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A Three-dimensional Porous Metal-organic Framework Based on Cyano Unit and 1,4-Bis(1,2,4-triazol-1-yl)butane(btb):{[Cu_8(btb)_2(CN)_8].3H_2O}_n 被引量:3
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作者 周馨慧 李洪辉 黄维 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2012年第1期33-38,共6页
The title coordination polymer 1,{[Cu8(btb)2(CN)8].3H2O}n(btb = 1,4-bis(1,2,4-triazol-1-yl)butane),has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex... The title coordination polymer 1,{[Cu8(btb)2(CN)8].3H2O}n(btb = 1,4-bis(1,2,4-triazol-1-yl)butane),has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in monoclinic,space group C2/c with a = 1.2938(3),b = 1.9422(5),c = 0.9406(2) nm,β = 121.891(4)°,V = 2.0066(9) nm3,C24H30Cu8N20O3,Mr = 1155.00,Dc = 1.912 g/cm3,μ(MoKα) = 4.209 mm?1,F(000) = 1140,GOF = 1.184,Z = 2,the final R = 0.0634 and wR = 0.1503 for I 2σ(I).In complex 1,one-dimensional CuCN zigzag chains are linked by triazolyl groups of btb ligands to form two-dimensional networks,which are further bridged by 1,4-butyl moieties of btb ligands to fabricate a three-dimensional order framework,in which one-dimensional ellipsoid-like channels are observed. 展开更多
关键词 CYANO 1 4-bis(1 2 4-triazol-1-yl)butane metal-organic framework(MOF) complex Cu+
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Synthesis,Crystal Structure and Theoretical Calculations of a Cadmium Complex Containing 3-Hydroxybenzoic Acid and 1,4-Bis(imidazol-1-yl)-butane 被引量:2
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作者 王志涛 王少杰 +1 位作者 李秀梅 潘亚茹 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2018年第3期467-474,共8页
A new complex [Cd(hba)2(bib)]n·nH2O(1,Hhba = 3-hydroxybenzoic acid,bib = 1,4-bis(imidazol-1-yl)-butane) has been hydrothermally synthesized and characterized by elemental analysis,IR spectrum,thermogravim... A new complex [Cd(hba)2(bib)]n·nH2O(1,Hhba = 3-hydroxybenzoic acid,bib = 1,4-bis(imidazol-1-yl)-butane) has been hydrothermally synthesized and characterized by elemental analysis,IR spectrum,thermogravimetric analysis,fluorescence spectrum,and singlecrystal X-ray diffraction.Yellow crystal crystallizes in the orthorhombic system,space group Pbca with a = 16.220(5),b = 14.980(5),c = 20.521(5) ?,V = 4986(3) ?~3,C(24)H(26)CdN4O7,Mr = 594.89,Dc = 1.585 g/cm^3,μ(Mo Kα) = 0.927 mm^(-1),F(000) = 2416,Z = 8,the final R = 0.0242 and w R = 0.0589 for 4076 observed reflections(I 〉 2s(I)).In 1,the Cd(Ⅱ) ion takes a six-coordination mode,and bib ligand bridges adjacent Cd(Ⅱ) ions to generate 1D zigzag chains; these neighboring chains are connected by O–H···O hydrogen bonding interactions,producing a 2D folded layered structure.Furthermore,by O–H···O hydrogen bonding between layers and layers,a 3D supramolecular architecture is formed.In addition,we analyzed Natural Bond Orbital(NBO) in using the PBE0/LANL2 DZ method built in Gaussian 03 Program.The calculation results indicated obvious covalent interaction between the coordinated atoms and Cd(Ⅱ) ion. 展开更多
