席夫碱的一锅法合成及还原

席夫碱是一种应用广泛的配体,它能与元素周期表中的大多数金属形成配合物,部分席夫碱配体稳定性差,但席夫碱还原化合物的稳定性普遍较好,所以研究高效合成席夫碱还原化合物的方法对拓宽席夫碱在配位化学中的应用具有重要意义. 研究报道了一种“一锅法”合成及还原席夫碱的方法,使用的还原剂为醋酸硼氢化钠,反应条件温和,反应快捷（只需2~3 h即可完成反应）,产率高,中间体席夫碱可以不用分离而直接进行还原,反应的底物适用性广,且可以用于大剂量的目标化合物的制备中. 用该方法合成了8种席夫碱还原物,其中三种为邻碘芳基席夫碱还原化合物,它们是许多医药、农药的重要组成部分.     

芳香聚酰胺纳滤膜的制备及影响因素

以聚间苯二甲酰间苯二胺为原料，采用相转化法制备了芳香聚酰胺纳滤膜、实验重点考察了铸膜液固含量、溶剂蒸发时间、凝胶浴组成和温度、膜厚等因素对所制纳滤膜性能的影响．这些因素主要是通过改变膜表皮层中高聚物的胶束聚集体孔和空间网络孔的大小和数目来影响所制膜的性能．采用扫描电子显微镜（SEM）观察了膜的微观形态结构，表明所制纳滤膜具有典型的不对称结构．     

对一磺酰胺基苯肼的合成

本文主要讨论了由对一氨基苯磺酰胺经重氮盐还原成对一磺酰胺基苯肼的一种合成方法。其中对重氮化反应的温度,及由重氮盐还原成对一磺酰胺基苯肼时还原介质的PH值和亚硫酸钠用量等对反应及产率的影响。     

一锅法催化合成N-苄基-4-甲基苯胺

以Raney-Ni为催化剂,对甲基硝基苯和苯甲醛为原料一锅法催化合成了N-苄基-4-甲基苯胺.考察了氢压、反应温度、反应时间、催化剂用量及物料配比等对N-苄基-4-甲基苯胺合成的影响,探讨了一锅法催化合成了N-苄基-4-甲基苯胺的反应机理.实验结果表明,以对甲基硝基苯和苯甲醛为原料一锅法催化合成N-苄基-4-甲基苯胺的反应过程是分二步进行的.优化的合成N-苄基-4-甲基苯胺工艺条件为:苯甲醛与对甲基硝基苯的摩尔比为1:1.0～1:1.02;Raney-Ni催化剂用量为5%(以对甲基硝基苯用量计);氢压为1.0 Mpa;反应温度为353 K;反应时间为90 min.在此所选择的条件下,N-苄基-4-甲基苯胺的收率达99.1%～99.7%.     

高渗透性芳香聚酰胺反渗透膜的影响因素及机理分析

随着反渗透膜应用的普及化和广泛化,提升其渗透性能成为了当下的迫切追求。为进一步改善以间苯二胺(MPD)与均苯三甲酰氯(TMC)为反应单体的芳香聚酰胺反渗透膜的分离性能以及表面形貌,从水相浸润时间、油相反应时间、热处理温度和时间、MPD及TMC的添加量、以及二甲亚砜(DMSO)的添加量等方面进行了研究,得到具有均一形貌的高渗透性芳香聚酰胺反渗透膜。通过对芳香聚酰胺反渗透膜进行性能评价、扫描电子显微镜(SEM)以及傅里叶红外变换光谱仪(FT-IR)等测试。结果表明：改善工艺参数后得到的反渗透膜拥有良好的渗透性能、分离性能以及表面形貌。     

半芳香族聚酰胺成炭剂的合成与应用

采用对苯二甲酰氯与丙二胺通过低温溶液法合成了一种半芳香族聚酰胺(PPTA)成炭剂,研究了反应温度、反应时间、单体摩尔比等因素对产物产率和比浓黏度的影响。确定了PPTA的最佳合成工艺:预聚温度0℃,单体摩尔比(丙二胺∶苯二甲二酰氯)1.05∶1,助溶盐CaCl2用量4 g/100 mL溶剂,单体浓度0.7 mol/L,聚合时间4 h。用傅里叶红外、核磁共振氢谱和热失重分析方法对产物进行了表征。探讨了以PPTA为碳源,聚磷酸铵(APP)为酸源的膨胀型阻燃体系(IFR)对ABS的成炭阻燃效应。结果表明,PPTA的热分解性能与ABS的分解温度较为匹配,可显著提高ABS/APP阻燃体系在高温下的残炭量和阻燃性能。SEM形貌显示PPTA的加入能促进阻燃体系在燃烧后表面形成均匀、致密的炭层结构。     

