气相色谱法测定对氨基苯乙醚及其有机杂质

采用气相色谱对对氨基苯乙醚及其有机杂质进行分离,用峰面积归一化法进行定量分析。通过气相色谱-质谱联用仪对对氨基苯乙醚及其有机杂质进行分离并定性,给出了各化合物的结构式及结构信息。使用精密度数据对分析方法进行了评价。     

Skeletonized hybrid liposomes

Summary Giant hybrid liposomes of polymerizable lipid and cholesterol were prepared by the hydration method and were polymerized by UV irradiation. The obtained giant liposomes were freeze-dried and washed with chloroform to skeletonize the frame structure of the polymerized membrane. The skeletonized liposomes were directly confirmed by scanning electron microscopy. The single-layered and fully spherical liposome frame were easily confirmed by the stereo-pair of the obtained micrographs.     

低粘度酚醛改性胺环氧固化剂的性能研究

采用非等温DSC法对自制的低粘度酚醛改性胺固化剂与环氧树脂的固化反应工艺参数进行了推导,并通过测试体系的固化度加以验证。固化物采用红外光谱进行了表征,同时测定了浇注体的力学性能、热性能(TG),并通过扫描电镜(SEM)对拉伸断裂面的表面形貌进行了观察。结果表明:环氧树脂E-51与自制固化剂的质量比为100∶35,固化工艺条件为常温/24 h+80℃/2 h时,体系力学性能最佳,拉伸强度55.2 MPa、弯曲强度92.8 MPa、压缩强度83.0 MPa,断裂伸长率2.2%,Tg达到280.3℃。该固化剂粘度低、耐热性好、具有很好的柔韧性,可用于建筑结构胶。     

Analysis of autoxidized fats by gas chromatography-mass spectrometry. IX. Homolytic vs. Heterolytic cleavage of primary and secondary oxidation products

To elucidate the genesis of volatile lipid oxidation products, thermal homolytic and acid heterolytic decomposition processes were compared. Secondary oxidation products were decomposed thermally (200 C), and the volatiles formed were identified by capillary gas chromatography-mass spectrometry (GC-MS). Oxidation products also were decomposed in the presence of HCl-methanol, and the resulting dimethyl acetals were identified by GC-MS. The volatile thermal decomposition products were those expected by homolytic β-scission on both sides of the hydroperoxide group. No dialdehydes were identified under our thermal decomposition conditions. In contrast, the acetals formed by acid decomposition were those expected by selective heterolytic scission between the hydroperoxide group and the allylic double bond. Dialdehydes identified from acid decomposition of cyclic peroxides and dihydroperoxides included malonaldehyde and 2,4-hexadienedial.     

Adsorption of different molecular weight lignosulfonates on dimethomorph powder in an aqueous system

Different molecular weight lignosulfonates were acquired by ultrafiltration and their adsorption behavior on dimethomorph powder were investigated. The results showed that as the molecular weight of lignosulfonates increased the adsorption amounts increased and the adsorption processes were driven by van der Waals forces and hydrophobic effects. The adsorption isotherms were fitted well by Langmuir model. Relations of adsorption amounts and zeta potentials with particle size of dimethomorph particles were established to disclose the dispersing mechanism of dimethomorph suspensions. The average particle sizes were determined by zeta potentials rather than adsorption amounts, which confirmed the dispersing mechanisms were electrostatic repulsive forces.     

制备条件对Co-Mo/nano-TiO2-Al2O3催化剂HDS性能的影响

采用TiCl4水解法制备了一系列纳米TiO2粉体,用机械混捏法制备了nano-TiO2-Al2O3二元复合载体,进而采用等体积浸渍法制备了Co-Mo-P-CA(柠檬酸)/nano-TiO2-Al2O3汽油选择性加氢脱硫催化剂;对TiO2粉体进行了TEM、XRD表征,对nano-TiO2-AlO3二元复合载体进行了吡啶吸...     

Thermally Stable Polymers Derived from Itaconic Acid

Thermally stable polyamides were prepared by reaction of aromatic diamines with pyrrolidone dicarboxylic acids obtained by reaction of itaconic acid with aromatic diamines. The reaction was carried out either by melt poly-condensation or by converting the diacids to their active mixed anhydrides and reacting them with the diamines. Polybenzimidazoles were prepared by melt polymerization of the pyrrolidone dicarboxylic acids with 3,3′-diamino-benzidine. All the polymers were soluble in concentrated sulfuric acid and part of them were also partially soluble in DMF or DMSO. DTA and TGA measurements in air showed that the polyamides were stable up to about 400° and the polybenzimidazoles were stable to 500°.     

