方酸钾与18-冠-6配合物的合成及表征

以甲醇为反应介质,18—冠—6及方酸阴离子与K~+离子可生成稳定的2:1:2配合物K_2(C_4O_4)(18—冠—6)_2·4H_2O,通过元素分析、ICAP、UV、~1HNMR、λ_M、DTA、TGA等对配合物的组成和结构进行了表征。     

金属-载体相互作用对CH4/CO2重整反应中Rh基催化剂抗积炭性能的影响

考察了Rh/Al2O3,Rh/SiO2和Rh/CeO2催化剂上金属-载体间相互作用对CH4/CO2重整反应抗积炭性能的影响,并与反应前后催化剂的程序升温还原和程序升温氧化(TPO)测试结果相关联.实验发现,Rh与Al2O3和SiO2载体间的相互作用越强,催化剂还原后Rh的分散度越高,晶粒越小,高分散的Rh表面生成的碳物种CHx越多,其作为活泼的反应中间体越易与CO2反应生成CO和H2.而游离态的Rh还原后晶粒较大,生成的碳物种与CO2反应能力较低,从而导致催化剂失活.TPO和CO2脉冲实验结果表明,反应过程中Rh/CeO2催化剂上反应生成的CHx物种比Rh/Al2O3和Rh/SiO2上的CHx物种更活泼.同时由于Rh-CeO2间独特的相互作用,部分CeO2还原后生成CeO2-x和氧空位,促进CO2分子的活化解离,导致生成的表面氧容易与CHx反应,从而抑制催化剂积炭.     

激光二级管抽运的Nd：GdVO4激光器

用高亮度激光二极管作抽运源,研究了连续、腔内倍频和被动调QNd:GdVO4激光器的输出特性.在抽运功率为881mW时获得了119mV的连续绿光输出,光-光转换效率13.5%.用Cr^4 :YAG作可饱和吸收体实现了Nd:GdVO4激光器的被动调Q运转,脉冲宽度为116-24ns.重复频率在500kHz-1.8MHz的范围内可调.     

硫化态Mo/γ-Al2O3催化剂活性位的低温CO-FTIR方法表征及噻吩HDS活性

ＭｏＳ2 是钼基加氢精制催化剂 [Ｃｏ(Ｎｉ)Ｍｏ/γ Ａｌ2 Ｏ3]活性相的主要组份 ,其形态与结构对Ｃｏ(Ｎｉ)Ｍｏ/γ Ａｌ2 Ｏ3的加氢脱硫 (ＨＤＳ)、加氢脱氮 (ＨＤＮ)活性的影响至关重要[1 ,2 ] .目前 ,人们通常使用的ＴＰＲ方法虽可测定过渡金属硫化物的表面活性位 ,并可有效地区分位于催化剂活性相 (ＭｏＳ2 ｓｌａｂ)周边的硫物种 ,但对不同价态的钼尚无法鉴别[3] .本文制备了硫化态Ｍｏ/γ Ａｌ2 Ｏ3催化剂 ,以ＣＯ为探针分子 ,利用ＦＴＩＲ技术在液氮温度 (77Ｋ)下考察了催化剂的表面活性位 (钼物种 )及催化噻吩ＨＤＳ的活性 .1　实…     

不同Ni前驱物对Ni催化剂甲烷部分氧化制合成气的影响

考察了由硝酸镍,醋酸镍和氯化镍为前驱物制备的催化剂（分别记为Ｎｉ－Ｎ,Ｎｉ－Ａｃ和Ｎｉ－Ｃｌ）对催化甲烷部分氧化反应的影响,并结合和ＴＧ等手段对催化剂进行了表征,结果表明,Ｎｉ－Ａｃ催化剂在６２５℃就能自引发甲烷部分氧化反应,而在Ｎｉ－Ｎ和Ｎｉ－Ｃｌ催化剂上,直到７５０℃甲烷部分氧化反应仍未能引发,三种催化剂上的反应结果表明,Ｎｉ－Ｎ和Ｎｉ－Ｃｌ的催化活性较低。９００℃下的高温反应结果表明,Ｎｉ－     

2,3-二苯基丙烯酸酯在DTBP/CaCl_2作用下的氧化偶联

多甲氧基菲-9-甲酸及酯是合成娃儿藤生物碱及其类似物的关键中间体。实验发现,以DTBP作为氧化剂,CaCl2存在下,能有效提高分子内氧化偶联合成多甲氧基菲-9-甲酸及酯产率,且反应条件温和,后处理方便,为合成许多重要化合物前体菲提供了一种新的思路。     