关键词 crystal structure Cd(Ⅱ) complex 3-hydroxybenzoic acid 1 4-bis(imidazol-1-yl)-butane natural bond orbital
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Synthesis and spectral studies of macrocyclic Pb(Ⅱ),Zn(Ⅱ),Cd(Ⅱ)and La(Ⅲ) complexes derived from 1,4-bis(3-aminopropoxy)butane with metal nitrate and salicylaldehyde derivatives
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作者 Salih Ilhan Hamdi Temel Salih Pasa 《Chinese Chemical Letters》 SCIE CAS CSCD 2009年第3期339-343,共5页
Eight new macrocyclic complexes were synthesized by template reaction of 1,4-bis(3-aminopropoxy)butane with metal nitrate and 1,3-bis(2-formylphenyl)propane or 1,4-bis(2-formylphenyl)butane and their structures ... Eight new macrocyclic complexes were synthesized by template reaction of 1,4-bis(3-aminopropoxy)butane with metal nitrate and 1,3-bis(2-formylphenyl)propane or 1,4-bis(2-formylphenyl)butane and their structures were proposed on the basis of elemental analysis, FTIR, UV-vis, molar conductivity measurements, ^1H NMR and mass spectra. The metals to ligand molar ratios of the complexes were found to be 1: 1. The complexes are 1:2 electrolytes for Pb(II), Zn(II) and Cd(II) complexes and 1:3 electrolytes for La(III) as shown by their molar conductivities (Am) in DMSO at 10^-3 mol L^-1. Due to the existence of free ions in these complexes, such complexes are electrically conductive. The configurations of La(III) and Pb(II) were proposed to probably octahedral and Zn(II) and Cd(II) complexes were proposed to probably tetrahedral. 展开更多
关键词 Macrocyclic Schiff base Macrocyclic complexes Salicylaldehyde derivatives 1 4-bis(3-aminopropoxy)butane
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Syntheses, Structures and Characteristics of Two New Cu(II) Coordination Polymers Based on 4-tert-butyl-phthalate and Different Bis(1,2,4-triazol-1-yl) Co-Ligands 被引量:3
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作者 韩民乐 凌勋利 +2 位作者 常新红 刘广臻 杜德光 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2015年第4期543-550,共8页