“一锅法”合成β-苯甲酰基丙烯酸乙酯

以乙醛酸和苯乙酮为原料,采用"一锅法"合成β-苯甲酰基丙烯酸乙酯,较佳反应条件是n(苯乙酮)∶n(乙醛酸)∶n(乙醇)∶n(硫酸)=1.00∶1.25∶5.07∶0.02,酯化反应温度85℃、时间3 h,消除反应温度115~120℃、反应时间9 h。按苯乙酮计,β-苯甲酰基丙烯酸乙酯的收率77.74%,质量分数91.07%。     

油菜田除草剂DPX-A7881的合成 (Ⅰ)──中间体2-甲氧羰基苯磺酰胺的合成

以糖精为原料，采用直接酸催化法合成了２－甲氧羰基苯磺酰胺，收率达到９０．２％．     

One-pot synthesis and structural characterization of urea-isobutyraldehyde-formaldehyde resin

Urea-isobutyraldehyde-formaldehyde (UIF) resin was synthesized from urea, isobutyraldehyde, and formaldehyde using sulfuric acid as a catalyst by one pot method. The effects of molar ratios of isobutyraldehyde to formaldehyde (n(I)/n(F)) and aldehyde to urea (n(A)/n(U)) on the yield, hydroxyl value (vs KOH) and softening point of the resin were investigated. The structure of the resin was characterized by FT-IR, ¹H-NMR and ¹³C-NMR. The results show that when the molar ratio of urea to isobutyraldehyde to formaldehyde (n(U)/n(I)/n(F)) is 1.0/3.0/3.0, the yield UIF resin is 67.1%, and the softening point and hydroxyl value are 88 °C and 37 mg/g, respectively. The FT-IR, ¹H-NMR and ¹³C-NMR results show that the lactam is formed by aminomethylation from urea, isobutyraldehyde, and formaldehyde. Foundation item: Project(2006A10902001) supported by the Science and Technology Plan of Guangdong Province, China; Project(2007Z3-D0351) supported by the Science and Technology Plan of Guangzhou City, China     

Synthesis and characterization on semi-aromatic polyamide containing benzoxazole unit

In order to obtain a novel polyamide having excellent heat-resistant properties which could be anticipated as a thermal modifier for aliphatic polyamide,a series of new semi-aromatic polyamides (BO6,BO8,BO10) containing benzoxazole unit were synthesized based on 5-amino-2-(p-aminophenyl) benzoxazole (ABO) and aliphatic acids (adipic,suberic and sebacic acid) by means of Yamazaki phosphorylation method.The effect of reaction temperature on the inherent viscosity of the polymers was studied,and the structures of products were characterized by FTIR,1 H-NMR,and the heat resistance of the polymers was studied by DSC and TG.The results showed that the reaction temperature gives the polymers the highest viscosity at around 90 ℃,130 ℃ and 130 ℃ for BO6,BO8 and BO10,respectively.The heat resistance of the new semi-aromatic polyamides is much higher than that of the common aliphatic polyamides.In addition,the products show good solvent resistance and crystallization properties.     

One-pot synthesis of Sb-Fe-carbon-fiber composites with in situ catalytic growth of carbon fibers

A Sb-Fe-carbon-fiber (CF) composite was prepared by a chemical vapor deposition (CVD) method with in situ growth of CFs us-ing Sb2O3/Fe2O3 as the precursor and acetylene (C2H2) as the carbon source. The Sb-Fe-CF composite was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM), and its electrochemical per-formance was investigated by galvanostatic charge-discharge cycling and electrochemical impedance spectroscopy. The Sb-Fe-CF composite shows a better cycling stability than the Sb-amorphous-carbon composite prepared by the same CVD method but using Sb2O3 as the precur-sor. Improvements in cycling stability of the Sb-Fe-CF composite can be attributed to the formation of three-dimensional network structure by CFs, which can connect Sb particles firmly. In addition, the CF layer can buffer the volume change effectively.     

