催化活性,α-蒎烯转化率为99.89%,顺式蒎烷选择性为98.48%,收率为98.37%,且可重复使用8次。以XRD、BET、DSC、XPS、TEM为表征手段,对催化剂失活前后的结构及形貌进行了分析,结果表明：新鲜催化剂为粒径均一的球形颗粒,粒径约为100nm,分散性较好,引入TiO₂有效提高了Ni-P粒子的热稳定性,将其晶化温度分别提高了78℃、190℃和115.1℃,而失活催化剂的分散度、Ni⁰含量均有下降,出现了活性组分流失、氧化及团聚等现象,这可能是导致催化剂失活的主要原因。