Organic‐acid‐catalyzed sol–gel route for preparing poly(methyl methacrylate)–silica hybrid materials

In this study, a series of organic–inorganic hybrid sol–gel materials consisting of a poly(methyl methacrylate) (PMMA) matrix and dispersed silica (SiO₂) particles were successfully prepared through an organic‐acid‐catalyzed sol–gel route with N‐methyl‐2‐pyrrolidone as the mixing solvent. The as‐synthesized PMMA–SiO₂ nanocomposites were subsequently characterized with Fourier transform infrared spectroscopy and transmission electron microscopy. The solid phase of organic camphor sulfonic acid was employed to catalyze the hydrolysis and condensation (i.e., sol–gel reactions) of tetraethyl orthosilicate in the PMMA matrix. The formation of the hybrid membranes was beneficial for the physical properties at low SiO₂ loadings, especially for enhanced mechanical strength and gas barrier properties, in comparison with the neat PMMA. The effects of material composition on the thermal stability, thermal conductivity, mechanical strength, molecular permeability, optical clarity, and surface morphology of the as‐prepared hybrid PMMA–SiO₂ nanocomposites in the form of membranes were investigated with thermogravimetric analysis, differential scanning calorimetry, dynamic mechanical analysis, gas permeability analysis, ultraviolet–visible transmission spectroscopy, and atomic force microscopy, respectively. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Synthesis and thermomechanical characterization of polyurethane elastomers extended with α,ω‐alkane diols

A series of polyurethane (PU) elastomers was prepared by the reaction of poly(?‐caprolactone) and 4,4′‐diphenylmethane diisocyanate, which was extended with a series of chain extenders (CEs) having 2–10 methylene units in their structure. The completion of the reaction was confirmed by Fourier transform infrared spectroscopy. The chemical structures of the synthesized PU samples were characterized with Fourier transform infrared, ¹H‐NMR, and ¹³C‐NMR spectroscopy, and the thermal properties were determined by thermogravimetric analysis, DSC, and dynamic mechanical thermal analysis techniques. The mechanical properties were also studied and are discussed. The thermogravimetric analysis and DSC analysis showed that CE length had a considerable effect on the thermal properties of the prepared samples. The dynamic mechanical thermal analysis and damping peaks were also affected by the number of methylene units in the CE length. The elastomer extended with 1,2‐ethane diol exhibited optimum thermal properties, whereas the elastomer based on 1,10‐decane diol displayed the worst thermal properties. Tensile strength and elongation at break decreased with increasing CE length, whereas hardness showed the opposite trend. The glass‐transition temperature moved toward lower temperatures with increasing CE length. The decrease in the glass‐transition temperature and tensile properties were interpreted in terms of decreasing hard segments and increasing chain flexibility. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

用热分析法研究硝化棉的熔化过程

用ＭＤＳＣ，显微镜温台熔点测定仪和固体原位反应池／快速扫描傅立叶变换红外光谱联用装置考察了硝化棉的熔化过程。ＭＤＳＣ曲线表明吸热过程是可逆的，它系由ＮＣ和部分分解凝聚相产物的混合物的固液相变所引起。由ＮＣ的ＭＤＳＣ曲线得到的熔点，熔化含，熔化熵，分解含和分解反应热温熵分别为４７６．８４Ｋ，２０５．６Ｊ．ｇ＾－１，０．４３１２Ｊ．ｇ＾－１．Ｋ＾－１，－２４７５．０Ｊ．ｇ＾－１，－５．２４２Ｊ．ｇ＾－     

Platinum promoted zirconia-sulfate catalysts: one-pot preparation,physical properties and catalytic activity

A new innovative methodology for the single-stage preparation of ZrO₂-SO₄ and Pt/ZrO₂-SO₄ catalysts is reported, based on the sol-gel technique. Catalysts are characterized by analysis, XRPD, BET and IR methods and are tested in the isomerization of butane.     