非灌流法分离大鼠肝星形细胞及其鉴定

目的采用非灌流法分离大鼠肝星形细胞(Hepatic stellate cell,HSC),并进行鉴定。方法采用非灌流法结合酶消化法分离大鼠肝脏细胞,密度梯度离心进一步分离HSC,油红染色检测HSC胞质中的脂滴,免疫组化法检测细胞中α-平滑肌肌动蛋白(α-Smooth muscle actin,α-SMA)、结蛋白(Desmin)及神经胶质酸性蛋白(Glial fibrillary acidic protein,GFAP)的表达。结果非灌流法结合酶消化法可成功分离大鼠HSC;密度梯度离心纯化的HSC经油红染色,细胞核周围可见红色脂滴;该细胞中α-SMA、结蛋白及GFAP的免疫组化染色结果均呈阳性,细胞着色率可达90%以上。结论成功建立了大鼠HSC的非灌流分离模式,所获得的HSC纯度较高,该方法稳定简便,具有一定的推广应用价值。     

磁性活性炭的制备与表征

探讨了负压浸渍法制备磁性活性炭的浸渍条件,浸渍溶液为油酸修饰的Fe3O4磁性凝胶均匀分散在正己烷溶剂中形成的磁性溶液. 通过对油酸修饰的磁性凝胶进行差热、热重和微热容分析确立了浸渍产物的热处理条件,考察了磁性溶液浓度、浸渍时间、浸渍温度对浸渍产物的影响,并采用X射线衍射对磁性活性炭的组份和结构进行了表征,采用磁强计测定了磁性活性炭的磁性能,用比表面、孔容测试技术比较了活性炭和磁性活性炭的比表面、孔体积和孔分布.     

Novel Organometallic Aromatic Azo Polyesters Based on Ferrocene

Some ferrocene containing aromatic azo polyesters were prepared by condensing 1,1-ferrocenedicarbonyl chloride with different azo groups containing aromatic diols, which were synthesized by diazotization coupling reaction from aromatic diamines. The polymeric products were separated as two portions on the basis of their solubility and subsequently characterized by their elemental analysis and FTIR spectral studies. Thermal properties of the products were measured by differential scanning calorimetry and thermogravimetry and the activation energies of pyrolysis were calculated using Horowitz and Metzger's method. The molecular weights of the soluble portions were determined by gel permeation chromatography (GPC) and these portions were also characterized by their inherent viscosities and UV-Vis spectroscopic studies.     

用铝硅复合催化剂催化聚合的聚酯性能研究

以三氧化二锑(Sb2O3)、不同质量比的铝酸钠/硅酸钠复合物分别作为聚酯缩聚催化剂制取聚酯切片,利用凝胶渗透色谱(GPC)、色值、差示扫描量热(DSC)及热失重(TG)对聚合产物分别进行分析.结果表明:以铝硅复合催化剂F1[n(铝酸钠)∶m(硅酸纳)=4∶1]催化制取的聚酯相对分子质量及分子质量分布接近以Sb2O3催化制取的聚酯,而且色相指标比用Sb2O3催化制取的聚酯好,其白度L值高,黄度b值低;复合催化剂制取的聚酯的玻璃化转变温度(Tg)低于Sb2O3催化制取的聚酯,但结晶温度高于Sb2O3催化的聚酯,表明聚酯的结晶能力有所提高;复合催化剂催化聚合的聚酯热性能与常规Sb2O3催化的聚酯基本接近.     

Preparation and Properties of Natural Rubber/Palygorskite Composites by Co-Coagulating Rubber Latex and Clay Aqueous Suspension

Natural rubber (NR)/Palygorskite composites were prepared by co-coagulating rubber latex and clay aqueous suspension. Org-palygorskite was attained by using cetyltrimethylammonium bromide (CTAB) and the four factors influencing the average diameter of palygorskite were discussed. Four optimal conditions of preparing minimum average diameter were determined which included the concentration of palygorskite, the concentration of sodium polyacrylate, ultrasonic time and ultrasonic power. Mechanical properties suggested that composites using modified palygorskite which were dispersed by ultrasonic wave were the best, the tensile strength, tear strength, 300% modulus and shall hardness increased by 77.14%, 118.18%, 242.86% and 65.2%, respectively. Modified palygorskite was shown by FTIR spectrogram and observed by ESEM. Modified palygorskite dispersed by ultrasonic wave were dispersed into the rubble uniformly, some stick particles inserted into the rubber and it is difficult to find stick shape, and there were 20% particles belonging to nanomaterials and 80% micromaterials.     

