色谱/质谱联用技术对乙氧-叔丁氧基硅烷水解-聚合行为的研究

采用色谱／质谱联用技术研究了一种复合硅醇盐：乙氧－叔丁氧基硅烷（Ｓｉ（ＯＥｔ）ｘ（ＯＢｕ＾ｔ）４－ｘ）的水解－聚合过程,测定了水解过程不同阶段胶体中各物质的水解行为,空间结构构成以及含量的变化,结果表明：Ｓｉ（ＯＥｔ）（ＯＢｕ＾ｔ）３具有高于Ｓｉ（ＯＥｔ）２（ＯＢｕ＾ｔ）２的水解速率,随着水解的进行,二聚体和三聚体相继形成。     

Microstructure evolution in chelated partially hydrolysed alumina sols during sonogelling

Optically transparent alumina sonogels with optical transmittance of over 90% have been prepared by chemically modifying a partially hydrolysed aluminium sec-butoxide precursor with ethyl acetoacetate. Chelating the alkoxide in a 1:2 molar ratio has permitted an enhanced control over microstructural changes during the sol to sonogel synthesis. Particle size and morphology changes during controlled sonogelling indicate that the sol to sonogel evolution in chelated alkoxides occurs by a dissolution-nucleation process in which the chelated species dissolves and aluminium hydroxide nucleates. The chelated agglomerates break down with increasing amount of water, and finally dissolve into the alcohol rich medium. The breakdown of chelated agglomerates is accompanied by the formation of nanosized aluminium hydroxide particles which grow with water addition into aggregated micron sized, spherical species. The chelated agglomerates evolve from a spherical geometry to a cylindrical morphology to a tapelike structure with a preferred orientation, and finally to a wavy sheet-like matrix. The nano-aluminium hydroxide particles increase in size at every water addition and grow to about 1 μm at the sonogel point.     

新型纤维油剂的研制与应用

植物油与乙醇胺在120～140℃酰胺化反应3～4h，得到植物油烷醇酰胺，讨论了该反应的主要影响因素，通过分析合成产物的红外谱图验证了植物油烷醇酰胺的生成．该合成产物与多种有效成分复配成的纤维油剂的抗静电性好。     

Concerted mechanisms of acid-base catalysis in coordination sphere of metal complexes

Kinetics and mechanisms of the following reactions in organic solvents have been studied: (i) formation of Schiff bases from aniline and derivatives of salicylic aldehyde coordinated to Cu(II) and Zn(II); (ii) substitution of one -diketonate ligand coordinated to Fe(III) by another -diketonate ligand; (iii) formation of coordinated hemiacetals from -diketonate ligands and alcohols in coordination sphere of Fe(III); and (iv) formation of urethanes in coordination sphere of Fe(III) (acac)₂ OR where acac and OR are acetylacetonate and alkoxide anions. Such compounds as aniline, alcohols and phenylacetylene serve as catalysts of these reactions. Their catalytic action is explained by concerted processes of hydrogen atom transfer in cyclic intermediate structures.Presented in part at the Royal Society-U.S.S.R. Academy Workshop on Catalysis, Oxford, April 1989.     

Single-Source Sol-Gel Synthesis of Nanocrystalline ZnAl2O4: Structural and Optical Properties

Nanometer-sized zinc aluminate (ZnAl₂O₄) particles were synthesized from heterometal alkoxides, [ZnAl₂(OR)₈], possessing an ideal cation stoichiometry for the ZnAl₂O₄ spinel. ZnAl₂O₄ is formed at 400°C, which is the lowest temperature reported for the formation of monophasic ZnAl₂O₄. ²⁷Al magic-angle spinning nuclear magnetic resonance spectroscopy revealed that ZnAl₂O₄ possesses an inverse structure at <900°C, while the normal spinel phase is observed at higher temperatures. The homogeneity of the in-depth composition and Zn:Al stoichiometry (1:2) was confirmed by electron spectroscopy for chemical analysis. Evaluation of the valence-band spectra of ZnAl₂O₄ and ZnS suggested that the hybridization of O 2 p and Zn 3 d orbitals is responsible for lowering the bandgap in the latter. The average crystallite size showed an exponential relationship to the calcination temperature (X-ray diffractometry and transmission electron microscopy data). The optical spectra of different spinel powders (average particle sizes, 20–250 nm) showed that the absorption edge exhibits a blue shift as particle size decreases.     

含铝PSBR复合橡胶的制备及其力学性能

利用铝的醇盐与PSBR季铵盐乳液反应,制成含铝有机－无机杂化弹性体胶片,再与天然橡胶进行并用,制得含铝PSBR复合硫化胶,这种复合硫化胶具有优良的力学性能和独特的抗震作用,用IR和NMR以及其它方法分析了其相关结构.     

Template Effect on Structure and Morphology of Ni(OH)2 Powders Prepared by Hydro-chemical Method

Ｐｒｏｐｅｒｔｉｅｓｏｆｐｏｗｄｅｒｓａｒｅｃｌｏｓｅｌｙｒｅｌａｔｅｄｔｏｔｈｅｉｒｓｔｒｕｃｔｕｒｅｓａｎｄｍｏｒｐｈｏｌｏｇｉｅｓ ,ｍａｉｎｌｙｉｎｃｌｕｄｉｎｇｐａｒｔｉｃｌｅｓｉｚｅ,ｓｈａｐｅａｎｄｃｒｙｓｔａｌｌｉｎｉｔｙｏｆｐｏｗｄｅｒｓ[1].Ｆｏｒｐｏｗｄｅｒｓｐｒｅｐａｒｅｄｂｙｈｙｄｒｏ ｃｈｅｍｉｃａｌｍｅｔｈｏｄ ,ｓｔｒｕｃｔｕｒａｌａｎｄｍｏｒ ｐｈｏｌｏｇｉｃａｌｃｏｎｔｒｏｌｏｆｐｏｗｄｅｒｓｗｅｒｅｃｏｎｖｅｎｔｉｏｎａｌｌｙｒｅａｌｉｚｅｄｂｙｔｈｅａｄｊｕｓｔｍ…     

在线基体消除-毛细管离子色谱测定有机溶剂中的痕量阴离子

建立了在线基体消除-毛细管离子色谱测定有机溶剂中痕量阴离子的方法。有机溶剂样品经过阴离子浓缩柱（MAC200整体柱）,痕量目标阴离子被浓缩的同时,有机溶剂不被保留而去除,接着目标离子转入毛细管离子色谱系统进行分析。六种阴离子（氟离子、氯离子、亚硝酸根、硝酸根、硫酸根和磷酸根）在1-100μg/L线性范围内,相关系数（r2）为0.9991～0.9999,考察的阴离子检出限（以S/N=3计）为2.2-34.8ng/L。用于实际样品检测,取得了很好的效果。     

电路板表面无机阴离子和有机酸的离子色谱法研究

建立了一种梯度淋洗离子色谱法分析印刷电路板中无机阴离子和有机酸污染物的方法。印刷电路板经体积分数为75%的异丙醇提取液提取后,经预处理柱除去异丙醇对测定的干扰,以阴离子交换分离柱分离,氢氧化钠淋洗液梯度洗脱。方法简单可行,几种离子的相对标准偏差在6%以下,回收率达到92%～105%,可用于印刷电路板的质量控制。