Two new Cu(Ⅱ) coordination polymers, [Cu2(tbph)2(btb)2]n (1) and {[Cu2(tbph)2- (bth)2]·H2O}n (2), (H2tbph = 4-tert-butyl-phthalic acid, btb = 1,4-bis(1,2,4-triazol-1- yl)butane, bth = 1,6-bis(1... Two new Cu(Ⅱ) coordination polymers, [Cu2(tbph)2(btb)2]n (1) and {[Cu2(tbph)2- (bth)2]·H2O}n (2), (H2tbph = 4-tert-butyl-phthalic acid, btb = 1,4-bis(1,2,4-triazol-1- yl)butane, bth = 1,6-bis(1,2,4-triazol-l-yl)hexane), have been synthesized and characterized by elemental analysis, FT-IR and X-ray single-crystal diffraction. Complex 1 has a 2D sql layer. Complex 2 shows a (3,4)-connected 2D sheet with a (4.6^4.8)(4.8^2) topology. The thermal behavior of the two cor- responding complexes has briefly been investigated. 展开更多
关键词 Cu(Ⅱ) complex crystal structure 4-tert-butyl-phthalic acid 1 4-bis(1 2 4-triazol- 1-yl)butane 1 6-bis(1 2 4-triazol-1-yl)hexane
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Two Three-dimensional Supramolecular Complexes Assembled by 2-Chlorinebenzoic Acid and Bis(imidazol)Ligands:Syntheses,Structures and Fluorescent Properties 被引量:2
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作者 刘博 吕丛 +3 位作者 李秀梅 潘亚茹 车广波 周实 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2018年第11期1821-1828,共8页
Two new three-dimensional supramolecular complexes, namely, [Cd(cba)2(bib)]n(1) and [Zn(cba)2(bib)]2 n(2)(Hcba = 2-chlorinebenzoic acid, bib = 1,4-bis(imidazol-1-yl)-butane)were hydrothermally designed and synthesized... Two new three-dimensional supramolecular complexes, namely, [Cd(cba)2(bib)]n(1) and [Zn(cba)2(bib)]2 n(2)(Hcba = 2-chlorinebenzoic acid, bib = 1,4-bis(imidazol-1-yl)-butane)were hydrothermally designed and synthesized. Their structures were determined by elemental analyses, IR spectroscopy, TG, fluorescence spectroscopy, single-crystal and powder X-ray diffraction. Complex 1 exhibits a one-dimensional zigzag chain and complex 2 shows a zero-dimensional structure, which were further extended into three-dimensional supramolecular structures through hydrogen bonds and π-π stacking interactions. 展开更多
关键词 crystal structure Cd(Ⅱ) complex Zn(Ⅱ) complex 2-chlorinebenzoic acid 1 4-bis(imidazol-1-yl)-butane
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Polynuclear Silver(Ⅰ) Complexes with Phosphorus Ligands and 4,4'-Bipyridine:Synthesis,Structural Characterization and Spectroscopic Properties
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作者 崔洋哲 刘敏 +3 位作者 项今朝 李中锋 姚佳毅 金琼花 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2015年第1期140-146,共7页
Two novel silver(I) complexes {[Ag(OTf)(PPh3)(4,4'-bipy)]}∞(1) and {[Ag2-(OTf)2(dppb)3](CH3CN)4}∞(2)(OTf = trifluoromethanesulfonate, PPh3 = triphenylphophine, 4,4'-bipy = 4,4'-bipyridine, dppb... Two novel silver(I) complexes {[Ag(OTf)(PPh3)(4,4'-bipy)]}∞(1) and {[Ag2-(OTf)2(dppb)3](CH3CN)4}∞(2)(OTf = trifluoromethanesulfonate, PPh3 = triphenylphophine, 4,4'-bipy = 4,4'-bipyridine, dppb = bis(diphenylphosphino)butane) have been synthesized and characterized by