流延热释电厚膜陶瓷制备单元红外探测器

本文报道采用流延法制备的热释电厚膜陶瓷材料直接装配的单元红外探测器，该方法大大简化了目前探测器的制备工艺，极大地提高了材料的利用率，器件的性能也达到了目前探测器的水平。     

快速启动微型J—T制冷器

在一些特殊应用中，要求把红外探测器必须在几秒钟或更短的时间内冷却到工作状态。微型Ｊ－Ｔ式制冷是常用致冷方式。本文介绍了快速启动冷却红外探测器的Ｊ－Ｔ制冷器的设计及达到快速冷却的方法以及测试结果。     

TiO_2-聚乙烯复合膜的制备及红外光谱对其膜层结构的表征

开发了以Ｔｉ４＋为桥联剂制备无机－有机复合膜的新方法以自制的硅藻土多孔陶瓷为基膜（支撑体），使用浸涂法－热致相转化法相结合制备了ＴｉＯ２－聚乙烯复合膜，并用红外光谱表征了复合膜层与层之间的结合方式和强度，支撑体中的ＳｉＯ２通过Ｔｉ４＋与聚乙烯的分子之间形成了新的化合物型膜层     

碱土金属氧化物催化氧化异丙苯反应研究

考察了碱土金属氧化物CaO、MgO和SrO在催化氧化异丙苯合成过氧化氢异丙苯 (CHP)反应中的性能。3种催化剂的活性顺序为 :CaO >MgO >SrO。采用Hammett指示剂分别表征了碱土金属氧化物的碱强度。碱强度H-=15 0～ 18 4的碱性中心有利于异丙苯过氧化合成CHP反应。采用红外光谱分析了异丙苯在MgO、CaO催化剂表面的吸附态。异丙苯通过异丙基叔碳原子上的氢原子与CaO催化剂表面碱中心发生化学吸附 ,弱化了异丙基叔碳原子上的C—H键 ,从而有利于催化异丙苯氧化合成CHP的反应。MgO与异丙苯的异丙基叔碳上的氢原子的相互作用弱于CaO与异丙苯的异丙基叔碳上的氢原子的相互作用 ,使MgO催化异丙苯氧化的反应活性低于CaO催化异丙苯氧化的反应活性     

Dual reaction capacity of hydrogenated nanodiamond

High temperature hydrogen stream treatment of nanodiamond was shown to produce nanodiamond with bifunctional surface. OH- and different CH-groups were shown to be the main functional groups on the surface. In this article we proposed two main strategies for further chemical modification of hydrogenated nanodiamond. OH-groups were shown to react with different types of acylating agents: anhydrides and chloranhydrides. Chlorination of hydrogenated nanodiamond with molecular chlorine and its subsequent treatment with alkyllithium reagents resulted in formation of alkyl-nanodiamonds. Chlorination was shown to reduce the size of nanodiamonds aggregates. We have also applied suspension-state NMR-H1 spectroscopy to study suspensions of alkyl-nanodiamonds for the first time.     

Vanadium species in new catalysts for the selective oxidation of methane to formaldehyde: Activation of the catalytic sites

New vanadium oxide supported on mesoporous silica catalysts for the oxidation of methane to formaldehyde were investigated by infrared and Raman spectroscopies to identify and characterize the molecular structure of the most active and selective catalytic sites. In situ and operando experiments have been conducted in order to understand the redox and hydroxylation/dehydroxylation processes of the vanadium species. (SiO)₂VO(OH) species were identified in these catalysts in reaction conditions and shown to undergo a deprotonation at 580 °C under vacuum, leading to a site giving a photoluminescence band at 550 nm attributed to reverse radiative decay from the excited triplet state:

(V⁴⁺–O⁻)^*  (V⁵⁺O²⁻). An activation mechanism of vanadium monomeric species with electrophilic oxygen species is proposed.