Characterization of the reactivity of limestones with SO2 in a fluidized bed reactor

The reaction between SO₂ and calcined limestone particles has been studied in a fluidized bed combustor. Measurements of sorbent reactivity with SO₂ were made for small batches of limestone injected into the combustor. Simultaneous continuous combustion of bituminous coal provided conditions like those of a boiler for study of the sulphation reaction. A semi-empirical rate model of the CaO-SO₂ reaction has been developed. External mass transfer of SO₂, diffusion within the particles and chemical reaction are taken into account. The limestone reactivity with SO₂ is characterized by two parameters which are dependent on the temperature and sorbent particle size. A model for predicting the limestone requirements in a fluidized bed boiler has been developed. Parameters from the batch experiments are included. The predictions for sulfur retention agree with the experimental results. In addition, effects of operating conditions (gas velocity, recycle, limestone particle size) on the retention of SO₂ were simulated using the model.     

电泳沉积法γ-Al2O3微孔膜的制备与表征

采用电泳沉积法制备γ－Al2O3微孔膜，考察了干燥及烧成制度对膜形成的影响，并用IR，XRD，SEM，N2吸附－脱附等测试手段对γ－Al2O3微孔膜进行了表征。结果表明：采用电泳沉积法可成功地制备均匀的γ－Al2O3保护膜；实验中采用室温慢速干燥法，制得了完整的凝胶膜，经过焙烧可获得与基片结合良好的γ－Al2O3多孔膜，在焙烧过程中，γ－AlOOH发生如下的晶型转变：γ－AlOOH→345℃γ－Al2O3，并且随着焙烧温度的升高，γ－Al2O3膜的结晶性得到改善。此外，γ－Al2O3膜的断面结构较疏松，膜厚度大面均匀：一次成膜厚度达十几μm，γ－Al2O3微孔膜的孔径尺寸为纳米级。     

异佛尔酮二异氰酸酯三聚体的合成

合成了3－异氰酸酯基亚甲基－3，3，5－三甲基环己基二异氰酸酯（IPDI）三聚体，对合成中催化剂，反应温度、反应时间等进行了探讨，并用红外光谱进行了表征。结果表明，采用醋酸钾化催化剂，在50－90℃下反应，再经脱催化剂处理，可制得IPDI三聚体。     

用二氧化硅表面改性纳米二氧化钛的制备及表征

针对二氧化钛(TiO2纳米颗粒在水性涂料中极易团聚、分散性差的问题,以提高TiO2分散稳定性为目的,用并流中和法,以锐钛矿型纳米TiO2粉体为载体,硅酸钠(Na2SiO3)为包覆剂,用硫酸(H2SO4)调节pH值,成功地在纳米TiO2表面包覆致密的SiO2膜.借助Fourier变换红外光谱(Fourier transform infrared spectroscopy,FTIR)、X射线衍射技术(X-ray diffraction,XRD)和X射线能量散射谱(X-ray energy dispersive spectroscopy,EDS),表征样品的键合情况、相态结构、表面的化学成分,同时测定包覆改性前后的纳米TiO2比表面积和酸溶性.FTIR和EDS结果表明:该包覆方法可行,氧化硅(SiO2)以化学键合的方式沉积在纳米TiO2表面,在包覆层和纳米TiO2颗粒之间的界面上形成了Ti-O-Si键.酸溶实验分析和XRD结果证实:在TiO2纳米颗粒表面包覆了一层致密SiO2膜.比表面测定的结果显示:改性后TiO2的比表面积随质量分数m(SiO2):m(TiO2)增加而减小.     

Catalytic hydrogenation of nitrile rubber using palladium and ruthenium complexes

The catalytic hydrogenation of acrylonitrile‐butadiene copolymer (nitrile rubber, NBR) using Pd(OAc)₂ or RuCl₂(PPh₃)₃ catalysts has been investigated in order to produce a totally saturated nitrile rubber. The hydrogenation of NBR is effective with both catalysts and achieved total conversion under the appropriate reaction conditions. In the case of palladium the effects of reaction parameters such as reaction temperature, pressure, time, catalyst concentration, and NBR concentration have been investigated. Even though both ruthenium‐ and palladium‐based catalysts are effective in the production of HNBR, the former requires harsh reaction conditions and has the drawback of gel formation under high conversion, motivating the migration to RuCl₂ (PPh₃)₃ as an alternative catalyst. The degree of hydrogenation was determined by IR and NMR spectroscopy. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007     

