γ-苄基膦酸-磷酸锆的合成、表征及插层性能研究

于220℃水热晶化下制备了高结晶度的γ-ZrP,合成了3种γ-苄基膦酸-磷酸锆层状化合物Zr(PO4).(H2PO4)0.15(C6H5CH2PO3H)0.85·0.4H2O(1,d=1.86nm),Zr(PO4)(H2PO4)0.30(C6H5CH2PO3H)0.70·0.6H2O(2,d=1.78nm)和Zr(PO4)(H2PO4)0.50(C6H5CH2PO3H)0.50·0.7H2O(3,d=1.66nm).用X射线粉末衍射和31P固态核磁共振等手段表征其结构,并研究了其与α-苯乙胺的插层性能.     

混合型甘氨酸-N，N-双亚甲基膦酸-磷酸锆：合成、表征及插层

采用氢氟酸络合法,在nP/nZr=2.0条件下,以甘氨酸-N,N-双亚甲基膦酸(DMPG)和H3PO4为原料,按不同投料物质的量的比制备了2个α、γ-混合型甘氨酸-N,N-双亚甲基膦酸-磷酸锆层状主体化合物Zr(PO4)0.41(HPO4)0.043[(O3PCH2)2NCH2COOH]0.67.H2O(1)和Zr(PO4)0.21(HPO4)0.038[(O3PCH2)2NCH2COOH]0.82.2H2O(2),用元素分析、X射线衍射、红外光谱、热分析、固体核磁磷谱等对化合物进行了表征,同时研究了与正丁胺客体分子的插层组装性能。     

草酸/四丙基溴化铵体系中磷酸锆晶体的离子热合成与表征

采用离子热合成方法,在草酸/四丙基溴化铵离子型低共熔混合物中对磷酸锆骨架材料的合成进行了系统地研究,通过改变反应条件合成了2种不同的磷酸锆,α-Zr（HPO4）2？H2O和（NH4）Zr2（PO4）3.体系中的四丙基季铵阳离子对磷酸锆骨架没有体现出模板作用,后者是在较高的反应温度下（220℃）以四丙基季铵离子的热分解产...     

磷酸钙骨水泥水化机理研究进展

本文综述了Ca(H2PO4)2·H2O-Ca3(PO4)2-Ca4(PO4) 2O,Ca4(PO4)2O-CaHPO4,α-Ca3(PO4)2-少量β-TCP、HAP,β-Ca3(PO 4)2-CaHPO4·H2O-CaCO3及α-Ca3(PO4)2-Ca(H2PO4)2·H2O -CaCO3等几种主要磷酸钙骨水泥体系的特点和水化机理研究进展.     

新型磷-钒-氧层状化合物[H2en]2[H3O]6[Co(H2O)2(VO)8(OH)4(PO4)8]的水热合成与晶体结构

金属磷酸盐材料在吸附、离子交换、离子传导和催化剂方面有潜在的应用前景[1～5]. 近年来, 通过水热反应合成了一些A-V-P-O化合物. 在这些化合物中, A一般为碱金属或有机阳离子, 如层状结构的[H2N(C4H8)2NH2][(VO)4(OH)4(PO4)2][6] 和[H2N(C2H4)3NH2][(VO)8(HPO4)3(PO4)4*(OH)2]*2H2O[6], 一维链状结构的 [H2NCH2CH2NH3(VO)(PO4)][7], 手性双螺旋结构的 [(CH3)2NH2]K4[(VO)10(H2O)2(OH)4(PO4)7]*H2O[8]以及具有三维骨架结构的化合物 [H3N(CH2)3NH3K(VO)3(PO4)3][9], [H3N(CH2)3NH3]2[V(H2O)2(VO)6(OH)2(HPO4)3(PO4)5]*3H2O[10]和[H3N(CH2)2NH3][(VO)3(H2O)2(PO4)2(HPO4)4][11].     