硫化态三组元NiMoP/γ-Al2O3催化剂的TPR表征及噻吩HDS活性的研究

A series of sulfided tertiary NiMoP/γ-Al2O3 catalysts with different contents of MoO3 were prepared by using molybdophosphoric acid of Keggin structure(H3PMo12O40) and nickel nitrate as origins of active phase components of molybdenum, phosphorus and nickel, and characterized by TPR technique, with their HDS activity being investigated with thiophene as a model substrate. For the sulfided Mo-0 catalyst containing no nickel as promoter, the only hydrogen sulfide evolution peak Ⅰ　is observed at 462 K and attributed to the hydrogenation of the so-called edge sulfur atoms chemisorbed on coordinatively unsaturated(cus) Mox+ sites on the MoS2 phase(MoS2 slab). With the introduction of nickel into the active phase of the sulfided Mo-0 catalyst and with the increase of the molybdenum loading, a new hydrogen sulfide evolution peak Ⅱ gradually develops at the low temperature side of the peak Ⅰ, at the same time accompanied by both the increase of the area ratio of the peak Ⅱ to the peak Ⅰ and the shift of the hydrogen sulfide evolution maximum rate to lower temperatures, which may imply the existence of two kinds of active centers related to molybdenum and nickel respectively and the synergic action between the two centers above. It should be noted that for the sulfided NiMoP/γ-Al2O3 catalysts, the thiophene HDS rate and the quantity of hydrogen sulfide evolved during TPR process increase monotonously with the atomic ratio of molybdenum to nickel in the form of ［n(Ni)+n(Mo)］/n(Ni). On the basis of the results here, the conclusion may be reached that the two kinds of vacancies can be formed on the edge of Ni-Mo-S slab due to the loss of S during TPR process and vacancies or sites related to the H2S evolution peak II should be regarded as the mainly active reaction centers of thiophene HDS.     

土壤中铅、砷、铬、铜和锌含量的连续快速测定

建立了土壤中铅、砷、铬、铜和锌含量的连续快速测定方法。土壤样品经微波消解,用同一份消解液,分别连续测定土壤中的铅、砷、铬、铜和锌含量,铬、铜和锌采用火焰原子吸收光谱法,铅和砷采用氢化物发生-原子荧光光谱法。采用本方法,对环境土壤标准样品ESS-1黑钙土(GSBZ50011)和ESS-3红壤(GSBZ50013)进行多次测定,检测结果与标样的推荐值吻合。经统计计算,回收率为95.2%—103.6%,精密度RSD均小于7%。本法操作简单快速,光谱测定结果已成功地用于无公害水果和蔬菜生产基地的土壤环境质量评价。     

ENDPOINT ESTIMATES FOR THE COMMUTATOR OF PSEUDO-DIFFERENTIAL OPERATORS

It is well known that the commutator Tb of the Calder′on-Zygmund singular integral operator is bounded on Lp(Rn) for 1 p +∞if and only if b∈BMO [1]. On the other hand, the commutator Tb is bounded from H1(Rn) into L1(Rn) only if the function b is a constant [2]. In this article, we will discuss the boundedness of commutator of certain pseudo-differential operators on Hardy spaces H1. Let Tσbe the operators that its symbol is S01,δwith 0≤δ 1, if b∈LMO∞, then, the commutator [b, Tσ] is bounded from H1(Rn) into L1(Rn) and from L∞(Rn) into BMO(Rn); If [b, Tσ] is bounded from H1(Rn) into L1(Rn) or L∞(Rn) into BMO(Rn), then, b∈LMO_(loc).     

基于FPGA和蓝牙的远程图像采集同步系统

针对核物理实验中高精度时间同步触发图像采集系统的要求,设计了一套基于FPGA和蓝牙的远程图像采集同步系统。该系统以FPGA作为主控制器,负责USB 接口通信、命令解析、蓝牙通信和同步控制等,触发信号延时精度可达10 ns;使用RS485 或TTL 标准以适应长距离触发和短距离触发,通过GigE 千兆网口实现远程图像数据采集。采用LabVIEW 开发了上位机图形化软件界面,基于蓝牙BLE4.0 协议,实现了基于手机APP的无线终端控制,完成了对相机延时时间、同步触发脉冲宽度、图像采集等命令的同步控制。A image acquisition and synchronization control system based on FPGA (Field Programmable Gate Array) and bluetooth is studied in this paper. FPGA as the main controller is responsible for USB (Universal Serial BUS) interface, command analyze, delay control, and trigger signal generation. Trigger signal can be RS485 or TTL. RS485 signals can be used for long-distance transmission without distortion while TTL is suitable for near field. The system's delay accuracy is reached to 10ns. It can be obtain images from GigE Ethernet port. Meanwhile,a PC graphical control software is developed by LabView. And based on the Bluetooth BLE4.0 protocol, a Android mobile phone APP is developed for wireless control.