红外光谱法测定航空润滑油液压油中2,6-二叔丁基对甲酚含量

用红外光谱法测定航空润滑油、航空液压油中抗氧剂2,6-二叔丁基对甲酚的含量.用光学衰减器作补偿,记录试样在3 760～3 550cm-1区间的红外光谱,基线法计算试样中2,6-二叔丁基对甲酚的羟基伸缩振动吸收带在3 650 cm-1处的吸光度.以工作曲线定量.2,6-二叔丁基对甲酚的质量分数在0.05%～0.10%范围内服从比耳定律.其线性回归方程为A=0.003 03+0.560 81 C,相关系数为0.998 0.     

CeZrYLaO对Fe基整体式稀薄甲烷催化燃烧性能的影响

采用共沉淀法制备了高性能低铈储氧材料Ce_0.35Zr_0.55Y_0.07La_0.03O_1.95(OSM,储氧材料)和胶溶法制备了耐高温、高比表面的La-Al₂O₃并以它们为载体,制备了一系列整体式铁基催化剂。考察了该系列催化剂对甲烷稀薄燃烧的催化性能,并用低温N₂吸附-脱附,储氧能力(oxygen storage capacity,OSC),XRD,XPS和H₂-TPR等测试手段对载体和催化剂进行了表征。活性测试结果表明所制得的整体式催化剂Fe/OSM+La-Al₂O₃可在50 000 h^-1的高空速条件下使含量为1%的甲烷在474 ℃起燃,565 ℃完全转化;低温氮吸附-脱附测试结果表明,所制得的Ce_0.35Zr_0.55Y_0.07La_0.03O_1.95经1 050 ℃焙烧5 h后的BET比表面积达33 m²·g^-1,孔容为0.14 mL·g^-1;La-Al₂O₃经1 050 ℃焙烧5 h后的BET比表面积达125 m²·g^-1,孔容为0.46 mL·g^-1,是优良的催化剂载体;OSC测试结果表明,加入储氧材料(oxygen storage material(OSM))能增加催化剂的储氧性能,有利于催化活性的提高;XRD测试结果表明,OSM以均一固溶体存在;XPS测试结果表明,Fe₂O₃与OSM载体之间的相互作用最强;H₂-TPR测试结果表明,加入OSM能增加催化剂的还原性能,从而提高了催化活性。     

Microwave-assisted fast and efficient synthesis of some crown ethers

13-Crown-4,16-crown-5,dibenzo-12-crown-4 and dibenzo-14-crown-4 were synthesized by a one-pot microwave-assisted procedure in good yields.Irradiation of diols and dichlorides in the presence of sodium hydroxide in DMSO gave title crown ethers presumably within a template effect.     

Two new C-glucofuranosyl isoflavones in puerarin injection

Two new C-glucofuranosyl isoflavones of impurities in puerarin injection were isolated.Their structures were determined to be 8-C-α-glucofuranosyl-7,4'-dihydroxyisoflavone and 8-C-β-glucofuranosyl-7,4'-dihydroxy-isoflavone by chemical and spectral analysis.     

Highly stable supramolecular hydrogels formed from 1,3,5-benzenetricarboxylic acid and hydroxyl pyridines

New supramolecular hydrogels with the maximal sol-gel transition temperature(T_(gel)) of 95℃were obtained by using gelators formed from 1,3,5-benzenetricarboxylic acid(BTA) and para-hydroxyl pyridine(PHP) or meta-hydroxyl pyridine(MHP).The single crystal structure of the complex formed from BTA and ortho-hydroxyl pyridine(OHP) indicated that the molecules assembled into superstructure via both hydrogen bonds andπ-πstacking interaction.     

Thermal degradation and isothermal crystalline behavior of poly（trimethylene terephthalate）

Poly(trimethylene terephthalate)(PTT) is an excellent fiber material.Its thermal degradation and isothermal crystalline behaviors were in this study investigated using thermogravimetric analysis(TGA),thermogravimetric analysis-Fourier transform infrared spectroscopy(TGA-FTIR) analysis,differential scanning calorimetry(DSC) and X-ray diffraction(XRD).The thermal degradation mechanism of PTT follows Mclafferty rearrangement principle.The PTTwithintrinsicviscosity(Ⅳ) of 0.74 dL/g has a maximum crystallinity...     

二次注射成型聚丙烯中剪切诱导连接界面的形态演变

研究了剪切作用对二次注射成型聚丙烯连接界面形态演变的影响.利用偏光显微镜研究了连接界面距离浇口不同区域和不同位置的形态差异,探索了连接界面形态的演变规律,通过改变注射压力和注射速度对其加以验证,并通过DSC分析证实了形态结构的差异.研究表明:剪切作用对连接界面形态的影响显著,在高剪切作用下分子链沿流动方向取向程度高,不利于其规整排列并沿垂直界面方向生成横晶;可以通过注射压力和注射速度来控制连接界面的剪切作用,从而得到具有完善横晶结构的连接界面形态.     

Two new bromoindoles from red alga Laurencia similis

Two new bromoindole alkaloids have been isolated from the ethanolic extract of the red alga Laurencia similis.On the basis of chemical and spectroscopic methods(including 1D and 2D NMR technique),their structures have been elucidated as 2,2′,5,5′,6,6′-sixibromo -3,3′-bi-1H-indole and 3,5-dibromo-1-methylindole,respectively.     

含偶氮苯基团的三枝状凝胶因子的合成和凝胶性质研究

设计合成了一种中心为三乙基氨基,酰胺基作为氢键连接基团,柔性的烷基链连接偶氮苯基团的含多种分子间弱相互作用的三枝状有机凝胶因子1.由于偶氮苯基团处于分子的外缘,在THF溶液中,凝胶因子1表现出良好的光致变色行为.凝胶性能测试中,分子间存在氢键作用、π-π相互作用等使得该化合物在醇类、有机酸类和乙腈等极性溶剂中极易形成稳定的有机凝胶.在少数的非极性溶剂,如正己烷和环己烷中也可以形成稳定凝胶,并且随着溶剂极性的不同,凝胶形貌呈现出规则的纤维状或带状结构.     

新型的双阴离子型镱(Ⅲ)胺化物{[Me_2Si(NPh)_2]_2Yb[(N~iPr)_2CN(SiMe_3)_2]}{Li(THF)_2}_2的合成及晶体结构

结构新颖的双阴离子型桥联胺基胍基镱(Ⅲ)配合物{[Me2Si(NPh)2]2Yb[(NiPr)2CN(SiMe3)2]}{Li(THF)2}2是通过二胍基镱氯化物[(SiMe2)2NC(N'Pr)2]2Yb(μ-Cl)2Li(THF)2和桥联胺基锂盐PhLiNSiMe2NLiPh反应制得,该配合物经过了IR、元素分析和X-ray晶体结构的测定.该晶体为单斜晶系,P 21/c空间群,a=14.0001(8),b=17.6808(9),c=24.9565(16)A,B=95.994(3),V=6143.8(6)A3,Dc=1.287g/cm3,Z=4.