胶粉/热塑性塑料共混材料的研究

以胶粉及通用塑料PP和LLDPE为原料,研究了原料种类、相容剂等对胶粉/热塑性塑料共混材料性能的影响,制得了性能较好的共混材料。通过热分析和扫描电镜对制得的共混材料进行分析表征,表明胶粉和LLDPE有较好的相容性及较强的结合力。     

含二氮杂萘酮结构聚醚酮酮的合成及表征

以１,４ 二（４ 氯代苯甲酰基）苯与４ （４ 羟基苯基） ２,３ 二氮杂萘 １ 酮单体经亲核取代反应,合成了含二氮杂萘酮结构聚醚酮酮聚合物．用ＦＴ ＩＲ、１Ｈ ＮＭＲ、ＤＳＣ、ＴＧＡ、Ｘ 射线衍射等方法对聚合物进行了表征,研究了聚合物的溶解性能．结果表明,该聚合物是一种具有高热稳定性的可溶性无规聚合物．     

Thermal studies on beryllium titanyl/zirconyl oxalates

Beryllium titanyl oxalate tetrahydrate and beryllium zirconyl oxalate tetrahydrate were prepared in aqueous medium and characterized by elemental analyses, magnetic susceptibility measurements and IR spectral studies. The thermal behaviour of these compounds under non-isothermal conditions was investigated by thermogravimetric, derivative thermogravimetric and differential scanning calorimetric (DSC) techniques. The intermediates obtained at the end of the various thermal decomposition steps were identified on the basis of elemental analyses and IR spectral studies. The decomposition proceeds through three major steps, viz, dehydration of the hydrate, decomposition of the oxalate to carbonate and decomposition of the carbonate to oxide. The graphical method of Coats and Redfern was employed to calculate kinetic parameters such as apparent activation energy and order of reaction. Heats of reaction for the different decomposition steps were calculated from the DSC curves.     

新型含环己烯结构的甲基二氮杂萘联苯型聚醚酮的合成及表征

合成了一种新型聚合单体 1 甲基 4,5 二 (4 氯代苯甲酰基 )环己烯 ,并与 4 (3 ,5 二甲基 4 羟基苯基 ) 2 ,3 二氮杂萘 1 酮单体经亲核取代反应 ,成功地合成了含环己烯结构的杂环联苯型聚醚酮聚合物 .用FT IR、1H NMR、DSC、X 射线衍射等方法对聚合物进行了表征 ,并研究了聚合物的溶解性能 .结果表明 ,聚合物是一种具有较高的玻璃化温度的可溶性无规共聚物 .聚合物含有不饱和双键结构 ,是一种反应性高分子     

聚环氧氯丙烷聚氨酯／聚甲基丙烯酸甲酯互穿网络聚合物的相容性与力学性能

用同步法合成了聚环氧氯丙烷聚氨酯／聚甲基丙烯酸甲酯互穿网络聚合物［ＰＵ（ＰＥＣＨ）／ＰＭＭＡＩＰＮ］，调节ＩＰＮ中两组分组成比制备出由完全弹性体、增强弹性体、增韧塑料到脆性塑料多种高聚物合金材料．用ＤＳＣ、动态力学谱、ＴＥＭ对ＩＰＮ的研究结果表明，ＰＵ（ＰＥＣＨ）／ＰＭＭＡＩＰＮ的两组分是完全相容的；同时对各种组成比的ＩＰＮ材料进行力学性能测试，用相容性ＩＰＮ中互穿、缠结结构解释其力学行为，并用ＳＥＭ对断面形貌进行了观察解释．     

Synthesis of poly(Schiff-base)s by organometallic processes

Some new monomers with Schiff-base structures and bromine final atoms were obtained by combining condensation reactions of dialdehydes or diamines with p-bromoaniline or p-bromobenzaldehyde. The corresponding polymers were synthesized by Ni- or Pd-catalyzed polycondensation reactions in combination with 2,5-dihexylbenzene-1,4-diboronic acid. The new structures were characterized by spectral methods (¹H NMR, IR, UV-vis) as well as by thermal analyses (TGA, DSC).     

Neodymium and europium complexes with amides and cyclic aminoxides

Complexes of neodymium and europium with amides and aminoxides were synthesized and characterized by complexometric analyses with EDTA, CHN microanalytical procedures, IR absorption spectra, absorption spectra of neodymium complexes, emission spectrum of europium compounds at 77 K, thermogravimetric analyses in N2 and differential scanning calorimetry (DSC) in N2. Infrared spectroscopy results revealed that the nitrate molecules are bound to the central ions as bidentate. Thermogravimetric plots indicated that the decomposition of the complexes occurs in the range 363-1163 K and resulted in the formation of Ln₂O₃ residues. This revised version was published online in August 2006 with corrections to the Cover Date.     

