常压气固催化间甲苯胺N-乙基化研究

合成了复合金属氧化物催化剂 ,进行了以乙醇和间甲苯胺为原料 ,常压固定床反应工艺研究。考察了反应温度、进料空速、原料配比对反应结果的影响。优化条件下 ,间甲苯胺的转化率为 96 %以上 ,N 乙基间甲苯胺的选择性为 93%以上     

Multidimensional ARKN methods for general oscillatory second-order initial value problems

Based on B-series theory, the order conditions of the multidimensional ARKN methods are presented for the general multi-frequency and multidimensional oscillatory second-order initial value problems by Wu et al. (2009). These multidimensional ARKN methods exactly integrate the multi-frequency and multidimensional unperturbed oscillators. In this paper, we pay attention to the analysis of the concrete multidimensional ARKN methods for the general multi-frequency oscillatory second-order initial value problems whose right-hand side functions depend on both  y$y$and  y^′$y^{\prime }$ (the class of physical problems which fall within its scope is broader). Numerical experiments are carried out to show that the new multidimensional ARKN methods are more efficient compared with some well-known methods for dealing with the oscillatory problems in the scientific literature.     

High resolution solid state 13C n.m.r. of butadiene grafted polypropylene

¹H dipolar decoupled ¹³C n.m.r. experiments with the aid of the magic angle spinning technique have been used to determine the graft content and the isomer content of the polybutadiene grafts in a graft copolymer with isotactic polypropylene.     

108m3PVC聚合釜的研制

介绍了新开发的大型聚氯乙烯生产设备——108m3PVC聚合釜,通过对其技术特性、结构特点及生产能力等的介绍,阐明了该釜又是一个适应我国PVC行业发展需求的新釜型。     

Premodification of Pt/γAl2O3 with Cinchonidine for the Enantioselective Hydrogenation of Ethyl Pyruvate: Effect of Premodification Conditions on Reaction Rate and Enantioselection

The premodification of a 5 wt% Pt/-Al₂O₃ catalyst with cinchonidine (0.01 and 0.2 g g^-1 _catalyst) is described and discussed. Premodification is carried out by treating the catalyst with a solution of cinchonidine followed by solvent removal. Catalysts premodified in this way give the same ee and initial rate of reaction for the enantioselective hydrogenation of ethyl pyruvate as those using the standard in situ modification procedure. Investigations of different solvents for premodification and reaction (dichloromethane, ethanol) show that it is the solvent used for the reaction that controls the observed enantioselection. Premodified catalysts also display the initial transient behavior typically observed with in situ modified catalysts in which the ee increases with conversion in the early part of the reaction. Premodified catalysts show an enhanced rate of reaction when ethanol is used as the reaction solvent compared with in situ modified catalysts under the same conditions. Premodification using aerobic conditions gives the best results and premodified catalysts can be stored prior to use for up to a week without loss of catalytic performance.     

硝化法制备对氨基间硝基苯磺酸的研究

以对氨基苯磺酸为起始原料 ,经过乙酰化、硝化、水解三步来制备标题物。通过正交试验找出了酰化的最佳反应条件为 :对氨基苯磺酸与乙酐的摩尔比为 1∶1.0 5 ,反应总时间为 1.5h ,反应温度为 2 5℃ ,酰化介质为酰化反应前用碳酸钠及水将对氨基苯磺酸完全溶解 ,使混合液 pH值为 5～ 6 ,反应过程中不再补加碳酸钠 ,其酰化转化率可达 99.6 % ,酰化产物的固体收率可达 96 .0 % ;硝化反应的最佳条件为 :硝化剂用 90 .2 %的硝酸 ,对乙酰氨基苯磺酸与硝化剂的摩尔比为 1∶1.0 5 ,反应温度为 10℃ ,浓硫酸与对乙酰氨基苯磺酸的摩尔比为 8.3∶1,其硝化转化率可达 96 .0 % ,硝化反应的选择性好 ,对氨基邻硝基苯磺酸的量不到 1.0 %。     

Structure–Function Relations in Supported Ni–W Sulfide Hydrogenation Catalysts

Ni–W catalysts were prepared by impregnation of commercial -alumina and silica supports. The sulfidation, performed directly after drying at 100°C, yielded fully sulfided Ni–W species on both supports (SEM-EDAX, XPS, XRD). At optimal metals loading (50 wt% NiO + WO₃, Ni/W = 2), the sulfided catalysts had similar texture (N₂ adsorption) and displayed similar activity in dibenzothiophene hydrodesulfurization (DBT HDS), while the activity of the Ni–W/SiO₂ catalyst in toluene hydrogenation (HYD) was six times higher than that of Ni–W/Al₂O₃. This is due to the more than two times higher WS₂ slabs stacking number in Ni–W/SiO₂ compared with Ni–W/Al₂O₃ (XRD, HR-TEM), yielding stronger adsorption of toluene (TPD).     

Structural analysis of Aleksinac oil shale kerogen by high-resolution solid-state C n.m.r. spectroscopy

A sample of kerogen from Aleksinac oil shale was examined by high-resolution solid-state ¹³C n.m.r. spectroscopy. The presence and relative proportions of kerogen structural units were estimated using a combination of NQS and T_1C methods with a peak-synthesis technique applied to the ¹³C CP—MAS spectrum. Relaxation parameters from these experiments were used to estimate differences in relative ‘mobility’ of various structural units. The kerogen was found to be highly aliphatic and to contain 79% long-chain aliphatic plus alicyclic structures, as well as 9% aromatic structures. These findings are in good agreement with the characterization of the same kerogen from its oxidation products.     

溴素法α-溴代间氯苯丙酮合成研究

在金属卤化物催化剂 HD2 0 0 1存在下 ,溴与间氯苯丙酮在乙酸中反应得到盐酸安非他酮中间体 α-溴代间氯苯丙酮。最佳反应条件是 :n(间氯苯丙酮 )∶n(溴 ) =1∶ 1 ,催化剂用量为 1 %(质量分数 ) ,溴滴加时间为 1 h,反应温度为 1 0°C,此条件下 ,产物纯度为 98.83%,收率为 96.1 %。     

智能电网的安全可控性

计算机与信息技术在电力系统中的广泛应用提高了电网的自动化、智能化水平,同时也将传统IT领域的众多安全隐患引入了电网。智能电网是社会域、信息域、物理域多域交互、渗透形成的大规模新型融合网络,其安全威胁具有多域渗透、跨域攻击的特点。文中描述了智能电网基本安全需求及其与传统IT安全需求的不同;分析了智能电网中多域渗透攻击并且对信息-物理安全威胁进行分类;基于分域防护、多域协同、边界防护的思想提出了智能电网多域协同安全防护模型。