新型杂多化合物[(CH3CH2)4N]4H3O· {Na[(HMo2O5)3(HPO4)(H2PO4)3]2}·(H2PO4)2·10H2O的水热合成与晶体结构

杂多化合物在催化、医药、材料及光化学等方面具有广泛的应用前景 [1～ 4 ] ,其中钼磷多金属氧酸盐具有优异的氧化催化性能 [5,6 ] .近年来合成的新奇结构的钼磷多金属氧酸盐中已测定结构的有含帽[7,8] 和非帽[9～ 12 ] 系列 .本文利用水热法合成了未见文献报道的结构新颖的夹心型磷钼多金属氧酸盐[( CH3CH2 ) 4N]4 H3O{Na[( HMo2 O5) 3( HPO4 ) ( H2 PO4 ) 3]2 }· ( H2 PO4 ) 2 · 1 0 H2 O,并测定了其晶体结构 .1　实验与晶体结构分析1 .1　仪器与试剂　元素 Na用美国原子吸收分光光度计测定 ;C,H和 N用 Perkin- Elmer 2 4 0…     

A Novel Borophosphate Coordination Polymer with Sandwich-type Supramolecular Architecture

A novel borophosphate (Hmel)3{Co2[(mel)2(HPO4)2(PO4)]·H3BO3·H2O} (mel= melamine) has been synthesized under mild solvothermal conditions. The structure of the compound exists a high ordered organic-inorganic sandwich-type supramolecular architecture via metal-coordination, hydrogen bonds and π-π stacking interactions.     

若干镧系络合物的空间群

摘要 藉助模拟强度精修将九个镧系络合物晶体结构的空间群作了修正 .（ 1） NaN[Nd(DMSO)5(H2O)3]Cl3· 3H2O从 P1修正为 P;（ 2） Er(ClO4)3· 6(CH3)2NC(O)N(CH3)2从 P修正为 R;（ 3） Nd(O3SCF3)3· DMF· 6H2O从 P1修正为 R3m;(4)[NaNCCH3][Nd{S2CN(CH2CH3)2}4]从 P修正为 C 2/c;(5)[(CH3)2NCS2]3La· 2DMSO从 Cc修正为 C 2/c;（ 6） Yb(C9H7)2· 2THF从 Cc修正为 C 2/c;（ 7） [(C6H5)3Ge]2Yb· 4THF从 P21修正为 P 2;(8)TlPr(C36H44N4)2从 Pna2,修正为 Pnma;(9)[CuLaSm(C4O4)4(H2O)16]· 2H2O从 P2修正为 P2.（ 8）、（ 9）两个络合物结构从非心修正到有心时,不仅改进了键长与键角值,而且影响到分子结构特征的描述 .     

不同阴/阳离子表面活性剂复配体系的缔合结构研究

测定了十二烷基磺酸钠(AS)/十六烷基三甲基溴化铵(CTAB)/正丁醇(n-C4H9OH)/正庚烷(n-C7H16)/水(H2O),十二烷基硫酸钠(SDS)/十六烷基三甲基溴化铵(CTAB)/正丁醇(n-C4H9OH)/正庚烷(n-C7H16)/水(H2O)体系的微乳液正四面体相图,并用电导法划分了AS/CTAB/n-C4H9OH/n-C7H16/H2O体系微乳液的结构(W/O,B.C.和O/W);同时研究AS/CTAB/n-C4H9OH/n-C7H16/H2O/盐类(NaCl,CaCl2或AlCl3)体系和SDS/CTAB/n-C4H9OH/n-C7H16/H2O/盐类(NaCl,CaCl2或AlCl3)体系形成中相微乳的盐宽,从中得出上述两体系中相微乳的盐宽随盐类阳离子价态的增大而的规律。     

二维层状磷钒多金属氧酸盐的水热合成及晶体结构

利用中温水热技术合成了新型的磷矾铁酸盐(NH3CH2CH2NH3)4[FeV8O12(HPO4)6(PO4)2(H2O)2]·5H2O,通过元素分析、IR光谱、热重分析和X射线衍射确定了晶体结构.该晶体属单斜晶系,P21/n空间群,晶胞参数:a=1.4304(3)nm,b=1.0145(2)nm,c=1.8356(4)nm,β=90.15(3)°,V=2.6637(9)nm3,Z=2,最终偏差因子R1=0.0631,wR2=0.1874.     

