新型磷酸铝分子筛AlPO_4-CJ_2的合成与结构研究

在Al_2O_3-P_2O_5-六次甲基四胺-H_2O体系中,水热合成出新型磷酸铝分子筛(AlPO_4-CJ_2),培养了单晶,经多晶X射线衍射、四圆单晶结构测定及红外光谱研究证明,AlPO_4-CJ_2具有空旷的骨架结构,沿(100)和(001)方向具有8元环孔道,骨架中Al原子以AlO_5(三角双锥)和AlO_5F(扭曲八面体)形式存在,水分子氧的桥联产生Al—O—Al连接模式。     

乙二胺基乙磺酸钠的合成与表征

乙二胺基乙磺酸钠是水性聚氨酯合成中重要的亲水性扩链剂, 又可作为有机中间体、生化试剂应用于其它领域.采用乙二胺(EDA)和2-氯乙磺酸钠反应合成乙二胺基乙磺酸钠, 由红外光谱(FTIR)、核磁氢谱(1H NMR)和碳谱(13C NMR)、X射线衍射(XRD)、元素分析等手段表征了产物的结构与特性. 在EDA与2-氯乙磺酸钠物质的量比为6.5∶1时, 合成产物中乙二胺基乙磺酸钠含量高达94.4%. 产物极易溶于水, 微溶于甲醇, 乙醇, 不溶于丙酮, N,N-二甲基甲酰胺, 四氯化碳, 氯仿等有机溶剂.     

无机微孔晶体AlPO4-CJ1合成与性能研究Ⅰ.

自从八十年代美国UCC首次合成出非硅铝酸盐的AlPO₄-n系列分子筛以来^[1],由于其特殊的骨架结构和物化性质,引起人们的广泛重视^[2].我们用乙二胺基乙醇作模板剂合成出AlPO₄-CJ₁.经多晶X射线衍射,红外光谱及扫描电镜等结构表征,证明其为纯的,新型无机微孔晶体,吸附实验证明其具有4Å的孔道.     

磷酸硅锌铝分子筛（ZnAPSO—5）的合成,结构及性能研究

以二乙氨基乙醇为导向剂,用水热晶化法合成了磷酸硅锌铝分子筛纯相,测定其组成为Zn_(1.12)Si_0.38Al_(10.88)P_(11.62)O_(48),并对其结构和性能进行了研究.实验结果表明,ZnAPSO-5具有AlPO_4-5型分子筛结构,由于锌和硅进入骨架同晶取代了部分铝和磷,致使ZnAPSO-5分子筛有了B酸酸性,而热稳定性也较磷酸锌铝分子筛(ZAPO-5)有所提高.     

离子热法制备多级孔AlPO_4-5分子筛

采用离子热法,以磷酸为磷源,γ-Al_2O_3为铝源,在1-丁基-3-甲基溴化咪唑离子液体中于320℃反应10 min内快速合成了多级孔AlPO_4-5分子筛,其结构和形貌经傅里叶红外光谱(FT-IR),X-射线衍射(XRD),扫描电子显微镜(SEM),氮气物理吸-脱附(BET)和透射电镜(TEM)表征。     

新型三维开放骨架磷酸铝化合物的合成及晶化过程中的共模板效应

以1,2-丙二胺(1,2-DAP)为结构导向剂,在180℃加热摩尔组成为n(Al_2O_3)∶n(P_2O_5)∶n(1,2-DAP)∶n(H_2O)=1∶6∶5.5∶139的初始混合物,合成了具有AlPO-CJ31骨架结构的新型三维开放骨架磷酸铝化合物(1);加热摩尔组成为n(Al_2O_3)∶n(P_2O_5)∶n(1,2-DAP)∶n(H_2O)=1∶6∶7.5∶139的初始混合物,合成了二维层状磷酸铝化合物APDAP_(12)-150.利用X射线粉末衍射分析(XRD)、元素分析、热重/差热分析等表征手段确认了化合物1的分子式为[Al_4P_5O_(20)·H_3O·H_2O]·[H_3NCH_2CHNH_3CH_3],质子化的水分子与双质子化的1,2-丙二胺共同起到了导向化合物1的作用.调变初始混合物中1,2-丙二胺的比例可显著影响其模板效应.1,2-丙二胺比例较低[n(1,2-DAP)=5.5]时,产物为三维开放骨架化合物,而当其比例较高[n(1,2-DAP)=7.5]时,产物为二维层状化合物.     

