增白剂4,4'-双(2,4-二氯苯乙烯基)联苯的合成工艺及表征

以2,4-二氯苯甲醛、4,4'-二(氯甲基)联苯和亚磷酸三甲酯为原料,通过Arbuzow和Wittig-Horner反应合成了4,4'-双(2,4-二氯苯乙烯基)联苯荧光增白剂,两步合成的总收率93.1%以上,该物质具有很好的荧光增白效果,与CXT和CBS相比,白度有了很大的提高。     

4,4'-双(三氯甲基)联苯水解合成4,4'-联苯二甲酸工艺研究

以副产物4,4'-双(三氯甲基)联苯为原料,经碱性水解一步反应合成出4,4'-联苯二甲酸.考察反应物料摩尔比、反应温度、反应时间对4,4'-联苯二甲酸产品收率的影响,得到优化工艺条件:氯苯为溶剂,4,4'-双(三氯甲基)联苯与10％氢氧化钠溶液的摩尔比为1∶9,反应温度为105℃,反应时间为14 h.在上述条件下,4,...     

4,4'-双(氯甲基)联苯的合成

研究了 4,4′-双 (氯甲基 )联苯 ( BCMB)的合成方法及工艺条件。以多聚甲醛、联苯、氯化氢气体为原料 ,氯化锌为催化剂 ,经氯甲基化反应合成 BCMB,最佳工艺条件 :多聚甲醛∶联苯∶氯化锌 =2 .1～ 2 .3∶ 1∶ 1.68(摩尔比 ) ,氯化锌∶水 =2 .8(质量比 ) ,反应温度 5 6～ 60°C,反应时间 5 h。产品熔点 12 7-13 3°C,收率 (以联苯计 )达 48%。     

4,4'-联苯-3,3'-二(2,4-戊二酮)的合成与热谱研究

以4,4'-二(氯甲基)联苯和2,3-丁二酮-亚磷酸三甲酯(1:1)加合物为原料合成了标题化合物,采用核磁共振谱、质谱、红外光谱和紫外可见光谱对化合物进行结构表征.在静态空气气氛中用热重-差示扫描量热分析法(TG-DSC)对其进行了热分析研究:168～436 ℃之间质量损失76.67%,最后的固体残留物为联苯骨架不完全燃烧的残留物.在272 ℃有一个放热峰,在210、302 ℃分别出现强吸热峰.结果表明该固态化合物在168 ℃以下很稳定.     

4,4’-双(三氯甲基)联苯水解合成4,4’-联苯二甲酸工艺研究

以副产物4,4’-双(三氯甲基)联苯为原料,经碱性水解一步反应合成出4,4’-联苯二甲酸。考察反应物料摩尔比、反应温度、反应时间对4,4’-联苯二甲酸产品收率的影响,得到优化工艺条件:氯苯为溶剂,4,4’-双(三氯甲基)联苯与10%氢氧化钠溶液的摩尔比为1∶9,反应温度为105℃,反应时间为14 h。在上述条件下,4,4’-联苯二甲酸的收率为95.25%,纯度可达99.20%,通过红外光谱、核磁共振氢谱及高效液相色谱等对产物进行了表征。     

4,4'-双(氯甲基)联苯的合成

研究了 4,4′-双 (氯甲基 )联苯 ( BCMB)的合成方法及工艺条件。以多聚甲醛、联苯、氯化氢气体为原料 ,氯化锌为催化剂 ,经氯甲基化反应合成 BCMB,最佳工艺条件 :多聚甲醛∶联苯∶氯化锌 =2 .1～ 2 .3∶ 1∶ 1.68(摩尔比 ) ,氯化锌∶水 =2 .8(质量比 ) ,反应温度 5 6～ 60°C,反应时间 5 h。产品熔点 12 7-13 3°C,收率 (以联苯计 )达 48%。     