IR, single-crystal X-ray diffraction, fluorescence spectrum and 1H NMR spectroscopy. Complex 1 crystallizes in orthorhombic, space group Pna21 with a = 19.259(2), b = 9.85070(12), c = 16.3827(17) A, V = 3108.0(5) A3, C29H23F3N2O3 PSAg, Mr = 675.39, Z = 4, Dc = 1.443 g/cm3, F(000) = 1360, μ = 0.816 mm-1, the final R = 0.0675 and w R = 0.1722 for 3662 observed reflections(I 〉 2σ(I)). Complex 2 crystallizes in triclinic, space group P1 with a = 12.9370(11), b = 13.5261(13), c = 16.4539(15) A, α = 106.7120(10), β = 97.3830(10), γ = 113.027(2)A, V = 2441.2(4)A3, C94H96F6N4O6P6S2Ag2, Mr = 1957.43, Z = 1, Dc = 1.331 g/cm3, F(000) = 1006, μ = 0.605 mm-1, the final R = 0.0717 and w R = 0.1795 for 5128 observed reflections(I 〉 2σ(I)). Complex 1 is of zigzag chain structure, in which each Ag atom is coordinated by one OTf- anion, two N atoms from two 4,4'-bipy molecules and one P atom from PPh3 ligand. In 2, the central Ag atom is coordinated with one OTf- anion and three P atoms from three dppb ligands, which leads to the formation of a zigzag ring-bridge-ring chain with each ring consisting of two Ag atoms and two dppb ligands. 展开更多
关键词 chain structures SILVER biPYRIDINE TRIPHENYLPHOSPHINE bis(diphenylphosphino)butane
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Crystal Structure and Theoretical Calculation of 1,4-Bis- (1-ferrocenesulfonyl-2-benzimidazolyl) Butane
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作者 Yue Kefen Zhuo Fei Zhai Gaohong Hou Lei Lei Yibo Yin Bin Wang Yaoyu 《Chinese Journal of Chemistry》 SCIE CAS CSCD 2011年第2期223-228,共6页
A N,N'-bisferrocenesulfonyl bisbenzimidazole compound 1,4-bis(1-ferrocenesulfonyl-2-benzimidazolyl) butane was prepared. Its crystal structure was determined. The crystal belongs to triclinic with space group P-1 a... A N,N'-bisferrocenesulfonyl bisbenzimidazole compound 1,4-bis(1-ferrocenesulfonyl-2-benzimidazolyl) butane was prepared. Its crystal structure was determined. The crystal belongs to triclinic with space group P-1 and a= 0.87241(13) nm, b=0.97553(15) nm, c= 1.4120(2) rim, and α= 83.041(2)°, β= 72.454(2)°,γy= 69.732(2)°, the unit cell volume V= 1.0746(3) nm3, the molecule number in one unit cell Z= 1, the absorption coefficient u= 1.191 mm 1, the calculated density Dc= 1.584 g/cm3. The theoretical investigation of the compound as a structure unit was fully optimized by B3LYP/6-31G method in Gaussian 03 package, and the most stable structure of the compound in theory was obtained. The two results were compared. The optimized structure was in accordance with the crystal structure in the main, suggesting that the molecular geometry optimization of the structures was reliable and the calculation method used was reliable. The distribution of atomic charges and the energy, and composition of frontier molecular orbits were analyzed. Thermal analysis indicated that it is stable before melting. 展开更多