Cation mobility and kinetics of ion exchange in zirconium hydrogen monothiophosphate hydrate, Zr(HPO(3)S)(2)x1.5H(2)O

The ion conductivity of zirconium hydrogen monothiophosphate (Zr(HPO(3)S)(2)x1.5H(2)O) has been measured by impedance spectroscopy. The measured value of proton conductivity is 3 x 10(-5) S/cm at 298 K. Conductivity was shown to decrease with increasing temperature due to a dehydration process. Above 450 K, the conductivity is likely governed by proton transport in the anhydrous phase Zr(HPO(3)S)(2). The activation energies of proton conductivity were measured to be 18 +/- 2 kJ/mol for Zr(HPO(3)S)(2)x1.5H(2)O and 60 +/- 3 kJ/mol for the anhydrous compound. The kinetics of ion exchange was studied with the use of potentiometric titration for several ion pairs, H(+)/Na(+), H(+)/Zn(2+), and Na(+)/Zn(2+) in Zr(HPO(3)S)(2)x1.5H(2)O. The diffusion coefficient values for H(+)/Na(+) ion exchange in Zr(HPO(3)S)(2)x1.5H(2)O are lower than those reported in alpha-zirconium phosphate. At the same time, the mobility of zinc ions in Zr(HPO(3)S)(2)x1.5H(2)O is higher than sodium ion mobility. The ion exchange H(+)/Zn(2+) is accompanied by the slow hydrolysis of the initial compound. In all cases, the powdered solids were evaluated by powder X-ray diffraction, and particle sizes were controlled by grinding and sieving the powders.     

Effects of Structural and Textural Aspects on the Photocatalytic Performance of Zirconium Hydrogen Phosphate Doped with Tin Metal

Kinetics and Catalysis - The preparation of zirconium hydrogen phosphate, α-Zr(HPO4)2?·?H2O (α-ZrP), and its tin dopped derivatives were described. The structural and...     

十二烷基磺酸钠微乳状液结构转变的电化学研究

制备了C12H25SO3Na-C4H9OH-C7H16-H2O四组分体系在km=W(C4H9OH)/W(C12H25SO3Na)=2时的拟三元相图。使用二茂铁和铁氰化钾作为电化学探针用循环伏安法测定了起始含油量为21％的无水混合物在滴加水过程中所形成的微太液的扩散系数。从扩散系数随含水量的变化确定微乳液的结构转变。含水量为20％－45％时生成油包水型微液;含水量大于65％时生成水包油型微乳液。当含水量在45％－65％之间时形成的是二连续型微乳液。电导率数据证实了循环伏安法的测定结果。     

新型双链表面活性剂DDOBA的合成与高单分散性憎水纳米金的制备

自行设计合成了新颖的苄胺型双链表面活性剂3,4-双十二烷氧基苄胺(DDOBA). 利用DDOBA/正丁醇/正庚烷/甲酸/HAuCl₄·4H₂O自发形成的水/油(W/O)型微乳液作为微反应器, 通过微波辐射下的甲酸还原法成功制备了DDOBA保护的憎水性金纳米粒子, 并通过紫外-可见(UV-Vis)光谱、透射电镜(TEM)、高分辨透射电镜(HR-TEM)和X射线衍射(XRD)等方法进行了表征和分析. 结果显示, DDOBA既可参与形成稳定的W/O型(油包水型)微乳液, 又可作为金纳米粒子的良好保护剂. 在合适的微乳液体系组成范围内, 用本实验方法可以获得高单分散性的憎水性金纳米粒子, 并能在空气/水界面上自动形成大面积短程有序的纳米金二维自组装膜.     

