高温燃煤钙基纳米金属氧化物复合吸附剂同时除砷脱硫研究

将纳米MgO、Al2O3和ZnO分别添加于超细CaCO3中制备出钙基纳米金属氧化物复合吸附剂,并进行燃煤过程中除砷脱硫的试验研究。结果表明,在Ca/S摩尔比为1.8,燃烧温度为1200℃,纳米金属氧化物的添加量为超细CaCO3质量的8%时,添加了纳米MgO的复合吸附剂除砷脱硫性能最好,比单一的超细CaCO3除砷率和脱硫率分别高出了28.73%和37.21%,表现出同时除砷脱硫的良好性能。     

超细碳化钨及其复合粉末的制备

超细碳化钨(WC)是近年发展起来的硬质合金材料，本文根据超细碳化钨粉末在还原碳化过程中是否连续，将其制备方法分成一步法和两步法进行综述。同时，归纳了超细WC-Co复合粉末的主要制备方法，其中喷雾干燥-流化床法具有操作过程连续、复合粉与反应气体接触充分、复合粉末的活性高、反应温度低和最终粉末的晶粒细小均匀等优点，可望作为制备超细碳化钨及其复合粉末的重要方法。     

湿化学法制备超细粉末过程中的团聚机理及消除方法

超细粉末由于具有独特的物理和化学特性,已经被广泛应用于各行各业之中。开发制备超细粉末的方法越来越多,其中湿化学法制备超细粉末具有显著的优点：原料成本低,设备、工艺简单,生产的粉末纯度高、粒度小,粉度分布范围窄,粒度组成可控性好。但是湿化学法制备粉末过...     

超细AgO粉末:制备及热分解非等温动力学

采用化学沉淀法,以臭氧为氧化剂制备了超细AgO粉末,并用XRD、XPS、SEM和粒度分析仪对制备的粉末进行了表征,借助热重分析法(TG)和线性升温理论对超细AgO粉末的热分解过程和非等温热分解动力学机理进行了研究。结果表明,制备的AgO属于单斜晶系,形貌为片状,其粒径分布在45～551nm之间,大部分在200nm左右;AgO的热分解分两步,158℃开始分解,放出氧气形成Ag2O,413℃进一步分解形成Ag;其热分解反应服从核生成和核成长为控制步骤的A2机理,热分解表观活化能为90.26kJ·mol-1,反应频率因子为1.64×108s-1。     

超细全硫化粉末丁腈橡胶对聚氯乙烯性能的影响

制备了PVC/超细全硫化粉末丁腈橡胶(NBR-UFPR)二元、PVC/NBR-UFPR/纳米CaCO3三元复合材料,研究了3种NBR-UFPR(平均粒径分别为150nm、90nm和70nm)对硬质PVC性能的影响.测试结果表明,3种NBR-UFPR均可同时提高硬质PVC的热稳定性、耐热性和韧性.透射电镜(TEM)照片显示,3种NBR-UFPR均能以单个粒子均匀分散在PVC基体中,NBR-UFPR与PVC相间的界面积大于传统的PVC/弹性体共混物.PVC/NBR-UFPR/纳米CaCO3三元复合材料具有更高的热稳定性、耐热性和韧性,TEM照片显示,在三元复合材料中,分散相粒子间的平均距离进一步减小.     

氨基酸-表面活性剂体系合成CaCO_3晶体

以L-组氨酸和十二烷基苯磺酸钠(SDBS)作为CaCO3生长调节剂,用粉末X射线衍射、红外光谱测试技术对生成的CaCO3晶体进行了表征,扫描电子显微镜对生成的CaCO3晶体形貌进行了分析,研究了表面活性剂浓度、温度和溶剂的组成对CaCO3晶型和形状的影响。结果表明,在实验条件下表面活性剂的浓度对CaCO3晶型没有影响,但影响晶体的形状,温度和溶剂的组成对CaCO3晶型和晶体形状有很大的影响。     

X射线荧光光谱法分析碳酸盐时两种制样方法的比较

在X射线荧光光谱法分析碳酸盐时,采用了两种样片的制法,即熔融法和超细粉末压片法,并对此两种方法进行了比较研究。结果表明:在所测定的15种组分中,采用超细粉末压片法所制样品的分析结果,其检出限有较大的改善,这是由于样品在制备过程中未被稀释;对测定的精密度而言,虽然在主、次组分方面不如熔融法好,但对于痕量组分,则超细粉末压片法占优。此外,在超细粉末压片制样过程中不存在二氧化碳的逃逸,而且粒度效应也基本消除,因此可定量测定碳酸盐中二氧化碳的含量。     

直接沉淀法制备ZnO超细粉末及其性质测定

用直接沉淀法制备ZnO超细粉末,利用激光散射测定其粒径,与其比表面积的大小作对比。利用红外光谱(IR)、X-射线衍射(XRD)、差热分析(DTA)对ZnO超细粉末进行分析。确定了最佳的制备工艺条件。     

纳米镍包覆超细铝复合粉末的氧化性能

通过置换还原法, 快速、简洁、定量地制备出了纳米镍包覆的超细铝粉复合粉末. 利用扫描电子显微镜(SEM)、热重分析(TGA)、差示扫描量热(DSC)和X射线衍射(XRD)等分析手段对原料Al粉和复合粉末的形貌及其氧化性能进行研究. 结果表明, 原料Al粉在1050 ℃时增重率为122%, 当包覆的纳米镍粉质量分数为0.75%时, 可以使铝粉在1050 ℃时的增重率达到135%, 并且随着镍粉含量的增加, 铝粉的增重率进一步提高. 当镍的质量分数达到8.93%时, 复合粉末在约1000 ℃时出现点火燃烧现象. 纳米镍粉的氧传递对促进超细铝粉的氧化起到了至关重要的作用.     

纳米碳酸钙的表面改性研究

纳米产品(材料)是当今世界高科技产品之一.纳米碳酸钙作为粉体产品中的一种,以高纯、超细、改性和功能性为标志,广泛应用于橡胶、塑料、造纸、油墨、涂料、医药、化妆品等各行各业[1-2].主要用作填充材料,因粒度超细、分散性好,可以增加填充量,降低制品成本,改善制品性能,提高制品档次,拓宽制品使用范围.近年来,随着CaCO3的超细化、结构复杂化及表面改性技术的发展,极大地提高了它的应用价值.对不同形态的超细CaCO3制备技术的研究,已成为许多先进国家竞相开发的热点[3-5].     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.