关键词 1 4-bis(l-ferrocenesulfonyl-2-benzimidazolyl)butane crystal structure quantum chemistry therrnochemistry
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Synthesis and Characterization of New Macrocyclic Cu(Ⅱ) Complexes from Various Diamines, Copper(Ⅱ) Nitrate and 1,4-Bis(2-formylphenoxy)butane
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作者 ILHAN, Salih TEMEL, Hamdi KILIC, Ahmet 《Chinese Journal of Chemistry》 SCIE CAS CSCD 2007年第10期1547-1550,共4页
Six new macrocyclic complexes were synthesized by a template reaction of 1,4-bis(2-formylphenoxy)butane with diamines and Cu(NO3)2·3H2O and their structures were proposed on the basis of elemental analysis, F... Six new macrocyclic complexes were synthesized by a template reaction of 1,4-bis(2-formylphenoxy)butane with diamines and Cu(NO3)2·3H2O and their structures were proposed on the basis of elemental analysis, FT-IR, UV-Vis, magnetic susceptibility measurements, molar conductivity measurements and mass spectra. The metal to ligand molar ratios of the Cu(Ⅱ) complexes were found to be 1 : 1. The Cu(Ⅱ) complexes are 1 : 2 electrolytes as shown by their molar conductivities (∧m) in DMF at 10^-3 mol·L^-1. Due to the existence of free ions the Cu(Ⅱ) complexes are electrically conductive. Their configurations were proposed to be probably distorted octahedral. 展开更多
关键词 macrocyclic Schiff base complex 1 4-bis(2-formylphenoxy)butane diamine copper(Ⅱ) complex
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Syntheses, Structures, and Properties of Three Coordination Polymers: [Cd_2(bpp)_(1.5)(Hbpp)(phen)_2]_n, [Mn_3(Htptc)_2(phen)_2(H_2O)_2]_n, and {[Cu(btc)_(0.5)(1,4-bib)]·2H_2O}_n
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作者 丁元帅 范黎明 +2 位作者 逄越 张修堂 田来进 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2014年第4期569-578,共10页
Hydrothermal reactions of three aromatic polycarboxylic acids and the transitional metal cations in the presence of phen and 1,4-bib afford three new coordination polymers: [Cd2(bpp)1.5(Hbpp)(phen)2]n (1), [... Hydrothermal reactions of three aromatic polycarboxylic acids and the transitional metal cations in the presence of phen and 1,4-bib afford three new coordination polymers: [Cd2(bpp)1.5(Hbpp)(phen)2]n (1), [Mn3(Htptc)2(phen)2(H2O)2]n (2), and {[Cu(btc)0.5(1,4- bib)]·2H2O}n(3) (H2bpp = 2,6-bis(4'-carboxyphenyl)-4-phenylpyridine, H4tptc = terphenyl-2,5,2',5'-tetracar- boxylic acid, H4btc =biphenyl-2,2',4,4'-tetracarboxylic acid, phen =1,10-phenanthroline, and 1,4-bib = 1,4-bis(1H-imidazol-1-yl)benzene). Their structures have been determined by single- crystal X-ray diffraction analyses, elemental analyses, IR spectra, and powder X-ray diffraction (PXRD) analyses. In compound 1, the CdII cations are linked by bpp2- to form one ladder structure, based on which a 3D network is constructed with the help of non-covalent interactions. The topology of 2 is a 3D (3,4,5)-connected framework with the Point Schl?fli symbol of (42.6)2(43.62.8)(45.64.8)2. Compound 3 shows an unprecedented 3D (4,4)-connected framework with the Point Schl?fli symbol of (64.82)2(65.8). Moreover, the luminescent property of 1 has been investigated. 展开更多
关键词 2 6-bis(4'-carboxyphenyl)-4-phenylpyridine biphenyl-2 2' 4 4'-tetracarboxylic acid terphenyl-2 5 2' 5'-tetracarboxylic acid 1 10-phenanthroline 1 4-bis(imidazol-1-yl)butane
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以1,4-二氯甲氧基丁烷为氯甲基化试剂合成线型氯甲基化聚苯乙烯 被引量:20
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作者 申艳玲 杨云峰 +1 位作者 高保娇 朱勇 《高分子学报》 SCIE CAS CSCD 北大核心 2007年第6期559-565,共7页
采用自制的氯甲基化试剂——1,4-二氯甲氧基丁烷(BCMB),使用Lewis酸催化剂,在均相反应体系中高效地实现了聚苯乙烯的氯甲基化.研究了反应机理,考察了各种因素对氯甲基化反应的影响规律,优化了反应条件,通过红外光谱法与Volhard分析法表... 采用自制的氯甲基化试剂——1,4-二氯甲氧基丁烷(BCMB),使用Lewis酸催化剂,在均相反应体系中高效地实现了聚苯乙烯的氯甲基化.研究了反应机理,考察了各种因素对氯甲基化反应的影响规律,优化了反应条件,通过红外光谱法与Volhard分析法表征了产物的化学结构与组成.实验结果表明,反应机理可能由苯环亲电取代与伴随着醚键断裂的亲核取代两类反应构成,氯甲基化试剂用量、催化剂的酸性与用量、溶剂的性质与用量及反应温度等因素对反应都有显著的影响,其一,会影响聚苯乙烯的氯甲基化程度,其二,会导致或避免大分子链之间通过Friedel-Crafts反应而发生交联.以四氯化碳为溶剂、以SnCl4为催化剂并在较低温度(18℃)下进行反应,可制得氯甲基化程度达80%且完全线型化的氯甲基化聚苯乙烯. 展开更多
关键词 聚苯乙烯 1 4-二氯甲氧基丁烷 氯甲基化反应 亲电取代反应 醚键断裂反应
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制备氯甲基化聚苯乙烯交联微球的新方法 被引量:43
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作者 申艳玲 杨云峰 +1 位作者 高保娇 李刚 《高等学校化学学报》 SCIE EI CAS CSCD 北大核心 2007年第3期580-583,共4页
使用Lewis酸催化剂,用自制的氯甲基化试剂1,4-二氯甲氧基丁烷(BCMB),在室温下对聚苯乙烯交联微球(白球)进行氯甲基化反应,制得了氯含量接近17%的氯甲基化聚苯乙烯交联微球(氯球);通过红外光谱法与佛尔哈德分析法表征了产物的化学结构与... 使用Lewis酸催化剂,用自制的氯甲基化试剂1,4-二氯甲氧基丁烷(BCMB),在室温下对聚苯乙烯交联微球(白球)进行氯甲基化反应,制得了氯含量接近17%的氯甲基化聚苯乙烯交联微球(氯球);通过红外光谱法与佛尔哈德分析法表征了产物的化学结构与组成;考察了各种因素对氯甲基化反应过程的影响规律.结果表明,各种因素对白球氯甲基化过程的影响表现在两个方面:(1)影响白球的氯甲基化程度;(2)抑制或促进分子链之间通过Friedel-Crafts反应进一步交联,影响微球的强度. 展开更多
关键词 聚苯乙烯 1 4-二氯甲氧基丁烷 氯甲基化聚苯乙烯交联微球 氯甲基化反应
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高交联大孔吸附树脂氯甲基化研究 被引量:5
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作者 董方 陈振斌 +1 位作者 邸多隆 康磊 《精细化工》 EI CAS CSCD 北大核心 2010年第8期760-764,818,共6页
以无水ZnCl2为催化剂,以自制1,4-二氯甲氧基丁烷(BCMB)为氯甲基化试剂,对高交联度的非极性大孔吸附树脂D101进行氯甲基化反应研究。得到该氯甲基化的最佳工艺条件:m(D101)∶m(BCMB)∶m(CCl4)=1∶4∶18.6,溶胀时间12h,反应温度50℃,反应... 以无水ZnCl2为催化剂,以自制1,4-二氯甲氧基丁烷(BCMB)为氯甲基化试剂,对高交联度的非极性大孔吸附树脂D101进行氯甲基化反应研究。得到该氯甲基化的最佳工艺条件:m(D101)∶m(BCMB)∶m(CCl4)=1∶4∶18.6,溶胀时间12h,反应温度50℃,反应时间14h,以无水ZnCl2为催化剂,在该工艺条件下制得氯质量分数为4%的树脂,为以后树脂的改性、功能化和进一步研究大孔吸附树脂吸附分离规律提供了实验基础。 展开更多
