表面化学接枝改性阻燃棉织物的制备与性能

采用高碘酸钠对棉织物表面进行选择性氧化生成醛基,选取乙二胺与醛基反应,通过膦氢化加成反应将阻燃剂亚磷酸二甲酯接枝到棉织物表面,最后通过三羟甲基三聚氰胺对棉织物表面进行接枝改性,制备了含三羟甲基三聚氰胺/乙二胺/亚磷酸二甲酯阻燃棉织物.通过傅里叶红外光谱（FTIR）对改性后棉织物的结构进行了表征,通过极限氧指数（LOI）测试研究了其阻燃性能,通过锥形量热测试研究了其燃烧行为,通过在40℃皂水中洗涤10次考察了其耐水性能,通过扫描电子显微镜测试了其表面及燃烧后炭层的形貌.研究结果表明,经表面改性后,棉织物的LOI值由（19.5±1.0）%提高到了（43.1±1.0）%,经耐水洗测试后,LOI值仅下降至（42.6±1.0）%,保持了非常好的阻燃性能,表明通过表面接枝方法制备的三羟甲基三聚氰胺/乙二胺/亚磷酸二甲酯阻燃棉织物具有非常好的耐水洗性能.表面阻燃改性提高了棉织物在燃烧过程中的成炭性能,形成的连续膨胀的炭层较好地保护了内部织物,抑制了织物的降解和燃烧,从而提高了棉织物的阻燃性能.     

环交联聚磷腈微球的合成及阻燃聚碳酸酯的研究

本文合成了一种环状交联型不溶、不熔的聚(环三磷腈-二羟基二苯砜)微球(PZS)并应用于聚碳酸酯(PC)的阻燃.通过傅里叶变换红外光谱(FTIR)、扫描电子显微镜(SEM)以及透射电子显微镜(TEM)对PZS微球进行表征;热重分析(TG)探究聚碳酸酯复合材料的热稳定性,并通过极限氧指数测试(LOI)和锥形量热(CONE)表征其阻燃性能.TG结果表明,PZS微球具有良好的热稳定性及优异的成炭能力.燃烧测试结果表明,PZS微球可以显著提高聚碳酸酯的阻燃性能.当阻燃剂添加量为5%时,LOI值从纯PC的27.4%提高到了31.5%.锥形量热实验结果表明,PZS微球的加入使得复合材料的热释放速率、总放热量以及平均质量损失速率显著降低,材料的点燃时间显著延长.通过扫描电镜和红外光谱对残炭进行分析,结果显示PZS微球在燃烧过程中产生磷酸类物质,促进PC基体交联炭化,在外表面生成致密炭层,从而起到隔热隔氧的阻燃效果.     

直接鉴别延胡索及其伪品的FTIR-主成分分析法研究

采用傅里叶变换红外光谱直接测定法测定了延胡索及其伪品齿瓣元胡、东北延胡索、土元胡、新疆延胡索及夏天无的傅里叶变换红外光谱,采用主成分析法比较了正伪品之间的差异程度.结果表明基于傅里叶变换红外光谱的主成分分析在反映同属不同种植物化学组成差异程度上具有应用价值.     

含羟基磷灰石纳米线复合夹层的高性能锂硫电池

通过水热合成法制备羟基磷灰石[Ca₅（PO₄）₃（OH）]纳米线（HN）,并与多壁碳纳米管（MWCNTs）导电纸形成层次交联的新型羟基磷灰石纳米线复合（HN/CNT）夹层.利用扫描电子显微电镜、傅里叶变换红外光谱（FTIR）和紫外-可见光谱（UV-Vis）等对材料的形貌与结构进行表征.电化学测试结果表明,含HN/CNT夹层的锂硫电池在1C倍率下循环200次后放电比容量仍保持在871 mA · h/g,每次循环衰减率仅为0.031%.     

自组装金电极的电化学测试及其FTIR和AFM分析

利用交流阻抗谱测试了自组装免疫电极的抗原响应特性，对生物电极解离过程的机理进行了研究，用傅里叶变换红外反射光谱（FTIR）和原子力显微镜（AFM）对电化学实验过程进行了直观观测和定量分析。     

CNT表面修饰对Pt/CNT在邻氯硝基苯加氢反应中催化性能的影响

用乙二醇还原法制备了碳纳米管(CNT)负载的铂催化剂(Pt/CNT).考察了CNT化学修饰与物理修饰对催化剂的影响.CNT化学修饰采用H2SO4-HNO3氧化法,物理修饰采用十二烷基硫酸钠(SDS)吸附法.用X射线衍射、透射电子显微镜、电感耦合等离子发射光谱、H2程序升温脱附、傅里叶变换红外光谱和元素分析对Pt/CNT催化剂进行了表征,并以邻氯硝基苯选择加氢为探针反应考察了Pt/CNT的催化性能.结果表明,化学修饰与物理修饰都能在CNT表面引入一定数量的活性位,有助于促进Pt异相成核,提高Pt的分散性,进而提高催化剂的活性.SDS在一定浓度下可形成特定结构的胶束,导致形成特定形貌的Pt纳米粒子.     

