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     

合成十二烷基葡萄糖苷的工艺条件

采用对甲苯磺酸为催化剂 ,以D 葡萄糖和正十二醇为原料直接合成十二烷基糖苷 ,研究了工艺条件对反应速率、产物收率与色泽的影响。结果表明 ,催化剂用量对产物色泽无影响 ,适宜的工艺条件为 :正十二醇 /D 葡萄糖 (摩尔比 ) =4∶1,反应温度 110～ 12 0℃ ,反应时间 4h ,反应压力 4kPa ,搅拌速率大于 840r/min ,对甲苯磺酸 /D 葡萄糖 (摩尔比 ) =1.5 %,MgO为较好的中和剂。产物为乳白色 ,十二烷基糖苷总收率大于89%。     

组成对MgO-ZrO2-CaO系合成料结构与性能的影响

以脱硅锆、轻烧氧化镁、消石灰为原料，进行了MgO-ZrO2-CaO系原料的合成，研究了化学组成(包括ZrO2含量、CaO／ZrO2比)，烧成温度，杂质等对合成料性能和组织结构的影响。     

Very Long SiC‐Based Coaxial Nanocables with Tunable Chemical Composition

We present a simple process for the fabrication of very long SiC‐based coaxial nanocables (NCs). The versatility of this technique is confirmed by the ability to change the chemical composition of the NC outer layers from silica to carbon and boron nitride. The NCs consist of a SiC core approximately 30 nm in diameter with lengths up to several hundred of nanometers. The thickness of the coating is in the range 2–10 nm. The morphology and structural characterization of the NCs is investigated by scanning electron microscopy (SEM) and high‐resolution transmission electron microscopy (HRTEM), respectively, and their chemical composition is probed by electron energy loss spectroscopy (EELS). A vapor–solid growth mechanism is proposed to explain the growth of SiC‐based NCs of various chemical compositions, depending on the chemical nature of the vapor phase. Because of the large quantity of very long and interlaced NCs produced during the synthesis, the macroscopic aspect of the as‐grown material is like a self‐supported felt.     

Accurate and simple synthesis formulas for coplanar waveguides

Simple and accurate closed‐form formulas obtained by using a differential evolution algorithm are presented for the synthesis of coplanar waveguides (CPW). The results of the synthesis formulas proposed in this article are compared with those of the quasi‐static analysis, the synthesis formulas reported by the other researchers and also the experimental works available in the literature. The accuracy of the proposed synthesis formulas is found to be better than 0.75% for 9256 CPWs samples. © 2008 Wiley Periodicals, Inc. Int J RF and Microwave CAE, 2008.     

3-N-丙酰基-2-芳基-5-(3-碘苯基)-1,3,4-(口恶)唑啉类化合物的合成及表征

以3-碘苯甲酸为原料,在浓硫酸作用下与乙醇反应制得3-碘苯甲酸乙酯(1),再以无水乙醇为溶剂,在105℃化合物1与80％的水合肼反应8 h,制得3-碘苯甲酰肼(2)。在无水乙醇中,在90～95℃化合物2分别与4-甲基苯甲醛、2-氯苯甲醛、4-氯苯甲醛、4-羟基苯甲醛、2,4-二氯苯甲醛、4-甲氧基苯甲醛、3-硝基苯甲醛、4-硝基苯甲醛和4-二甲氨基苯甲醛反应得到相应的酰腙[3(a～i)]。最后化合物3(a～i)分别与丙酸酐脱水环化成了3-N-丙酰基-2-芳基-5-(3-碘苯基)-1,3,4-(口恶)唑啉类化合物[4(a～i)],收率分别为86．2％,70．5％, 80．1％,68．2％,62．4％,75．2％,73．2％,70．5％和63．2％。并通过元素分析,IR,1H NMR和MS对化合物4(a～i)的结构进行了表征。     

Direct synthesis and catalytic performance of ultralarge pore GaSBA-15 mesoporous molecular sieves with high gallium content

Mesoporous GaSBA-15 molecular sieves with different n_Si/n_Ga ratios have been directly synthesized using Pluronic 123 triblock polymer as a structure-directing agent by pH-adjusting method. The mesoporous materials have been characterized using ICP-AES, XRD, N₂ adsorption, ⁷¹Ga-MAS NMR, SEM and TEM. ICP-AES studies show a high amount of gallium incorporation on the silica pore walls. The structural and textural properties of calcined GaSBA-15 are characterized by XRD and N₂ adsorption. ⁷¹Ga MAS NMR results demonstrate that a high amount of tetrahedral-gallium could be substituted for Si in the framework of SBA-15. TEM and FE-SEM images show the uniform pore diameter and rope-like hexagonal mesoporous structure of GaSBA-15. These GaSBA-15 materials have been used as catalysts for vapour-phase t-butylation of 1,2-dihydroxybenzene (DHB) for selective synthesis of 4-t-butylcatechol (4-TBC) under different reaction conditions. GaSBA-15(10) gave the highest 93.2% conversion of DHB and 95.7% selectivity of 4-TBC as compared with other GaSBA-15 catalysts.     

丙烯酸二甲氨基乙酯的合成

以丙烯酰氯与二甲氨基乙醇为原料 ,乙醚为溶剂 ,过量的二甲氨基乙醇为缚酸剂合成了丙烯酸二甲氨基乙酯。较佳实验条件为 :丙烯酰氯 /二甲氨基乙醇 /乙醚 (物质的量比 ) 1∶2 .0 5∶5 .6 ,反应温度 5℃ ,反应时间 4h ,w(吩噻嗪 ) 0 .5 0 %,产物为无色透明液体 ,相对密度 0 .943 1( 2 0℃ ) ,折光率为 1.435 2 ,收率大于 91%。