螺旋状配位结构的碱土金属开链冠醚三元配合物

合成并表征了4种碱土金属苦味酸盐与N,N,N´,N´-四苯基-3,6,9-三氧杂十一烷二酰胺(TTD)的固态配合物M (Pic)₂TTD (1. M = Mg, 2. M = Ca, 3. M = Sr, 4. M = Ba). 配合物3的结构分析表明, Sr (Ⅱ)与TTD及两个二齿Pic^-配位, 配位数为9, 配位多面体为变形三帽三角棱柱; TTD作为五齿配体, 其螯合链形成右手螺旋状配位结构, 这种螯合螺旋链具有较为固定的螺旋半径, 对金属离子有较高的配位选择性. 在结构上初步解释了TDD对碱土金属离子具有高选择性的原因.     

Synthesis and Structural Characterization of 1,4-Di（2-methoxyphenyl）-2,5-piperazinedione

A new derivative of 2,5-piperazinedione, 1,4-di（2-methoxyphenyl）-2,5-piperazinedione （I）, was synthesized by the cyclocondensation reaction of N-2-methoxyphenyl chloroacetamide, and its structure was characterized by elemental analysis, IR, ^1H NMR and single crystal X-ray diffraction method. The crystal belongs to monoclinic system, space group P21/c with unit cell dimensions a=0.56934（10） nm, b=1.3880（2） nm, c=1.00329（17） nm, β= 90.376（3）°, V= 0.7928（2） nm^3, Z=2, Dc = 1.367 g·cm^-3,μ = 0.98 cm^-1, R and wR being 0.0606 and 0.1564 respectively for 1549 unique reflections with 1247 observed reflections [I〉2σ（I）]. The molecule has a crystallographically imposed symmetry center. The three rings in the molecule are each coplanar with their attached groups, excluding methyl H atoms and the H atoms attached to the piperazinedione ring, while the whole molecule is not planar, with dihedral angles of 74.7（1）° between the piperazinedione and each of the two aromatic rings. The crystal structure is stabilized by van der Waals and dipole-dipole forces.     

π络合脱硫吸附剂Cu(Ⅰ)-Y的生物再生

吸附与生物技术的耦合是实现燃料油品清洁生产的新发展方向, 提出了一种吸附剂生物再生循环使用的新耦合方法, 首先用吸附剂吸附脱除油品中的含硫化合物, 然后用微生物脱附吸附剂表面吸附的硫化物, 实现吸附剂再生. 利用Y型分子筛通过离子交换再用He保护自动还原的方法制备了(络合吸附剂吸附Cu(Ⅰ)-Y, 以DBT为模型化合物考察了吸附剂的吸附性能. 以选择性脱硫菌德氏假单胞菌(Pseudomonas delafieldii)R-8为生物催化剂, 考察了细胞浓度、油相体积、水相/吸附剂比对吸附剂脱附率的影响. 加入油相可以大大提高DBT脱附量和生成2-HBP的量. 增加水相中脱硫菌R-8的浓度、增大水相/吸附剂比, 可以实现DBT脱附, 促进DBT转化为2-HBP. 在水相脱硫菌株R-8浓度为75 g·L-1、水相/吸附剂比为300 mL/g、油相/水相比1/3(V/V)的条件下, 脱附的DBT在6 h内转化率达到89%, 24 h内转化率为100%. 生成2-HBP的量主要由吸附剂吸附硫化物的量、水相中微生物细胞的浓度、油相/水相体积比、水相/吸附剂比决定. 吸附剂经过正辛烷洗涤、100℃下干燥24 h、He保护450℃还原活化3 h, 再生吸附剂的吸附能力为新鲜吸附剂的95%.     

