Preparation of Small Particle Sized ZnAl-Hydrotalcite-Like Compounds by Ultrasonic Crystallization

Ultrasonic technology has been intensively studied recently due to its special features. In this paper, an ultrasonic crystallization method was introduced for the preparation of ZnAl-Hydrotalcite-Like compounds (ZnAl-HTLcs). Samples with high crystallinity, small particle size and narrow particle size distribution were obtained and fully characterized using conventional techniques of XRD, FT-IR and TGDTA. The results prove that both ultrasonic frequency and ultrasonic power have effects on the sizes of the product particles. By varying the ultrasonic power from 250 W to 88 W, with the ultrasonic frequency fixed at 59 kHz, the median particle size of the samples increased from 0.37 μm to 0.82 μm. By altering the hydrothermal treatment time from 1 h to 5 h at 110℃, the median particle size of ZnAl-HTLcs synthesized via ultrasonic crystallization increased from 0.88 μm to 1.11 μm.     

Growth transition and morphology change in polypropylene

The growth rate of isotactic polypropylene is deduced from microscopic observations during isothermal crystallizations. A change in the growth regime is observed at 138 C and interpreted as a Regime III Regime II transition, according to Hoffman's kinetic theory of polymer crystallization. A Regime II Regime I transition is also theoretically predicted at 155 C, i. e. at a temperature outside the investigated temperature range. The Regime III Regime II transition is related to the positive to negative change in the spherulite birefringence, which is generally attributed to a change in the organization of crystalline lamellae: quadritic arrays of intercrossing lamellae atT _c < 138 C (Regime III) and preferentially radiating lamellae atT _c > 138 C (Regime II). It is suggested that such a morphological change could be interpreted using the concept of non-adjacent re-entry introduced in Hoffman's kinetic theory. This interpretation could also explain the interspherulitic ruptures observed in negative spherulites.     

孔壁部分有序化的介孔二氧化硅材料的合成与表征

采用一种“改进的二次晶化”的方法处理介孔二氧化硅SBA-15. 用X射线衍射(XRD)、 透射电镜(TEM)、 电子衍射(ED)、 红外光谱(FTIR)以及固体核磁共振(NMR)等多种技术对样品进行了表征.　结果表明， 在所得样品的孔壁中, 原子的排列方式与普通介孔二氧化硅材料的孔壁不同， 显示一定程度的有序性. 同时, 高度有序的介孔结构得到很好的保持, 且样品的水热稳定性大幅度提高.     

EFFECT OF CRYSTALLIZATION TEMPERATURE ON MCM-41 SYNTHESIS

在Ｎａ２ＯＳｉＯ２ＣＴＡＢＨ２Ｏ四元水热体系中系统地考察了晶化温度对中孔ＭＣＭ４１分子筛合成及其骨架结构的影响。实验结果表明，提高晶化温度虽然能明显加快晶化速率，缩短晶化时间，但同时样品的结晶度和中孔骨架结构的有序度却被迅速破坏。这些特点与传统沸石的合成过程完全不同，其原因主要是合成ＭＣＭ４ｌ时所用的模板剂及其在合成中所起的模板作用与传统沸石完全不同。相对低的晶化温度（如１００℃）有利于高质量和高热稳定性的中孔ＭＣＭ４ｌ分子筛的合成。     

尼龙6,6(PA_(6,6)及其共混物结晶性能的研究

<正> 尼龙6,6(PA_(6,6))是一种典型的结晶性工程塑料,被广泛应用于纺织、机械制造等行业,但其加工温度范围较窄,耐热性差。聚醚砜(PES)具有较高的玻璃化转变温度,是非晶聚合物,可以诱发某些结晶聚合物结晶。PES与PA_(6,6)共混体系的研究报道较少,本文用熔融法将PES与PA_(6,6)制成共混物,企图改善PA_(6,6)的结晶性,以提高其耐热性,取得了较理想的结果。     

Crystallization-induced asymmetric transformation of chiral-at-metal ruthenium(II) complexes bearing achiral ligands