Zn-Al-[V_(10)O_(28)]~(6-)双层氢氧化物掺杂对LY12铝合金表面溶胶-凝胶涂层性能的影响

采用共沉淀法制备Zn-Al-[V10O28]6-双层氢氧化物(以下简称LDH-V),研究不同添加浓度(0.0、0.25×10-3、0.75×10-3、1.5×10-3、3.0×10-3mol·L-1)的LDH-V对LY12铝合金溶胶-凝胶涂层形貌、耐蚀性的影响.采用扫描电子显微镜(SEM)和傅里叶变换红外(FTIR)光谱研究LDH-V对涂层形貌和结构的影响.运用中性盐雾实验对涂层进行耐蚀性评估.利用电化学方法对涂层在0.05 mol·L-1的NaCl溶液中的腐蚀行为进行研究.探讨加入LDH-V后溶胶-凝胶涂层的耐蚀机理.结果表明,一定量LDH-V的加入不仅可以提高溶胶-凝胶涂层的耐蚀性能,还可对涂层被破坏区域进行自修复,起到延缓铝合金基体腐蚀的作用.然而,当LDH-V的添加溶度超过一定值时,会破坏涂层的完整性并降低涂层的腐蚀防护性能.实验结果表明LDH-V最佳的添加浓度为1.5×10-3mol·L-1.     

类牙釉状丝胶蛋白/羟基磷灰石复合材料的合成及表征

采用化学沉淀法合成了丝胶蛋白(SS)/羟基磷灰石(HAP)复合材料, 并研究了矿化时间对复合材料的影响. X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、透射电镜(TEM/HRTEM)和扫描电镜(SEM)表征结果表明: 在较短的矿化时间内, 合成的SS/HAP为直径约20 nm的复合颗粒; 随着矿化时间的延长, 这些复合颗粒能够沿轴方向组装并融合成类牙釉结构的较大晶体. 文章讨论了其可能的组装机制.     

柔性复合织物电极Graphene/Cotton和MnO_2/Graphene/Cotton的合成及在电化学电容器中的应用（英文）

通过热还原法成功地制备出了柔性复合织物电极石墨烯/棉布(graphene/cotton)。热还原条件对电极的导电性能具有较大的影响。导电柔性织物电极graphene/cotton特有的多级结构使其既有利于进一步负载膺电容材料,又有利于电子和电解质离子的传输与扩散。通过电化学沉积方法,利用导电柔性织物电极graphene/cotton进一步制备出了电极MnO_2/graphene/cotton。利用扫描电子显微镜(SEM),傅里叶变换红外(FTIR)光谱,四探针测试法等表征技术对电极的结构进行了较为详细的表征。结果表明电极MnO_2/graphene/cotton的比电容可以达到536 F?g~(-1)。良好的电化学性能和柔性使得此类电极在柔性储能材料应用中具有极大的应用前景。     

HATR-FTIR-排序法识别中药材紫花地丁及其伪品的研究

采用水平衰减全反射傅里叶变换红外光谱(HATR-FTIR)法测定了紫花地丁及其伪品如白花地丁、犁头草、辽宁堇菜及匍伏堇的根木质部和茎外表皮部的傅里叶变换红外光谱,采用主成分分析法(PCA)比较了正伪品之间的差异程度。结果表明：基于傅里叶变换红外光谱的主成分分析在反映同科同属不同种植物化学组成差异程度上具有应用价值。     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

化学计量中不确定度评定研究进展

测量不确定度是表征合理地赋予被测量之值的分散性的参数。本文针对化学计量不确定度评定基础模型仅适用于线性模型、概率分布为正态分布或缩放位移t分布等局限,介绍了近年来不确定度评定的研究热点:蒙特卡罗方法(Monte Carlo Method,MCM),不确定度评定的来源、评定概念、评估方法及其发展过程,扩大了测量不确定度评定与表示的适用范围。