N,N′-二己基对苯二胺的合成

以对苯二胺为起始反应物,利用取代N-烷基化方法,与1-溴己烷进行直接烷基化反应,通过元素分析和光谱分析,证实了合成产物为N,N′-二己基对苯二胺,反应产物收率大于60%,单N-己基化选择性达到100%。     

改性聚酰胺-胺阳离子树状大分子的合成与表征

以甲醇为溶剂、投料比为3.0GPAMAM/N,N-二甲基乙醇胺=1∶16,N,N-二甲基乙醇胺/环氧氯丙烷=1∶1、反应温度50℃、反应时间12h的优化条件下,利用环氧氯丙烷与整代产品进行加成反应,以及环氧氯丙烷与N,N-二甲基乙醇胺进行季铵化反应,对3.0GPAMAM树状大分子进行阳离子改性。并采用红外光谱(FT-IR)、核磁共振(NMR)对产品进行了结构表征。结果表明:所合成的产品与预期产物结构吻合较好,达到预期目标,且阳离子转化率达到90%以上。     

2,4-二-N-甲基丙烯酰胺-α-萘酚及其自聚物的合成与荧光性能研究

以α-萘酚与N-羟甲基丙烯酰胺为原料,经Friedel-Crafts反应合成了荧光单体2,4-二-N-甲基丙烯酰胺-α-萘酚并进一步合成其自聚物。考察了催化剂用量、反应温度、原料物质的量比、反应时间对产率的影响。分别用超导核磁共振谱仪和元素分析仪对产物结构进行分析,并对单体与自聚物的荧光性能进行了对比。结果表明,最佳反应条件为:n(α-萘酚)∶n(N-羟甲基丙烯酰胺)=1∶2,V(溶剂)∶V(催化剂)=10∶1,反应温度40℃,反应时间5h。聚合物的荧光强度高于单体的荧光强度。     

溴化1-乙基-3-甲基咪唑氯化锌离子液体的合成、表征及催化性能

采用溴代乙烷与N-甲基咪唑为原料合成了中间体溴化1-乙基-3甲基咪唑,并与氯化锌反应制备了1-乙基-3-甲基溴化咪唑氯化锌盐。分别经1 HNMR、FT-IR、TG、DSC对离子液体进行了结构表征及热分析。将该离子液体用于尿素醇解合成碳酸二乙酯反应体系,考查了[EMIM][Br][Zn2Cl4]离子液体的催化性能,碳酸二乙酯的收率超过25%。     

N′,N-二-(2-羟乙基)-草酰胺的制备方法研究

以甲醇为溶剂,草酸二乙酯与单乙醇胺为原料制备了N′,N-二-(2-羟乙基)-草酰胺,并对其进行红外光谱分析。研究溶剂用量、反应物配比、反应温度与保温时间对N′,N-二-(2-羟乙基)-草酰胺产率的影响。结果表明:最佳工艺条件为甲醇作溶剂,甲醇与草酸二乙酯质量比=5∶1,反应物摩尔比n(草酸二乙酯)∶n(单乙醇胺)=1∶2.3,反应温度为70℃,保温时间1.5h,此时N′,N-二-(2-羟乙基)-草酰胺产率达到97.1%。     

氨丙基三硅氧烷的合成

以氨丙基二乙氧基甲基硅烷(SG-Si902)、六甲基二硅氧烷(MM)为原料,通过四甲基氢氧化铵((CH3)4NOH)催化合成了氨丙基三硅氧烷。考察了催化剂用量、反应时间、反应物的摩尔比、以及水含量对产物收率及纯度的影响,从而确定出反应的优化条件为:n(SG-Si902)∶n(MM)=1∶5,催化剂占总反应物的摩尔分数为0.45%,N2保护下搅拌反应2h,反应体系中尽可能减少水的含量,产物收率可达42.8%。并通过氢核磁共振(1HNMR)和气相色谱(GC)确证了产物的结构与纯度,其纯度可达99%。     

3,3’,5,5’-四甲基联苯-4,4’-二羟乙基醚的合成与表征

以3,3’,5,5’-四甲基联苯二酚(TMBP)和2-氯乙醇为原料两步法合成了3,3’,5,5’-四甲基联苯-4,4’-二羟乙基醚。探讨了反应物物质的量比、碱用量、催化剂及反应温度对转化率的影响。结果表明,在n(TMBP)∶n(NaOH)∶n(2-氯乙醇)=1∶3.0∶2.5,反应时间为10h,反应温度为110℃条件下,总转化率达95.9%,纯度达99.1%。并用红外、质谱以及核磁等方法对产物结构进行了表征。     