Melt synthesis and characterization of poly(L-lactic acid) chain linked by multifunctional epoxy compound

High molecular weight(Mw) poly(L-lactic acid)s(PLLAs) were synthesized using multifunctional epoxy compound(Joncryl-ADR4370) as chain extender. The products were characterized by gel permeation chromatography(GPC) and spectroscopy(¹HNMR and FTIR). The results indicated that the Mw of PLLA increased with the increasing of the ratio of epoxy compound and the extending of reaction time. The highest M _w of PLLA reached 360 000 g/mol when the ratio of epoxy compound was 1.5 wt%. However, the reactants turned to cross-linking when the ratio of epoxy compound was over 1.5 wt%. Differential scanning calorimetry(DSC) measurements demonstrated that the glass transition(T _g) and melting temperatures(T _m ) of products increased slightly as the increase of the molecular weight. Analysis of the hydrolytic degradation in vitro showed that the branched PLLA possessed the quicker degradability than that of the linear PLLA.     

硝基苯加氢合成对氨基苯酚绿色催化反应过程

对氨基苯酚是一种重要的化工原料及有机中间体.本课题组对非硫酸介质中硝基苯加氢合成对氨基苯酚催化剂及合成工艺进行了系统研究.本文综述了这方面的研究进展,包括铂均匀分散的酸性离子液体催化剂、Pt/SiO2和酸性离子液体构成的固-液相型双功能催化剂、固载型Pt-离子液体催化剂、Pt-超强酸双功能催化剂、Pt-杂原子取代磷酸铝分子筛催化剂、Pt-碳基固体酸催化剂及Pt-Lewis酸金属盐催化剂等.其中,Pt-Lewis酸金属盐催化体系的反应活性和选择性达到或接近了工业上以硫酸为酸催化剂的水平,具有良好的工业应用前景,目前正在对其进行工业放大过程的相关研究.     

主链含间位砜酮结构聚芳醚的合成与表征

以苄川氯和氯磺酸制备间磺酰氯基苯甲酰氯,再以间磺酰氯基苯甲酰氯和氯苯在无水三氯化铝催化剂下反应制备1-(对氯苯甲酰基)-3-(对氯苯磺酰基)苯,以DMAc为溶剂,1-(对氯苯甲酰基)-3-(对氯苯磺酰基)苯和双酚A为单体合成新型聚芳醚砜酮,通过FT-IR和1H-MNR对聚合物的结构进行了表征并通过TG、DSC进行了性能测试。结果表明,含有间位砜酮结构的新型聚芳醚砜酮具有良好的热稳定性和可溶性。     

主链含间位砜酮结构聚芳醚的合成与表征

以苄川氯和氯磺酸制备间磺酰氯基苯甲酰氯,再以间磺酰氯基苯甲酰氯和氯苯在无水三氯化铝催化剂下反应制备1-(对氯苯甲酰基)-3-(对氯苯磺酰基)苯,以DMAc为溶剂,1-(对氯苯甲酰基)-3-(对氯苯磺酰基)苯和双酚A为单体合成新型聚芳醚砜酮,通过FT-IR和1H-MNR对聚合物的结构进行了表征并通过TG、DSC进行了性能测试。结果表明,含有间位砜酮结构的新型聚芳醚砜酮具有良好的热稳定性和可溶性。     

新型聚芳酰胺酰亚胺的合成与表征

基于新型邻二苯基取代偏三酸酐合成了粘度在0．39－1．43系列聚芳酰胺酰亚胺，新型无定型聚合物在极性非质子溶剂DMAC，NMP，DMF，DMSO等中有良好的溶解性，其玻璃化转变温度在284－336℃．5%热失重温度大于468℃。     

丙烯腈/丙烯酸甲酯与相变微胶囊共混物薄片的制备及性能表征

采用水相沉淀聚合法制备相变材料微胶囊质量分数为0%～25%的丙烯腈/丙烯酸甲酯共聚物的混合物,经熔融压制成厚度为1 mm的薄片;分别采用差示扫描量热分析仪(DSC)、X-射线衍射分析仪(XRD)、动态热机械性能(DMA)和扫描电子显微镜观察(SEM)对混合物薄片的结构和性能等进行分析测试.结果表明:相变材料微胶囊的加入使混合物薄片的玻璃化转变温度升高,薄片的熔融焓和结晶焓随微胶囊含量的增加而增大.