一维链状冠醚配合物:[{Na(18-C-6)}2(H2O)]n[M(SCN)4]n(M=Pd、Pt)的合成与结构

The reactions of 18-crown-6 with Na₂[M(SCN)₄] (M= Pd,Pt) were studied and the complex 1 [{Na(18-C-6)}₂(H₂O)]_n[Pd(SCN)₄]_n and complex 2 [{Na(18-C-6)}₂(H₂O)]_n[Pt(SCN)₄]_n were characterized by ele-mental analysis, IR and X-ray diffraction analysis. The complexes belong to monoclinic, space group P2₁/n with cell dimensions, 1:a=1.05734(7),b=1.42250(10),c=1.47762(10) nm,β=107.5330(10)°,V=2.1192(2)nm³,Z=2,D_calcd=1.460g·cm^-3,F(000)=964,R₁=0.0406,wR₂=0.1264 and 2:a=1.05985(19),b=1.4237(3),c=1.4744(3) nm,β=107. 096(3)°, V=2.1264(7)nm³,Z=2,D_calcd=1.690g·cm^-3,F(000)=1028,R₁=0.0292,wR₂=0.0859. In the solid state, the complexes 1 and 2 show an one-dimensional chain of [{Na(18-C-6)}₂(H₂O)]²⁺ complex cations and [M(SCN)₄]^2- (M=Pd,Pt) complex anions bridged by Na-N in-teractions.     

均匀沉淀法制备Co(OH)2及其超电容特性

以氯化钴为原料、氨水(28wt%)为沉淀剂采用均匀沉淀法成功地合成了Co(OH)₂。X-射线衍射(XRD)、扫描电镜(SEM)测试表明，表面活性剂Tween-80的加入使所制备的α-Co(OH)₂呈现出类似花朵的形貌;循环伏安、恒电流充放电、交流阻抗和循环寿命等电化学测试表明，该材料的电化学性能也得到一定的提高，其单电极比电容可达到370 F·g^-1。     

长链脂肪酸LB膜的X射线衍射研究

利用Langmuir-Blodgett技术制备了硬脂酸、花生酸及其混合酸的多层LB膜。用低角X射线衍射研究了它们的周期结构,硬脂酸和花生酸的LB膜在2θ=0.8°～23°的范围内分别出现13个和12个布拉格衍射峰,由此计算了它们的等同周期。用模型计算了它们衍射峰的强度,得到了与实验一致的衍射强度奇偶起伏的结果。在混合酸的LB膜中,可以观察到等同周期随混合比变化的规律。     

One Novel Vanadium-Phosphate Cluster [PV_(2.5)O_(8.5)]-3.83{H_2O} with Three-Dimensional Architecture

A novel vanadium-phosphate compound [PV_2.5O_8.5]·3.83{H_2O}(1)was obtained from the hydrothermal reac-tion and structurally characterized by elemental analysis and single-crystal X-ray diffraction,which exhibited thatthe title complex crystallized in cubic space group I-43m with crystal data:a=1.6115(1)nm,V=4.1848(1)nm~3,Z=12,D_c=1.783 g/cm~3,F(000)=2278,R_1=0.0528,and wR_2=0.1329[I>2σ(I)](all data).The basic unit of{PV_2.5O_8.5}symmetrically extended to closed sphere-like structure of{P_4V_(10)O_(34)},which was further linked to in-terleaving three-dimensional network via sharing four phosphate through μ_3-oxygen atoms around the closedsphere-like structures.     

选区激光熔化FeCoNiCr系高熵合金微观组织的实验研究

介绍了关于选区激光熔化的热分析理论,利用选区激光熔化技术制备FeCoNiCrAl_0.5和FeCoNiCrAl_0.8高熵合金试件.利用超景深显微镜对试件微观组织进行观测,分析了粉末粒径、元素含量,以及工艺参数等因素对选区激光熔化高熵合金的微观组织的影响.结果表明,随着激光功率增大,试件顶部等轴晶的占比越来越少,尺寸越来越细小,试件底部组织中枝晶的占比逐渐增多,尺寸不断增大;随着扫描速度增大,高熵合金试件底部组织中枝晶尺寸逐渐减小、宽度变窄;搭接率对高熵合金试件微观组织影响较小;制得的高熵合金试件存在着裂纹、凹陷及气孔等缺陷.     

北江洪水预报模型

将北江流域按区域下垫面特征进行分区,建立起各单元区产汇流模型,并与北江干流非恒定流水力学演算模型耦合,形成适合北北流域洪水特点的实时洪水预报模型,用北江“９４．６”洪水验证的结果表明,模型预报精度较高,最后,还指出了模型存在的问题和进一步研究的方向。     

受迫二维广义KdV方程的反周期行波解的变分方法

用变分法研究了受迫二维广义ＫｄＶ方程的反周期行波解的存在性。