1-甲基-4-苯基-2(1H)喹啉酮衍生物的合成及表征

以苯丙炔酸与氮甲基苯胺合成的N-甲基-N-苯基-3-丙炔酸胺为原料,通过铁催化氧化、重氮化水解合成了一系列1-甲基-4-苯基-2(1H)喹啉酮衍生物。并对喹啉酮衍生物产物进行质谱、核磁共振氢谱和碳谱的定性及结构表征。此方法路线简单,反应条件温和,合成的各种目标产物产率和纯度较高,实验结果令人满意。     

荧光化合物α-N-甲基苯甲酰胺-β-萘酚的合成及表征

以N-羟甲基苯甲酰胺与β-萘酚为原料制备了荧光化合物α-N-甲基苯甲酰胺-β-萘酚。采用FT-IR、1 HNMR、元素分析仪表征了产物结构。利用Gauss03程序包6-31G机组优化化合物结构,得到化合物最优结构的键长、键角。利用紫外可见分光光度计、荧光分光光度计检测化合物的光学性质。通过探讨反应物物质的量比、催化剂与反应溶剂的体积比、反应温度和反应时间对反应产率的影响,得到最佳反应条件为:n(β-萘酚)∶n(N-羟甲基苯甲酰胺)=1∶1.25,V(催化剂)∶V(溶剂)=1∶10,反应温度控制在40℃回流反应7h,此条件下产率为88%。化合物的最大吸收波长为280nm,发射峰分别为348nm和359nm,359nm处的发射峰略低。     

N,N-二-2,3-环氧丙基月桂胺的合成工艺研究

通过将月桂胺(DA)与环氧氯丙烷发生开环反应所得的氯醇分子进一步在KOH-H2O溶液中进行闭环反应,制备得到具有良好反应活性的表面活性剂中间体N,N-二-2,3-环氧丙基月桂胺(EDA)。采用FTIR,1 H-NMR,13 C-NMR等表征手段对产物的结构进行了表征。研究了闭环反应温度、碱的用量、环氧氯丙烷的用量、碱的种类和闭环反应时间等反应条件对产物中EDA含量的影响,在此基础上确定了N,N-二-2,3-环氧丙基月桂胺的最优化反应条件。     

Synthesis and properties of N, N, N ′-tris-(2-ethoxy-naphthalenen-1-yl)??? N, N, N ′ triphenylbenzene 1, 3, 5-triamine for dye sensitized solar cell

New starburst ethoxy naphthylamine is synthesized using multi-step organic reactions. The synthesized compound is characterized using UV-Visible, FT?CIR and NMR spectrometric techniques. The thermal and electrochemical property of the compound was studied using DSC and cyclic voltammetry. Using this compound and a natural dye, organic dye sensitized solid state solar cell was fabricated and the performance analysed.     

Electrosynthesis and properties of N,N dimethylaniline

Poly-N,N-dimethylaniline was prepared by electrochemical polymerization of the monomer on gold, platinum and tin oxide electrodes in an acid medium. The polymer was characterized by cyclic voltammetry and scanning electron microscopy. Poly-N,N-dimethylaniline electrodes, modified by electrodeposition of palladium particles, were prepared.     

橡胶硫化剂N,N'-间苯撑双马来酰亚胺的合成

研究了以乙酸做溶剂,以马来酸酐和间苯二胺为主要原料合成间苯撑双马来酰亚胺的合成方法;通过正交试验,找出了反应的优化条件;通过熔点仪、红外光谱仪、高效液相色谱仪对合成产品进行定性和定量分析.结果表明:溶剂乙酸的用量为间苯二胺质量的3倍,反应容易操作进行;催化剂与间苯二胺的摩尔比为0.05～0.3;马来酸酐与间苯二胺的摩尔比为2.1/1,在此优化条件下产物的得率为90.2%;红外光谱图与标准图谱一致,合成产物的含量为96%.     

五羟乙基二乙烯三胺在0.5 mol/L H2SO4溶液中对2024铝的缓蚀性能

为抑制2024铝在硫酸酸洗液中的腐蚀,以二乙烯三胺与2-溴乙醇为主要原料合成了五羟乙基二乙烯三胺(PHT),采用静态失重法、极化曲线法和电化学阻抗谱研究了PHT在0.5 mol/L H2SO4溶液中对2024铝的缓蚀性能,通过扫描电子显微镜进行了腐蚀形貌分析,并通过腐蚀反应动力学和吸附模型探讨了其缓蚀机理.结果 表明:25℃下PHT的缓蚀效率随其浓度的增加而增大,当PHT的浓度为700 mg/L时,其缓蚀效率可达90.85％以上,具有显著的缓蚀性能.PHT的添加显著增大了腐蚀反应的表观活化能,有效抑制了腐蚀反应的进行,是一种以抑制阳极过程为主的混合型缓蚀剂.25℃下PHT在2024铝表面的吸附是物理吸附和化学吸附的混合吸附,且吸附遵循Langrnuir吸附等温模型.     