关键词 1 4-二氯甲氧基丁烷 高交联度 大孔吸附树脂 氯甲基化 功能材料
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铽(Ⅲ)的双亚砜配合物的荧光性质 被引量:9
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作者 张若桦 马宝清 +2 位作者 鹿守亮 卜显和 王淑芳 《发光学报》 EI CAS CSCD 北大核心 1998年第2期150-154,共5页
测量了双(苯基亚砜)乙烷(bphse),双(苯基亚砜)丙烷(bphsp),双(苯基亚砜)丁烷(bphsb)和铽(Ⅲ)的配合物的吸收光谱和荧光光谱及其寿命.讨论了配体性质、阴离子及镧系离子对铽(Ⅲ)配合物荧光性能的影响.
关键词 铽配合物 双亚砜 荧光性质 发光强度
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氯甲基聚苯乙烯/硅胶复合微粒的制备与表征 被引量:6
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作者 戚昌盛 高保娇 刘青 《高分子学报》 SCIE CAS CSCD 北大核心 2008年第3期209-215,共7页
采用"接出(grafting from)"方式,在溶液聚合体系中将苯乙烯(St)接枝聚合在微米级硅胶表面,制备了接枝微粒PSt/SiO2;使用新型氯甲基化试剂1,4-二氯甲氧基丁烷,对接枝在硅胶表面的聚苯乙烯进行了氯甲基化(CM)反应,制得了氯甲基... 采用"接出(grafting from)"方式,在溶液聚合体系中将苯乙烯(St)接枝聚合在微米级硅胶表面,制备了接枝微粒PSt/SiO2;使用新型氯甲基化试剂1,4-二氯甲氧基丁烷,对接枝在硅胶表面的聚苯乙烯进行了氯甲基化(CM)反应,制得了氯甲基聚苯乙烯/硅胶(CMPS/SiO2)复合微粒.采用热重分析(TG)测定了PSt/SiO2的接枝度,并使用扫描电子显微镜(SEM)观察了其形貌;通过红外光谱法(FTIR)与佛尔哈德分析法表征了CMPS/SiO2的化学结构与组成.重点考察了各种因素对PSt/SiO2氯甲基化反应过程的影响规律.研究结果表明,CMPS/SiO2的制备不仅具有绿色环保的特点,而且反应容易控制.反应时间、溶剂种类与用量、催化剂种类与用量及氯甲基化试剂的用量等因素均会对该复合微粒的制备产生影响,如影响CMPS/SiO2的氯甲基化程度;抑制或促进已接枝的PSt大分子链之间通过Friedel-Crafts反应发生交联.若选用SnCl4为催化剂,以CH2Cl2为溶剂,在室温下反应10 h左右,可制得氯含量接近16 wt%(以接枝的PSt为基准计算)的CMPS/SiO2. 展开更多
关键词 聚苯乙烯 硅胶 1 4-二氯甲氧基丁烷 接枝聚合 氯甲基化反应
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1,1-二(4-羟基苯基)丁烷的合成与表征 被引量:2
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作者 王莉莉 张军营 +3 位作者 程珏 张耀平 张晓丰 林欣 《石油化工》 CAS CSCD 北大核心 2011年第4期425-429,共5页
以苯酚、正丁醛为原料合成了1,1-二(4-羟基苯基)丁烷(简称双酚BD),考察了以硫酸、盐酸和磷钨酸为催化剂的催化效果。实验结果表明,以磷钨酸为催化剂的效果最好,双酚BD的质量分数为98.40%,产物选择性好;以盐酸为催化剂,产物中双酚BD的含... 以苯酚、正丁醛为原料合成了1,1-二(4-羟基苯基)丁烷(简称双酚BD),考察了以硫酸、盐酸和磷钨酸为催化剂的催化效果。实验结果表明,以磷钨酸为催化剂的效果最好,双酚BD的质量分数为98.40%,产物选择性好;以盐酸为催化剂,产物中双酚BD的含量较低,副产物含量高;以硫酸为催化剂未得到目标产物,得到树脂状物质。以磷钨酸为催化剂,利用正交实验考察了反应温度、原料配比、催化剂用量和助催化剂巯基乙酸用量对反应的影响。得到优化的反应条件为:反应温度80℃、苯酚和正丁醛的摩尔比5、催化剂占反应物系总质量的0.50%、助催化剂占反应物系总质量的0.62%、反应时间4.0h;在此条件下,双酚BD的收率达62.5%;FTIR和1H NMR表征结果显示,合成的产物为双酚BD。 展开更多
关键词 苯酚 正丁醛 1 1-二(4-羟基苯基)丁烷 磷钨酸催化剂
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正交法优化氯甲基试剂BCMB合成条件的研究 被引量:2
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作者 李超 韩泳平 《西南民族大学学报(自然科学版)》 CAS 2011年第5期795-797,共3页
以l,4—丁二醇为原料,通过均相法合成了氯甲基化试剂1,4—二氯甲氧基丁烷(BCMB)并用红外光谱(IR)对产物进行了表征.采用正交试验法,考察了反应时间、反应温度、液料比三个因素对BCMB得率的影响.较佳的合成条件是:反应时间4小时,反应温度... 以l,4—丁二醇为原料,通过均相法合成了氯甲基化试剂1,4—二氯甲氧基丁烷(BCMB)并用红外光谱(IR)对产物进行了表征.采用正交试验法,考察了反应时间、反应温度、液料比三个因素对BCMB得率的影响.较佳的合成条件是:反应时间4小时,反应温度是20摄氏度,液料比是3:1时,产物的得率为80%. 展开更多
关键词 正交法 均相合成 BCMB 合成条件
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1,4-二叠氮-2,3-二叠氮甲基-2,3-二硝基丁烷的合成 被引量:8
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作者 王娟 刘大斌 周新利 《爆破器材》 CAS 北大核心 2012年第4期1-4,8,共5页