一氧化碳加氢Fe_2O_3/AlPO_4-5催化剂的表面分散状态及性质

1.前言 采用具有ZSM-5,ZSM-11和ZSM-48沸石结构的高硅沸石作为CO加氢反应的催化剂载体,有效地控制了产物分布范围。AlPO_4-5分子筛的孔道结构和表面性质决定了它同样可作为催化剂载体以代替沸石。关于AlPO_4-n分子筛的研究,目前多着重于合成和结构方面,以其作为催化剂和催化剂载体的报道较少。由于AlPO_4-n分子筛无离子交换性,致使负载金属AlPO_4-n催化剂的制备受到限制。根据“某些盐类或氧化物与高比表面载体混合,在低于熔点的适当温度下焙烧,这些盐类或氧化物在载体表面能自发分散”的原理,本文采用固相焙烧法制备了系列Fe_2O_3/AlPO_4-5催化剂并用于CO加氢反应,研究铁活性组分在AlPO_4-5分子筛表面的分散状况及催化活性。     

4-甲基-4-氮杂-21E-苯亚甲基-5-孕烯-3,20-二酮类化合物的合成

报道了一种以KF/Al_2O_3催化合成4-甲基-4-氮杂-21E-苯亚甲基-5-孕烯-3,20-二酮类化合物的方法。以黄体酮为原料,经NaIO_4/KMnO_4氧化裂解、胺解关环得到重要中间体4-甲基-4-氮杂-5-孕烯-3,20-二酮,后者在KF/Al_2O_3催化下经克莱森缩合得到目标产物。考察了不同的催化剂、反应温度、催化剂用量对目标产物的影响。条件优化的结果为:n(3)∶n(KF/Al_2O_3)=1∶1,回流状态下反应4 h,产率为56%~68%。此方法适用性好,为4-氮杂甾体苯亚甲基衍生物的合成提供了一种方便而有效的方法。     

C(2)-酰胺基-4-芳基-1,5-苯并硫氮杂的合成及抑菌活性的研究

设计合成了三类C(2)酰胺基取代的1,5-苯并硫氮杂衍生物:2-酰胺基(N-芳基)-4-芳基-1,5-苯并硫氮杂、2-酰胺基(N-烷基)-4-芳基-1,5-苯并硫氮杂和2-酰胺基(N,N-二烷基)-4-芳基-1,5-苯并硫氮杂,其结构用元素分析,IR,MS及1H NMR确证.测定了目标化合物的抑真菌活性,结果表明部分化合物对新生隐球菌具有中等强度的抑真菌活性.还研究了2-酰胺基-4-芳基-1,5-苯并硫氮杂的合成反应条件.     

磷酸铝基分子筛研究进展

美国联合碳化物公司Flanigen研究中心1982年首次公布无硅骨架氧化物——AlPO_4系列分子筛。在已合成出的二十种磷酸铝晶体中有六种二维结构和与沸石相同骨架结构的AlPO_4—17(毛沸石)及AlPO_4-20(方钠石)、新型结构AlPO_4-5、-11、-14、-16、-18、-31等十四种三维结构。它们内径孔体积从0.04—0.35cm~3/克,孔径从0.3—0.8?。AlPO_4系列     