荧光增白剂4,4′-双-(2-磺酸钠苯乙烯基)联苯的合成新工艺

以氯化苄和对硝基氯苄为原料,经Wittig反应合成中间体2-磺酸钠-二苯乙烯和2-磺酸钠-4′-硝基-二苯乙烯。后者经还原反应、重氮化反应后,在氢氧化钠存在下与前者反应生成最终产品荧光增白剂4,4′-双-(2-磺酸钠苯乙烯基)联苯。     

4,4'-二氯甲基联苯的合成研究

本文通过催化剂种类与用量、溶剂、反应温度及时间的筛选与优化,使4,4'-二氯甲基联苯的收率达到87.8%,纯度达到98.0%,同时消除了有害物质二氯甲醚对环境的影响.     

荧光增白剂4,4''''-双-(2-磺酸钠苯乙烯基)联苯的合成新工艺

以氯化苄和对硝基氯苄为原料，经Wittig反应合成中间体2-磺酸钠-二苯乙烯和2-磺酸钠-4‘-硝基-二苯乙烯。后者经还原反应、重氮化反应后，在氢氧化钠存在下与前者反应生成最终产品荧光增白剂4，4‘-双-(2-磺酸钠苯乙烯基)联苯。     

植物生长调节剂2-(2,4-二氯苯氧基)三乙胺的合成新方法

以2,4 二氯苯酚为原料,采用相转移催化剂,经过醚化、胺化反应合成了2 (2,4 二氯苯氧基)三乙胺,总收率大于80%。研究了反应物的摩尔配比、反应时间及反应温度对2,4 二氯苯酚和二溴乙烷的醚化反应的影响,优惠工艺条件为:2,4 二氯苯酚与1,2 二溴乙烷配比为1∶30(mol/mol),反应温度80℃、反应时间10h。通过红外光谱、核磁共振氢谱和元素分析确定了目标化合物的结构。     

3,3',4,4'-联苯四甲酸二酐的合成研究

以4-氯-邻苯二甲酸酐为原料,经酯化、偶联、水解、脱水合成标题化合物。目标化合物须保存在真空干燥箱中,防止水分倾入。通过改进工艺路线,可得到高收率、高纯度的目标产物,使工业化生产成为可能,为全芳香族聚酰亚胺的生产提供高质量原料。     

Magnetoelectrochemistry of 4,4′-bis(dimethylamino)biphenyl and 4,4′-dinitrobiphenyl azacrown macrocyclic lactams

The voltammetric behaviour at carbon fibre microelectrodes under the application of static magnetic fields of two series of macrolactams containing in their structure 4,4′-bis(dimethylamino)biphenyl or 4,4′-dinitrobiphenyl groups in MeCN solution is described. The response of 4,4′-dinitrobiphenyl receptors is dominated by two successive one-electron reduction processes at −0.9 and −1.6 V versus AgCl/Ag. 4,4′-bis(dimethylamino)biphenyl-containing receptors display two one-electron oxidations above +0.8 and +1.0 V. In both cases, a dihedral/planar interconversion precedes the second electron transfer step. Upon application of moderate (0.05-0.2 T) static magnetic fields to the electrochemical cell, the rate of such dihedral/planar interconversion is lowered for both the reduction of 4,4′-dinitrobiphenyl receptors and the oxidation of 4,4′-bis(dimethylamino)biphenyl lactams. The electrochemical response of N-methylated receptors, for which different cisoid-cisoid, cisoid-transoid, and transoid-transoid forms exist, exhibits a significant peak splitting that can be associated to the presence of such conformational isomers. Application of magnetic fields produces a relative enhancement of some peaks that can be interpreted in terms of differential magnetoconvection involving such conformational isomers.     