四种杜仲样品中生物活性物质含量的测定

对四种村珍贵吕绿原酸类物质进行了提取，首次用蛊硅胶Ｇ薄板一次将它们逐一分离。采用高压液相色谱、紫外、红外、质谱及核磁工振等对绿原酸类物质进行了定性及结构分析；并用紫外分光光度计测定了该四种类型杜仲中绿原酸类物质的总含量     

纳米MoS2的制备及其与聚吡咯物复合膜光学性能的研究

以有机热溶剂法制备MoS2,并以XRD对其结构进行表征.TEM形貌观察表明晶粒具有纳米尺寸。以电化方法在ITO导电玻璃基体上制备聚合物聚吡咯薄膜。在导电聚合物膜上涂布纳米MoS2晶体,荧光分析发现其荧光光谱相对于聚合物膜有一定程度的红移。Z-Scan测试其折射率的结果表明其具有非线性光学特性。     

The influence of particle size of slurry on life on BME-MLCC

Four slurries and base metal electrode multiplayer ceramic capacitor (BME-MLCC) samples（0603-X7R-50V-104）were prepared by using different grinding ways. The particle sizes of slurries were characterized by grading analysis and the micro-morphology of films and samples were analyzed by scanning electronic microscopy (SEM). The structure was characterized by X-ray powder diffraction (XRD). Finally, the life of samples were tested by highly accelerated life testing (HALT). Results showed that the particle size distribution of slurry which was made using smaller grinding media by sander was narrow. The micromorphology of as-prepared films and samples were more tightly, the numbers of particles in single dielectric were more, the initial reliability was better and the life was longer.     

间羟基-N,N-二乙基苯胺的分析方法研究

采用气相色谱对间羟基-N,N-二乙基苯胺及其有机杂质进行分离,用峰面积归一化法进行定量分析。通过气相色谱-质谱联用仪对间羟基-N,N-二乙基苯胺及其有机杂质进行分离并定性,给出了各化合物的结构式。使用精密度数据对分析方法进行了评价。     

Der Einfluß von Genotyp und Anbauort auf verschiedene Inhaltsstoffe von Samen des Ölkürbis (Cucurbita pepo L.)

Influence of Genotype and Cultivation Place on Various Ingredients of Oil-Gourd Seeds (Cucurbita pepo L.) In the seed of oil pumpkin from an international variety trial several components were analysed. The following results were found: 1. Oil contents were about 49% in mean and were significantly influenced by location, year, variety and by the interaction between location and year. 2. Protein contents laid about 38% in mean and were significantly changed by location. 3. Average crude fibre contents were about 5.17%. The interaction location/year was secured in F-test. 4. Oleic acid contents laid about 27.9% in mean and were influenced by variety, location, year and by the interaction location/year. 5. Average linoleic acid content was about 54.4% of TEA whereby differences within varieties, locations and years as well as interaction location/year were statistically secured. A negative correlation (r=-0.9915) exists between both fatty acids. 6. The tocopherol contents were 437 mg/kg oil in mean and were modificated analogous to oleic- and linoleic acid by variety, location, year and interaction location/year. 7. Average phosphatide contents were about 0.82% and were significantly influenced by variety, location as well as interaction location/year. 8. Mean values of the different minerals were: P = 211 ppm; K = 183 ppm; Mg = 105 ppm; Ca = 26.9 ppm; Na = 3.6 ppm. All elements were significantly depending on location, P and K were depending on variety, too.     

Copolyester studies. V. Preparation and characterization of tetramethylene terephthalate–poly(tetramethylene oxide) random block copolymers

Random block copolymers of tetramethylene terephthalate and polytetrahydrofuran (PTHF) were prepared by melt polycondensation. Five different molecular weights of PTHF were used in the polymerizations with up to 30% by weight incorporation. The copolymers so obtained were characterized in terms of their molecular weight by means of endgroup analysis and solution viscometry. Compositions were established by nuclear magnetic resonance spectroscopy. Thermal properties were studied by differential scanning calorimetry and dynamic mechanical methods. Melting and glass transition temperatures are discussed in terms of the structural differences, particularly the effect of polyether composition and block size on chain flexibility.     

原位聚合不同填料/UHMWPE及其性能研究

用原位聚合法制备了分别加入纳米碳化硅、玻璃微珠、二硫化钼等填料的超高摩尔质量聚乙烯复合材料, 测试了其性能,并对原位聚合法和共混法的复合材料材料性能进行了对比。结果表明:该复合材料不但基本保持了超高摩尔质量聚乙烯原有的优异性能,而且与纯超高摩尔质量聚乙烯相比,该复合材料的硬度、热变形温度等都有不同程度的提高。原位聚合法制备的复合材料比共混法的综合性能高。     

皮革染料商品化研究

在染料水溶液中,加入聚乙二醇400、二乙醇胺、羟乙基纤维素、五乙烯六胺、四甲基胍、分散剂NNO等商品化助剂,喷雾干燥得到皮革染料。利用聚乙二醇400、二乙醇胺和羟乙基纤维素,可有效提高防尘性和溶解性;利用五乙烯六胺和四甲基胍成盐复配,可有效提高溶解性和对皮革的亲和力;利用表面活性剂,可有效提高匀染性和防尘性。该染料非常适合皮革的染色。