Fluorescence Quenching of Anthracene by N,N-Diethylaniline and Phenothiazine in Triton X-100/n-C_(10)H_(21) OH/H_2O Microemulsion

IntroductionDuring the last decade,microemulsions haveplayed important roles in the development of bio-logical,material,environmental and other relatedfields[1— 4] .Although photo- induced electron trans-fer processes are of considerable interest in biologyand chemistry,up to now,most of the studies ofthe photo- induced electron transfer in micelle andinverse micelle have been limited to one- or two-component water/surfactant systems[5] .As theirextensions to microemulsion,only a very limited…     

Syntheses and X-ray crystal structures of zirconium(IV) and hafnium(IV) complexes containing monovacant wells-Dawson and Keggin polyoxotungstates

The syntheses and crystal structures of a series of zirconium(IV) and hafnium(IV) complexes with Dawson monovacant phosphotungstate [alpha2-P2W17O61](10-) and in situ-generated Keggin monovacant phosphotungstate [alpha-PW11O39](7-), which was obtained by a reaction of [alpha-PW12O40](3-) with Na2CO3, are described. K15H[Zr(alpha2-P2W17O61)2].25H2O (K-1), K16[Hf(alpha2-P2W17O61)2].19H2O (K-2), (Et2NH2)10[Zr(alpha-PW11O39)2].7H2O (Et2NH2-3), and (Et2NH2)10[Hf(alpha-PW11O39)2].2H2O (Et2NH2-4), being afforded by reactions in aqueous solutions of monolacunary Dawson and Keggin polyoxotungstates with ZrCl2O.8H2O and HfCl2O.8H2O followed by exchanging countercations, were obtained as analytically pure, homogeneous colorless crystals. Single-crystal X-ray structure analyses revealed that the Zr(IV) and Hf(IV) ions are in a square antiprismatic coordination environment with eight oxygen atoms, four of them being provided from each of the two monovacant polyanion ligands. Although the total molecular shapes and the 8-coordinate zirconium and hafnium centers of complexes 1-4 are identical, the bonding modes (bond lengths and bond angles) around the zirconium(IV) and hafnium(IV) centers were dependent on the monovacant structures of the polyanion ligands. Additionally, the characterization of complexes 1-4 was accomplished by elemental analysis, TG/DTA, FTIR, and solution (31P and 183W) NMR spectroscopy.     

十二烷基硫酸钠/苯甲醇/水微乳液中吩噻嗪对蒽的荧光猝灭

吩噻嗪与蒽之间可以发生光诱导单电子转移反应. 用荧光光谱仪研究了十二烷基硫酸钠(SDS) / 苯甲醇(BA) / 水微乳液中吩噻嗪对蒽的荧光猝灭.结果表明，在W/O微乳液中，蒽位于苯甲醇连续相，吩噻嗪位于膜相，猝灭反应发生于膜相；而在O/W微乳液中，蒽既可位于油核中，也可位于膜相，吩噻嗪位于膜相，猝灭反应亦发生于膜相.     

Spectroscopy characterization of anthracene in SDS/BA/H2O system

Spectroscopy characterization of anthracene in sodium dodecyl sulfate (SDS)/benzyl alcohol (BA)/water (H(2)O) microemulsion was studied by UV-visible absorption and fluorescence emission spectroscopy. The impact of the composition and structure of the microemulsion on spectroscopy characterization of anthracene were discussed. At the same time, we indicated the location of anthracene in microemulsion. The results indicated that in O/W microemulsion in SDS/BA/H(2)O system, anthracene exists both in the membrane phase and oil core, while in W/O microemulsion, anthracene exists in the oil continuous phase.     

手性膦酸锆的原位合成与表征

不对称催化和对映体拆分是有机化学中最活跃的高技术领域,其中手性固体材料的设计与合成是极具挑战性的前沿课题之一.据Corey等研究的手性技术机理,手性固体一般应该具有空间允许、手性源为官能化的有机化合物和金属离子作为反应的活性中心等三大特征．然而,迄今同时具有上述特征的手性固体材料却很少．