4,4'-二羟基联苯合成新方法研究

设计了一种合成4,4'-二羟基联苯的新方法,以联苯为原料,经Friedel-Crafts酰基化反应、Baeyer-Villiger氧化反应、酯水解反应得到4,4'-二羟基联苯。中间体和产物的结构均经1H NMR、元素分析和熔点仪进行表征确认,并且对反应条件进行了优化,取得了较高的收率。     

Synthesis and characterization of donor-acceptor type 4,4′-bis(2,1,3-benzothiadiazole)-based copolymers

A series of novel donor-acceptor type polymers based on 4,4′-bis(2,1,3-benzothiadiazole) were synthesized and characterized. Two soluble regioregular tail-to-tail and head-to-head coupled polymers, poly[7,7′-bis(3-octyl-2-thienyl)-4,4′-bis(2,1,3-benzothiadiazole)] poly[3TBB3T], and poly[7,7′-bis(4-octyl-2-thienyl)-4,4′-bis(2,1,3-benzothiadiazole)] poly[4TBB4T] were synthesized by FeCl₃-mediated oxidative polymerization. To further decrease the band gap of the polymers, vinylene spacers were incorporated into the polymer backbone by Stille coupling of the corresponding monomers and (E)-1,2-bis(tributylstannyl)ethene. A crystal structure of a monomer analog shows near planar arrangement of the aromatic units in the solid state. The optical properties of the monomers and polymers were investigated by steady-state absorption and photoluminescence spectroscopy. Cyclic voltammetry measurements indicate that the polymers could be employed as acceptor materials in polymer-polymer bulk heterojunction solar cells due to their low LUMO energy of about −4.0 eV. A maximum photovoltaic power conversion efficiency of about 0.3% was observed for a 1:1 blend of regioregular poly(3-hexylthiophene) (rr-P3HT) and poly[4TBB4T] and the origin of the moderate efficiency is discussed by interpreting the device current-voltage characteristics, external quantum efficiency and incident light intensity dependence of the power conversion efficiency.     

4,4’,4”-三腈基三苯甲烷的合成

对4,4’,4-三腈基三苯甲烷的合成方法进行了研究。以苯胺和对氰基苯甲醛为起始原料经两步反应制得目标产物。     

Rheological characterization of 4,4′-bis(diethylamino)benzophenone-functionalized polybutadienes with low and medium vinyl content

An experimental study was undertaken to investigate the thermomechanical properties of a certain epoxy/amine configuration. The basic structure of all the epoxies was the same—DGEBA—and the curing agent used was PACM 20. By varying the epoxy prepolymer molecular weight and the stoichiometry between epoxy and amine, a range of different epoxy networks were produced. Glass transition temperatures were evaluated by using differentil scanning calorimetry (DSC). Modulus values as well as an alternative T_g determination were provided by dynamic mechanical analysis (DMA). Coefficients of thermal expansion were obtained from thermomechanical analysis (TMA). The tensile tests conducted at room and elevated temperatures provided additional modulus data along with the yield point, tensile strength, and elongation at break data. Property vs. stoichiometry curves exhibited a maximum for the glass transition temperature and the over the T_g modulus at the stoichiometric point. On the other hand, the under T_g modulus showed a minimum at the stoichiometric point. The results of the yield strength show remarkable similarity with the results of the modulus. Strength and elongation at break do not show clear trends, but a much different behavior is exhibited between room and elevated temperatures. © 1996 John Wiley & Sons, Inc.     

Rheological characterization of 4,4′-bis (diethylamino)benzophenone-functionalized polybutadienes with low and medium vinyl content

In this article a mechnical spectroscopic study of a series of low (?8%) and medium (? 70%) vinyl-content polybutadiences, some of them functionalized with 4,4′-bis(diethylamino)-benzophenone, is presented. Characterization of polymers with well-known structure by small-amplitude oscillatory shear flow enabled investigation of the effect of the vinyl content and functional groups on the rheological behavior of the samples in the linear viscoelastic region. The Doi–Edwards viscolastic model, without any adjustable parameter, proved to be adequate to describe the relationship between the macro/micro structure of the polymers and their viscoelastic properties. Results indicate that the vinyl content and functional groups modify the rheological behavior extensively. © 1995 John Wiley & Sons, Inc.