助催化剂对Fe1-xO基氨合成催化剂还原性能的影响

当助催化剂存在是地，Ｆｅ１－ｘＯ基催化剂的还原性能明显优于Ｆｅ３Ｏ４基催化剂，其原因是铝、钾、钙的氧化物对催化剂母体相Ｆｅ１－ｘＯ和Ｆｅ３Ｏ４还原性能的影响不同。由于Ａｌ＾３＋大量地进入Ｆｅ３Ｏ４的晶格而强烈地阻止Ｆｅ３Ｏ４的还原，只有少量的Ａｌ＾３＋能进入Ｆｅ１－ｘＯ晶格，因此对Ｆｅ１－ｘＯ的还原影响很小；     

Chemical bonding in the crystal structure of 1-hydrosilatrane

A study has been made of the crystal and molecular structure of 1-hydrosilatrane HSi(OCH_2CH₂)₃N. The quantum chemical calculations of its crystal structure have been carried out. According to an estimate of the energy, the coordination bond N→Si is by 5 kcal mol^?1 stronger than that in the crystal of 1-methylsilatrane. The charge values calculated within the framework of the topological analysis of the electron density demonstrate that the electron density of the coordination bond N→Si is primarily transferred to the region of the equatorial bonds Si—O and, to a lesser extent, to the bond Si—H. On going from the isolated molecule of 1-hydrosilatrane to its crystal, the interatomic distance N—Si decreases, mainly owing to the weak intermolecular interaction C—H...O.     

Synthesis and Crystal Structure of 1，5－Bis（1＇－phenyl－3＇－methyl－5＇－pyrazolone－4＇）－1－（4＇－aminobutand－1＇－imino）－5－pentaneone

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ１，５－Ｂｉｓ（１＇－ｐｈｅｎｙｌ－３＇－ｍｅｔｈｙｌ－５＇－ｐｙｒａｚｏｌｏｎｅ－４＇）－１－（４＇－ａｍｉｎｏｂｕｔａｎｄ－１＇－ｉｍｉｎｏ）－５－ｐｅｎｔａｎｅｏｎｅ￥ＹａｎｇＬｕ－Ｑ...     

3,3-二甲基-9-(5,5-二甲基-3-羟基-2-环己烯-1-酮-2-基)-1-氧代-2,3,4,9-四氢化氧杂蒽的合成和晶体结构

标题化合物C23H26O4是由水杨醛与5，5-二甲基-1，3-环己二酮在N，N-二甲基甲酰胺中反应而得．结构通过单晶X-射线行射法确定，其晶体属于单料晶系，空间群P21/c，a=7．056（7），b=20.263（3），c=13．665（2）A，β＝93．32（1）°，V=1950．7（4）A3，Mr=366．46，Dc=1.248g／cm3，Z=4，μ（MoKa）=0．84cm－1，F（000）=784。晶体结构用直接法解出，经全矩阵最小二乘法对原子参数进行修正，最后的偏离因子R=0．068，Rw=0．075。晶体结构分析结果表明，分子中存在一个共轭的烯醇式结构。     

1-benzoyl-2-(2-naphthyl)-selenourea

During our synthesis of N-benzoyl-N'-aryl selenourea derivatives, we isolated the title compound. One of them was selected optically for the diffraction study. The crystal belongs to the Monoclinic space group P21/n, Mr = 353.27, a = 11.073(1)A, b = 5.745(1) A, c = 24.356(5) A, β= 92.10 (1) °, V= 1548.3 (4) A3, Z = 4, Dx=1.515 Mg/m3, λ (Mo Kα )=0.71073 A, θ = 1.67-25, μ= 2.428 mm-1 , T = 296 (2) K.View of the molecule showing the labeling of the non-H atoms are described as:The selenourea and thiourea have analogous structure, a few literatures have reported the crystal of N-benzoyl-N'-aryl thiourea derivative1,2. In the reported crystal structure of N-benzoyl-N'-aryl thiourea derivative, there is a intermolecular hydrogen bond between the carbonyl O and H atom on N', in each -C(O)-NH-N'H- moiety, forming a planar six-membered ring. In this title compound,[2.654(2)A], C (8), N (1) and C (7)l.In the crystal structure of N-benzoy-N'-aryl thiourea derivative, there have a two dimensional With the intramolecular hydrogen bond [2.654(2)A] they form the planar four-membered ring between every molecular. The atom of Se dose not link the moleculars like the S atom of N-benzoyl-N'-aryl thiourea derivative, and it is only out of six-membered ring, which forms by N (2)H…O, C (8), N (1) and C (7).     