Micropore characterization using the Dubinin-Astakhov equation to analyze high pressure CO2 (273 K) adsorption data

The characterization of the pore structure of microporous materials is of interest because of the usefulness of these materials in many applications. Of these, the characterization of carbon adsorbents is particularly problematic because of the presence of small pores with size on the order of small molecules (micropores) along with a wide distribution of pore sizes, and their non-crystalline structure. In this paper, we present results obtained using the Dubinin-Astakhov equation to analyze data from high pressure CO₂ adsorption at 273 K to characterize two sets of microporous carbons. Our results support the conclusions of previous workers that the Dubinin-Astakhov (DA) equation is able to linearize adsorption data that gives rise to curved Dubinin-Radushkevich plots. However, when applied over different ranges of relative pressure on the adsorption isotherm, the Dubinin-Astakhov plots result in different values of micropore volume and characteristic adsorption potential. Furthermore, DA analysis of CO₂ (273 K) adsorption data over a wide range of pressures (10^–3–22000 Tort), gives results different from DA analysis of CO₂ (273 K) isotherms measured at low pressures only (10^–3–830 Tort). It would appear desirable to apply the DA equation to data that reflects the entire range of micropore filling on the adsorption isotherm, as opposed to data over a limited relative pressure range. For CO₂ adsorption at 273 K, this would necessitate adsorption studies at high pressures, to about 28 atm. Micropore volumes obtained in this manner, agreed with the total pore volumes determined by nitrogen (77 K) adsorption for all the activated carbons studied.     

Study of the deactivation and regeneration of copper chromite on γ-alumina and magnesium chromite on γ-alumina catalysts for fuel combustion

The causes of the deactivation of catalysts for fuel combustion MeCr₂O₄/ -Al₂O₃ (Me = Cu or Mg) have been investigated using a variety of complex physical-chemical methods: IRS, ESDR, XPS, TPD and a pulse microcatalytic method. It has been concluded that the observed deactivation of catalysts during fuel combustion is due to the combined effect of high temperatures and reduction media.     

莫来石纤维多孔陶瓷负载性能研究

用酸性偏磷酸盐作粘结剂、加压排液法成型制备了孔隙率高达96％的莫来石纤维多孔陶瓷，采用真空浸渍法，对其负载稀土复合金属氧化物La0.8Sr0.2CoO3的性能进行了研究，考察了浸渍时间、浸渍次数对负载量的影响，得出最佳浸渍时间为60min，浸渍次数为2次。通过扫描电镜(SEM)表征了内部架构，最后指出莫来石纤维多孔陶瓷有望成为具有较好效果的新型催化剂载体。     

2-(5-溴-2-噻唑偶氮)-5-二乙氨基苯酚的合成与结构分析

用2-氨基噻唑为原料经溴化和重氮化,与N,N-二乙基间氨基苯酚偶联,合成了新有机分析试剂2-(5-溴-2-噻唑偶氮)-5-二乙氨基苯酚〔2-(5-Bromo-2-thiazolylazo)-5-diethylaminophenol,简称5-Br-TADAP〕.用薄层色谱法、元素分析法、质谱法、红外吸收光谱法、核磁共振谱法和可见吸收光谱法等分析手段对产品进行了分析和结构鉴定.该试剂至今未见文献报导.     

Diamond growth by carbon ion implantation of diamond

Medium energy (5–25 keV) ¹³C⁺ ion implantation into diamond (100) to a fluence ranging from 10¹⁶ cm⁻² to 10¹⁸ cm⁻² was performed for the study of diamond growth via the approach of ion beam implantation. The samples were characterized with Rutherford backscattering/channelling spectroscopy, Raman spectroscopy, X-ray photoemission spectroscopy and Auger electron spectroscopy. Extended defects are formed in the cascade collision volume during bombardment at high temperatures. Carbon incorporation indeed induces a volume growth but the diamond (100) samples receiving a fluence of 4 × 10¹⁷ to 2 × 10¹⁸ at. cm⁻² (with a dose rate of 5 × 10¹⁵ at. cm⁻² s⁻¹ at 5 to 25 keV and 800 °C) showed no He-ion channelling. Common to these samples is that the top surface layer of a few nanometers has a substantial amount of graphite which can be removed by chemical etching. The rest of the grown layer is polycrystalline diamond with a very high density of extended defects.