含羧酸稀土光敏剂降解PVC塑料的可降解研究

以羧酸共生稀土作为PVC塑料紫外光氧化降解的光敏剂,采用人工加速老化实验、户外曝晒实验等方法进行降解试验,并用红外光谱,紫外光谱和凝胶色谱等方法对含羧酸共生稀土光敏剂可降解PVC塑料的可降解性能进行了研究。初步探讨了羧酸共生稀土敏化PVC膜光氧化降解的作用机理。结果表明,羧酸共生稀土(如La、Ce、Pr等)对PVC分子的结构具有明显的光敏化降解作用,并具有抑制PVC在光照过程中发生交联的作用。     

不同旋光度PLGA的制备及其结晶性能研究

以消旋丙交酯、左旋丙交酯和乙交酯为原料,以辛酸亚锡为引发剂,在高真空条件下本体熔融开环聚合,制得一系列不同旋光度的丙交酯乙交酯共聚物(PLGA),其结构经1H NMR, IR, XRD和DSC表征.并采用DSC研究了PLGA的熔体结晶行为,结果表明其结晶性能随其旋光度的减少而显著降低,甚至不结晶.     

A continuous process for solid-state dehydration,amorphization and recrystallization of metoclopramide HCL monohydrate studied by simultaneous DSC-FTIR microspectroscopy

The purpose of this study was to investigate the thermal-induced solid-state characterization of metoclopramide hydrochloride monohydrate (MCP H₂O) by using a combination of differential scanning calorimetry (DSC) and Fourier-transform infrared (simultaneous DSC-FTIR) microspectroscopy. The DSC and thermogravimetric (TG) analyses were also carried out. The result indicates that a continuous process of dehydration, amorphization and recrystallization for MCP H₂O in the solid state was easily evidenced via the thermal responsive IR spectral changes by using this simultaneous DSC-FTIR microspectroscopy. In the heating course, one mole of water was first dehydrated from the MCP H₂O sample beyond 77 °C, was then quickly transformed to an amorphous form due to the appearance of weak broad IR bands, and continuously recrystallized from 148 °C by showing the sharp IR bands. This one-step novel simultaneous DSC-FTIR microspectroscopy might be available for studying the changes in the progressive processes of the thermal-dependent solid-state characterizations of drugs.     

PBT/PEG型聚醚酯的鉴定

采用红外光谱、核磁共振和DSC热分析手段对一种未知聚合物样品进行表征。通过对样品红外谱图的吸收峰位和强度及对其核磁共振氢谱中各质子化学位移归属的分析,判明该样品为PBT/PEG型聚醚酯弹性体,且不含游离的聚乙二醇组分。样品的DSC测试表明其与PBT/PEG型聚醚酯的热行为较相符。该分析为此类聚合物提供了一种简单、快速且结果可靠的鉴定方法。     

Molecular state of chlorpheniramine in resinates

Chlorpheniramine (CPM) maleate was prepared as a series of resinates by the batch method. The several resinates were investigated by differential scanning calorimetry (DSC), X-ray powder diffraction (XRPD) and infrared (IR) spectrometry. The results from DSC and XRPD showed that the molecular state of the entrapped drug changed from the crystalline to amorphous state. IR spectra indicated that only CPM species was entrapped in the resinates. Moreover, it also showed that the positively charged amine group of the drug interacted with the sulfonate groups of the resin by ionic association. The dissolution of the drug and resinates was also studied where it was found that the dissolution of the resinates was retarded by their crosslinked structure and markedly affected by the quantity of resin.     

Zerovalent metal polymer composites. II. Metal–polymer microdispersions

Metallization of water-soluble polymers incorporating metal-binding ligand is achieved by binding palladium ions at substoichiometric quantities, followed by reduction to polymer–zero-valent palladium complex and deposition of transition metal ions by electroless plating solutions. The polymers studied include poly[N,N,N-trimethyl-N-(m- and p-vinylbenzyl)ammonium chloride], poly-L -glutamic acid, poly-L -lysine, and a copolymer of 2-phenylhydroquinone-2-amino-phthalic acid. Noble metal polyelectrolyte solutions were directly reduced with dimethylamineborane to stable microdispersions. The reactive nickel, cobalt and copper microdispersions were coated on KODAK ESTAR filmbase. Scanning electron microscopy (SEM), ESCA, and IR were used for material characterization. Conductivity and magnetic properties were also measured. Hydrophobic materials such as graphite and fluorinated graphite were metallized in organic solvents using hydrophobic trioctylammonium–tetrachloropalladate as the activating noble metal complex. The metallized conductive graphites were evaluated for their electrochemical properties.     