Targeted thrombolysis by using c-RGD-modified N,N,N-Trimethyl Chitosan nanoparticles loaded with lumbrokinase

Lumbrokinase (LK) has strong fibrinolytic and thrombolytic activities, but it has a short half-life, can be easily inactivated, and may cause hemorrhage as a side effect. This study develops a potential thrombolytic therapy by fabricating N,N,N-Trimethyl Chitosan (TMC) nanoparticles modified with the cyclic Arg-Gly-Asp-Phe-Lys peptide (c-RGD) and loaded with LK (i.e. c-RGD-LK-NPs). The binding of c-RGD to platelet membrane GPIIb/IIIa receptors is expected to enable targeted delivery of the c-RGD-conjugated TMC to the thrombus. The synthesized c-RGD-LK-NPs had a mean particle size of 232.0?nm, zeta potential of 19.8?mV, entrapment efficiency of 52.7%?±?2.5%, and loading efficiency of 17.4%?±?0.65%. Transmission electron microscopy showed that they were generally spherical. The c-RGD-LK-NPs gave a cumulative in vitro LK release of 80.6% over 8?h, and the activity of LK was close to 80%, indicating that the nanoparticles protected the activity of LK. In vitro blood clot lysis assays were carried out and in vivo thrombolysis effect was tested in Sprague-Dawley rats carotid artery thrombus model. In all cases, the c-RGD-LK-NPs showed superior performance compared with the free LK and the unmodified TMC nanoparticles loaded with LK. The c-RGD-LK-NPs reagent is expected to be potentially useful in treating thromboembolic diseases.     

Adsorption behavior of Cr(VI) on modified natural zeolite by a new bolaform N,N,N,N',N',N'-hexamethyl-1,9-nonanediammonium dibromide reagent

The demand for effective adsorbents is to increase in response to the widespread recognition of the deleterious health effects of Cr(VI)-oxyanions exposure through drinking water. In this study, Cr(VI)-oxyanions uptake from aqueous solutions by a new bolaform N,N,N,N',N',N'-hexamethyl-1,9-nonanediammonium dibromide reagent-modified natural zeolitic materials from Zahedan, Iran, was investigated using batch technique. Spectrophotometry method was used for Cr determination. The Cr(VI)-solution concentration varied between 2 and 104 mg L(-1). It was shown that the Cr(VI) uptake strongly depended on pH. The maximum removal of Cr(VI) occurred in acidic media at pH<1.5. The amounts of Cr(VI) adsorbed increased with increase in dose of both adsorbents and their contact time. Based on results an adsorption mechanism has been suggested. The adsorption data for modified zeolite using the amine was consistent with Langmuir isotherm equation and the equilibrium data was analyzed using the Langmuir isotherm.     

Sol-Gel Processing of Zr(C,N,O) and Al(C,N,O) Powders

,-Diaminoparaxylene was reacted with Zr(OPr ⁿ )₄ at a molar ratio r = 2 or with Al(OBu ^s )₃ with a molar ratio r = 1.5 or 2. Characterization of the obtained hybrid organic–inorganic gels by FTIR, XRD, TGA, and ¹³C CP-MAS NMR showed that a substitution reaction occurred between the OPr ⁿ or OBu ^s groups of the alkoxides and the HN—CH₂—C₆H₄—CH₂—NH groups of the diamine. Powders derived from hybrid gels pyrolysis were also analyzed.     

二苯甲烷双马来酰亚胺的合成和性能

采用3种方法合成了二苯甲烷双马来酰亚胺（BDM），用IR、DSC、SEM和凝胶化时间等方法表征和分析了各法合成BDM及其副产物（BPC）的结构和性能，探讨了BPC的影响。研究认为，BPC能抑制BDM的聚合和活性，对BDM性能不利，文中探索了合成BDM时减少BPC含的若干途径。     

季铵盐壳聚糖及其纳米粒子作为基因载体的研究

评价N,N,N-三甲基壳聚糖盐酸盐(TMC)及其纳米粒子对质粒DNA(pDNA)的负载及保护能力,考察了其纳米复合物对人类肝癌细胞株(HepG 2细胞)的转染能力。通过复凝聚法制备TMC/pDNA纳米粒子,并采用透射电镜及原子力显微镜表征粒子形态和粒径;采用凝胶阻滞分析观察其对pDNA的保护情况;采用四噻氮唑盐(MTT)比色法测定细胞毒性;以Lipofectamine 2000转染试剂作为阳性对照,检测其对HepG 2细胞的转染活性;采用荧光倒置显微镜观察转染情况。结果表明负载pDNA的TMC纳米粒子多呈球形,粒径为100～300nm,能有效地包裹和保护基因不被DNaseⅠ酶消化;当TMC与pDNA的质量比为10∶1时,在48h达到最高的转染效率。