3-羟基-1-金刚烷甲酸钴邻菲略啉配合物的合成和晶体结构

以硫酸钻、邻菲咯啉（phen）和3-羟基-1-金刚烷甲酸（HOC10H14COOH）为原料,合成了配合物[Co（HOG10H14COO）2（H2O）（phen）]·H2O;利用元素分析、红外光谱、热重分析对产物进行了表征,采用单晶X射线衍射方法测定了其晶体结构．结果表明,所合成的配合物C34H42N2O8Co属于单斜晶系,空间群C2／c,a=2．69798（7）nm,b=1．14319（3）nm,c=2．29092（6）nm,β=120．498（1）°,V665．63,F（000）=2808,Dc=1．452g·cm^-3,μ（Mo-Kα）=0．765mm^-1;R1=0.0805,wR2=0.2209,其通过氢键和π-π堆积作用相结合,形成稳定的二维超分子结构．     

Synthesis and Crystal Structure of 1-（Trifluoromethyl）-1-（propioloyl）-（E）-3-oxo-（2-thienyl）-（2-naphthylamine）

1INTRODUCTIONTheSchiffbasesderivedfromb-diketonesandaliphaticamineshavebeenshowntoexistastheketo-amines.However,ifsubstituentseitherattheketooraminogrouparearomatic,itmaybeexpectedtheenoliminewillbethefavoredtautomericform[1].Recently,someSchiffbasesderivedfromTTA(4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione)andPMBPhavebeenstudiedbyWang[2]andYu[3]etal.Inordertostudytherelationshipbetweenthestructuresandperformancesofthesecompounds,thetitlecom-poundwillbereportedherein.2EXPERIMENT…     

Synthesis and Crystal Structure of 3-(Pyrrole-2''-carboxamido)propanoic Acid·(1/2)H2O

3-(Pyrrole-2'-carboxamido)propanoic acid I has been synthesized from the reaction of β-alanine methyl ester with 2-trichloroacetylpyrrole followed by saponifying and acidating in 85.4% yield, and the crystal structure of 3-(pyrrole-2'-carboxamido)propanoic acid· (1/2)H2O (C8H11N2O3.5, Mr = 191.19) was obtained and determined by X-ray diffraction method. The crystal is of monoclinic, space group C2/c with a = 19.010(4), b = 8.3515(17), c = 13.788(3) (A), β = 125.88(3)°, V = 1773.6(6) (A)3, Z = 8, Dc = 1.432 g/cm3, λ = 0.71073 (A), μ-MoKα) = 0.114 mm-1 and F(000) = 768. The structure was refined to R = 0.0354 and wR = 0.0942 for 1642 observed reflections with I > 2σ(I). It is revealed that the title compound has one pyrrole ring and one propionic acid subchain linked by an amido bond at C(4), and there are 8 molecules of com- pound I and 4 crystal water molecules in each unit cell. The supramolecular layers are stabilized by the hydrogen bonds of N(2) H…O(2), N(1) H…O(4), O(4) H(1W)…O(2) and O(3) H…O(1).     

Beta-alanine-hydrochloride (2:1) crystal: structure, 13C NMR and vibrational properties,protonation character

The crystal structure of beta-alanine-hydrochloride (2:1) complex (2A-HCl) has been determined by X-ray diffraction method at 298 and 100 K as monoclinic, space group C2/c, Z=4. The crystal comprises chloride anions and protonated beta-alanine dimers: two beta-alanine zwitterions are joined by strong, symmetric (Ci) hydrogen bond with the O...O distance of 2.473 A at room temperature. Powder FT-IR and FT-Raman as well as solid state 13C NMR spectra provide insights into the solid structure of this complex, character of its hydrogen bonds and the beta-alanine protonation.