两个新的氢键诱导液晶化合物的合成

通过４－丁氧基苯甲酸（４ＢＡ０与两个手性取代的苯乙烯基吡啶（ＶＳＺ及ＬＳＺ）间的氢键作用合成了２个新的液晶化合物，用ＤＳＣ、偏光显微镜研究了其液晶行为，并由红外光谱证实了分子间氢键的存在，形成的复合物４ＢＡ－ＶＳＺ具有手性近晶Ｃ相。     

Characterization of the solid phases of paracetamol and fenamates at equilibrium in saturated solutions

Differential scanning calorimetry (DSC), supported by hot stage microscopy, IR spectroscopy and X-ray powder diffractometry, was used to investigate the characteristics of the solid phases of mefenamic, niflumic, and flufenamic acids and of paracetamol, before and after equilibration with saturated solutions in different solvents. Mixtures of Lewis base (dioxane and ethyl acetate) and amphiprotic solvents (ethanol and water) were prepared for evaluating the influence of both nature and polarity of the solvents. Solid-state analysis performed on the original samples (commercial products) made it possible to establish that paracetamol, mefenamic acid and flufenamic acid were in their respective Form I. No polymorphic modifications are known for niflumic acid. Paracetamol, niflumic and mefenamic acids did not show any change after equilibration with the various solvents or solvent mixtures, regardless of their different chemical nature. In contrast, DSC, IR and X-ray analyses revealed the partial recrystallization of flufenamic acid into its polymorphic Form III in solid phases at equilibrium with ethanol, ethyl acetate and their blends, as well as in dioxane-water mixtures containing 30 to 100% dioxane and in ethanol-water mixtures with a water content less than 50%. This revised version was published online in July 2006 with corrections to the Cover Date.     

Synthesis and Characterization of Novel Polyamines Containing Different Substitute Groups Via Chemical Oxidative Polymerization

In this study, polymers of substitute aromatic amine compounds were synthesized by chemical oxidative polycondensation in aqueous alkaline medium using NaOCl as oxidant. The structures of synthesized compounds were confirmed by FT‐IR, UV‐Vis and NMR analyses. The characterizations of synthesized compounds were made by fluorescence, TG‐DTA, DSC, scanning electron microscopy (SEM) and Brunauer‐Emmett‐Teller (BET) surface area measurements. In addition, electrochemical and electrical conductivity values of compounds were carried out with cyclic voltammetry (CV) and four points probe technique measurements, respectively. Synthesized polymers viewed structural change, optical, electrochemical and thermal differences.     

含咔唑生色团的三聚磷腈分子玻璃的合成

含咔唑生色团的三聚磷腈分子玻璃的合成;三聚磷腈;后重氮偶合;咔唑;光折变分子玻璃     

Influence of solid corrodents on high-temperature oxidation of cobalt powder

Complexes between members of a homologous series of alkylparabens and b-cyclodextrin (b-CD) have been prepared by both kneading and co-precipitation methods and their behaviour studied by differential scanning calorimetry (DSC), thermogravimetric (TG), infrared (IR) and powder X-ray diffraction (PXRD) techniques. PXRD revealed that complexation did occur by both the kneading and co-precipitation methods. DSC and IR techniques confirmed these results and TG indicated the presence and number of water molecules in each complex. This revised version was published online in July 2006 with corrections to the Cover Date.     

Photochromism of polymorphic 4,4'-methylenebis(N-salicylidene-2,6-diisopropylaniline) crystals

4,4[prime or minute]-Methylenebis(N-salicylidene-2,6-dialkylaniline) derivatives were prepared and their structures were determined by (1)H NMR, IR, DSC and X-ray crystallographic analyses. The 2,6-diisopropylaniline derivative yielded definite polymorphic crystals: the space groups of the crystals were C2/c and P2(1)/n, respectively. It was found that both polymorphs were similarly photochromic but the thermal stability of the photochrome was different due to the variance of the shape of molecule and cavity in each crystal.     

Thermal analysis of lipoic acid and evaluation of the compatibility with excipientes

Differential scanning calorimetry (DSC) was used as a screening technique for assessing the compatibility of lipoic acid with some currently employed cosmetic excipients. In the first phase of the study DSC was used as a tool to detect any interaction. Based on the DSC results alone, methyl p-hydroxybenzoate, propyl p-hydroxybenzoate, butylated hydroxytoluene, non ionic self emulsifying wax, propylene glycol and acetylated lanolin were found to exhibit interaction with lipoic acid. Stressed binary mixtures (stored at 50 °C for 1 week) of lipoic acid and excipients were evaluated by HPLC. Binary mixtures were evaluated by IR spectroscopy.