Recently, we observed that the enantiopure Lambda form of the tributylammonium salt of the chiral anion tris[tetrachlorobenzene-1,2-bis(olato)]phosphate, also named Trisphat, was able to induce an efficient resolution of a Delta,Lambda racemic mixture of cis-[Ru(dmp)2(NCCH3)2](PF6)2 (dmp=2,9-dimethyl-1,10-phenanthroline) due to the spontaneous and selective precipitation of the heterochiral pair [Delta-Ru(dmp)2(CH3CN)2][Lambda-Trisphat]2. We report here that the combination of such a stereoselective precipitation process and irradiation results in the quantitative conversion of the initial [Ru(dmp)2(NCCH3)2]2+ racemate into only one of the two enantiomers. This is the first example in inorganic chemistry of an asymmetric transformation that leads to a chiral complex with no chiral ligand. Finally, three new racemic ruthenium bis(diimine) complexes, namely [Ru(dmp)2(NCCH3)Py](PF6)2 (Py=pyridine), [Ru(dmp)2(1,3-diaminopropane)](PF6)2, and [Ru(dmp)2(ethylenediamine)](PF6)2 were synthesized. For all of them, crystallization-induced asymmetric transformation proved to be an efficient way of obtaining the corresponding optically active chiral-at-metal complexes in high yields and with excellent stereoselectivities.     

Syntheses and properties of related polyoxadiazoles and polytriazoles

New aromatic poly-1,2,4-triazoles and poly-1,3,4-oxadiazoles are studied as thermally stable membrane materials. Various groups were introduced onto the pendant phenyl groups of poly-1,2,4-triazoles. Glass transition temperature, degradation temperature, and cold crystallization behavior were studied as a function of these groups. Cold crystallization appeared to be highly sensitive to macromolecular regularity. The solubility of poly-1,3,4-oxadiazoles was highly improved upon incorporation of 5-t-butylisophthalic, 1,1,3-trimethyl-3-phenylindane, 4,4′-(2,2′-diphenyl) hexafluoro propane, and diphenyl ether groups into the polymeric main chain, whereas the high glass transition temperatures and degradation temperatures typical for aromatic poly-1,3,4-oxadiazoles were maintained. © 1994 John Wiley & Sons, Inc.     

Crystallization kinetics of the monoclinic modification of poly(3,3-dimethyl oxetane)

Poly(3,3-dimethyl oxetane) fractions ranging in number average molecular weights from 18500 to 130000 have been isothermally crystallized from the relaxed melt state in the temperature range from 12 to 44 °C, where only the monoclinic modification is formed. The influence of molecular weight and undercooling in crystallization kinetics has been analyzed. The level of crystallinity is very slightly dependent on molecular weight but the influence of this parameter on the time scale of the crystallization is relatively pronounced. The crystallization temperature coefficient was determined and it was found a constant value of the product of the interfacial energies in the range of molecular weights which has been analyzed. Growth rate measurements were carried out for fraction ¯M _n=130000 and it was found that the temperature coefficients for overall and growth rates are equal. Finally, the comparison of the experimental results for this polymer with those reported for poly(oxetane) shows two main differences: first, the crystallization rate is slower for poly(3,3-dimethyl oxetane) and second, the temperature coefficient is smaller for this polymer.     

Fraktionierte Kristallisation von Ammonium- und Magnesiumdoppelnitraten der Ceriterden; Bestimmung der Trennfaktoren und Vergleich der Trennwirkung

Summary The Separation Factors for Pr/La, Nd/Pr, and Sm/Nd, characterizing the crystallization of ammonium and magnesium double nitrates under practical conditions, were determined analytically and are discussed. They confirm that La and Pr can be separated better by fractional crystallization of ammonium double nitrates, whereas in the presence of Sm the magnesium double nitrates are preferable.

     

Effect of multi-walled carbon nanotubes on non-isothermal crystallization kinetics of polyamide 6

The non-isothermal crystallization behaviors of multi-walled carbon nanotubes (MWNTs)/polyamide 6 (PA6) composites were investigated by differential scanning calorimetry (DSC). Three methods, namely, Avrami, Ozawa and Mo, were carried out to analyze the non-isothermal crystallization data. The results showed that the MWNTs in PA6 acted as effective nucleation agents. However the crystallization rate of composites obtained was lower than that of the neat PA6. It is indicated that the presence of MWNTs influenced the mechanism of nucleation and the growth of PA6 crystallites.