以硝基甲烷为原料合成了1,4-二叠氮-2,3-二叠氮甲基-2,3-二硝基丁烷,总收率为37.8%。采用1HNMR﹑IR和MS对目标产物及中间体的结构进行了表征。在三羟甲基硝基甲烷的合成中,结合反应机理确定了氢氧化钙的用量为:n(CH3NO2)n(Ca(OH)2)=10... 以硝基甲烷为原料合成了1,4-二叠氮-2,3-二叠氮甲基-2,3-二硝基丁烷,总收率为37.8%。采用1HNMR﹑IR和MS对目标产物及中间体的结构进行了表征。在三羟甲基硝基甲烷的合成中,结合反应机理确定了氢氧化钙的用量为:n(CH3NO2)n(Ca(OH)2)=1001;通过对催化剂浓硫酸﹑三氟化硼—乙醚络合物和对甲苯磺酸的比较,得出对甲苯磺酸为中间体2,2-二甲基-5-羟甲基-5-硝基-1,3-二氧杂环己烷合成的较优催化剂;分别采用2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四硝酸酯和2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四对甲苯磺酸酯与NaN3反应,发现磺酸酯基易离去,叠氮化反应更易进行,收率较高;叠氮化反应的较优溶剂为DMSO。DSC分析表明,1,4-二叠氮-2,3-二叠氮甲基-2,3-二硝基丁烷的分解峰温为223.46℃。 展开更多
关键词 1 4-二叠氮-2 3-二叠氮甲基-2 3-二硝基丁烷 合成 表征 含能增塑剂
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线型氯甲基聚苯乙烯的制备新方法 被引量:3
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作者 申艳玲 高保娇 《合成化学》 CAS CSCD 2007年第4期426-429,共4页
在均相反应体系中,以SnCl4为催化剂,CCl4为溶剂,自制的1,4-二氯甲氧基丁烷(BCMB)为氯甲基化试剂,制得了完全线型化的氯甲基聚苯乙烯(CMPS),其结构和组成经IR和佛尔哈德分析法表征。最佳氯甲基化反应条件为:聚苯乙烯2.0 g,BCMB 10 mL,SnC... 在均相反应体系中,以SnCl4为催化剂,CCl4为溶剂,自制的1,4-二氯甲氧基丁烷(BCMB)为氯甲基化试剂,制得了完全线型化的氯甲基聚苯乙烯(CMPS),其结构和组成经IR和佛尔哈德分析法表征。最佳氯甲基化反应条件为:聚苯乙烯2.0 g,BCMB 10 mL,SnCl41 mL,CCl430 mL,于18℃反应17 h。在最佳反应条件下,CMPS的氯甲基化程度达68%。 展开更多
关键词 聚苯乙烯 1 4-二氯甲氧基丁烷 氯甲基化反应
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高柔性线型配体1,4-双(2-甲基-8-喹啉氧基)-丁烷的合成与表征 被引量:1
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作者 蔡跃鹏 张利 +2 位作者 石俊玲 张华新 康北笙 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 北大核心 2003年第4期487-490,共4页
2-甲基-8-羟基喹啉和二溴丁烷在正丁基锂的存在下反应,生成标题化合物(C24H24N2O2, Mr = 372.46)。X-射线单晶结构分析表明此晶体属于单斜晶系,空间群P21/c, a = 5.7002(5), b = 12.186(1), c = 14.312(1) , b = 92.503(2), V = 993.2(2... 2-甲基-8-羟基喹啉和二溴丁烷在正丁基锂的存在下反应,生成标题化合物(C24H24N2O2, Mr = 372.46)。X-射线单晶结构分析表明此晶体属于单斜晶系,空间群P21/c, a = 5.7002(5), b = 12.186(1), c = 14.312(1) , b = 92.503(2), V = 993.2(2) 3, Z = 2, m = 0.080 mm-1, Dc = 1.245 g/cm3, F(000) = 396, R = 0.0505, wR = 0.0705. 结果表明,该化合物的2个配位端基2-甲基-8-羟基-喹啉基处于间隔基团-(CH2)4-的两侧,整个分子呈现中心对称的反式构象。此外,通过分子间的p…p 堆积作用和 CH…p 作用,使分子堆积成三维网络结构。 展开更多
关键词 柔性线型配体 1 4-双(2-甲基-8-喹啉氧基)-丁烷 合成 表征 晶体结构 螺旋体
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SBS氯甲基化反应工艺条件探讨 被引量:4
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作者 黄锦标 黄雪红 《广东化工》 CAS 2008年第11期25-28,31,共5页
研究了SBS的氯甲基化反应,考察了加料方式、反应温度、氯甲基化试剂、催化剂、溶剂、反应时间对SBS氯甲基化反应的影响因素,通过实验得到的最佳工艺条件为︰反应时间6 h,反应温度18℃,SBS甲苯溶液的质量浓度0.025 g/mL,n(SBS)︰n(SnCl4)... 研究了SBS的氯甲基化反应,考察了加料方式、反应温度、氯甲基化试剂、催化剂、溶剂、反应时间对SBS氯甲基化反应的影响因素,通过实验得到的最佳工艺条件为︰反应时间6 h,反应温度18℃,SBS甲苯溶液的质量浓度0.025 g/mL,n(SBS)︰n(SnCl4)︰n(ClCH2OCH2CH2CH2CH2OCH2Cl)=1.2︰1.0︰1.8时,SBS的氯甲基化程度达32.13%,通过红外光谱法与Volhard分析法表征了产物的化学结构与组成,测试了产物的溶解性能,并对SBS的氯甲基化反应机理进行初步探讨。 展开更多
关键词 SBS 1 4-二氯甲氧基丁烷 氯甲基化反应 交联
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