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以DMF作溶剂,在四丁基氟化铵 (TBAF)存在下,对甲基苯基三甲硅基醚(1)和4,4'-二氯二苯砜(2)于100 ℃反应1 h,合成了4,4'-二(4-甲基苯氧基)二苯砜(3),产率为92%;加入催化量的N-溴代丁二酰亚胺(NBS)并在光照条件下,与氧气反应得到中间体-4,4'-二(4-羧基苯氧基)二苯砜(4),其产率达90%;将化合物4与二氯亚砜反应合成目标产物4,4'-二(4-氯甲酰基苯氧基)二苯砜(5),总收率为74.5%(以对甲基苯基三甲硅基醚为基准计算). 相似文献
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以两种V型的配体4,4′-二吡啶基苯(1,3-dpb)和4,4′-二羧基二苯砜(H2sdb),和钴(Ⅱ)通过溶剂热反应合成了1个配位聚合物{[Co(dpb)(sdb)(H2O)2]·2H2O·DMF}n(1)。对其进行了红外、热重、粉晶衍射、单晶衍射等表征,配合物属于三斜晶系,空间群P1。其中Co(Ⅱ)的2个顶点被水分子占据,相邻的钴(Ⅱ)离子连接着1,3-二吡啶基苯和4,4′-二羧基二苯砜形成一维的双绳链,相邻的链之间通过羧基-配位水和配位水-配位水间的氢键相互连接形成二维的层状结构,层状结构之间通过砜基-配位水间的氢键又相互连接形成三维结构。此外,还研究了配合物的固体紫外-可见光谱。 相似文献
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本文先通过缩合反应合成羟端基的二酰亚胺单体, 然后利用亲核缩聚反应, 与4,4′-二氯二苯砜及3,3′-二磺酸钠基-4,4′-二氯二苯砜共聚, 制备聚合物. 该合成路线反应周期短, 对温度和溶剂等条件要求不高, 简便易得. 相似文献
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一种新型聚酰亚胺离子型共聚物的合成与表征 总被引:1,自引:0,他引:1
以过氧化氢为氧化剂,在三氟乙酸中对2,6-二氯吡啶进行氧化,制备了2,6-二氯吡啶氮氧化物,该单体与4,4′-二巯基二苯砜、3,3′-二甲基-双(4-氯代酰亚胺)-4,4′-二苯甲烷(4-BCPI)通过亲核取代反应生成了含有离子基团的聚酰亚胺。采用红外分析(FT-IR)、黏度测试、溶解度实验、热失重分析(TGA)和示差扫描量热分析(DSC)等测试方法,对所合成的聚酰亚胺的结构与性能进行了表征。测试结果表明:该类聚酰亚胺在室温下不仅可溶于常用的极性非质子有机溶剂,也能溶于氯仿、吡啶等溶剂。此外,10%热失重温度高于430℃,玻璃化转变温度高于210℃。 相似文献
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以4,4′-二甲基-2,2′-二联吡啶为原料,经酸化、酰氯化,酯化和缩合反应合成了两个新型的4,4′-双取代-2,2′-二吡啶衍生物—4,4′双(4,5-二苯基嗯唑-2-基)-2,2′-二吡啶(6a)和4,4′-双(4,5-二对甲氧基苯嗯唑-2-基)-2,2′-二毗啶(6b),其结构经1H NMR,IR和MS表征.用UV-Vis和荧光激发光谱测定了6a和6b的光学性能,结果表明,6a和6b的λmax分别为229 nm和238 nm;最大发射波长均为432 nm. 相似文献
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A novel reactive polycarboxylic acid dye was synthesized by the reaction of polymaleic anhydride(PMA) with 3-methyl-1-(4- sulfonylphenyl)-4-(4-aminophenylazo)-2-pyrazoline-5-one.The structure of the novel dye was characterized by FTIR,UV-vis and 13C NMR spectra.The dyeing properties of dye on cotton were tested,and the novel dye possessed high fixation and good fastness. 相似文献
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A novel polyaniline/Bi(2)SnTiO(7 )composite polymer was synthesized by chemical oxidation in-situ polymerization method and sol-gel method for the first time. The structural properties of novel polyaniline/Bi(2)SnTiO(7) have been characterized by X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy and X-ray spectrometry. The lattice parameter of Bi(2)SnTiO(7) was found to be a = 10.52582(8) ?. The photocatalytic degradation of methylene blue was realized under visible light irradiation with the novel polyaniline/Bi(2)SnTiO(7) as catalyst. The results showed that novel polyaniline/Bi(2)SnTiO(7 )possessed higher catalytic activity compared with Bi(2)InTaO(7) or pure TiO(2) or N-doped TiO(2) for photocatalytic degradation of methylene blue under visible light irradiation. The photocatalytic degradation of methylene blue with the novel polyaniline/Bi(2)SnTiO(7) or N-doped TiO(2) as catalyst followed first-order reaction kinetics, and the first-order rate constant was 0.01504 or 0.00333 min(-1). After visible light irradiation for 220 minutes with novel polyaniline/Bi(2)SnTiO(7 )as catalyst, complete removal and mineralization of methylene blue was observed. The reduction of the total organic carbon, the formation of inorganic products, SO(4)2- and NO(3-), and the evolution of CO(2) revealed the continuous mineralization of methylene blue during the photocatalytic process. The possible photocatalytic degradation pathway of methylene blue was obtained under visible light irradiation. 相似文献
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氧化钙和氟化钾负载高岭土固体碱催化制备新型生物柴油 总被引:1,自引:0,他引:1
以高岭土为载体,利用浸渍法制备了氧化钙和氟化钾负载高岭土固体碱(GCK);利用X射线粉末衍射(XRD)、扫描电子显微镜(SEM)、红外光谱(FT-IR)和哈密特指示剂法等技术手段对催化剂进行表征;考察了KF负载量和反应条件对月桂酸甲酯(ML)与乙二醇单甲醚(EGME)酯交换反应制备新型生物柴油产率的影响。 结果表明,GCK碱强度(H_)在7.2~18.4之间,KCaF3为主要活性组分,当氟化钾负载量为25%、EGME与ML摩尔比3.0、催化剂用量相对于ML的质量分数为4.5 %、120 ℃下反应2 h,新型生物柴油的收率高达97.1%。 最后对催化剂的重复利用性能进行了考察。 相似文献
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Razieh FAZAELI Hamid ALIYAN Shadpour MALLAKPOUR Zahra RAFIEE Maryam BORDBAR 《催化学报》2011,32(4):582-588
A novel compound constructed from polyoxometalate (H3PW12O40,PW12) and poly(amidoamine) (PA) was prepared at room temperature in an aqueous solution by an impregnation method.A series of novel 1,3,5-triaryl-2-pyrazoline derivatives was synthesized by the reaction between chalcone and phenylhydrazine in the presence of the title compound,PW12/PA,in high yields.The structures of the compounds obtained were determined by IR and 1H NMR spectra. 相似文献
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Shaojian Lin Jiaojiao Shang Jianwu Lan Ronghui Guo Xia Huang Wen He 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(10):1060-1069
A novel thermally stable thermoplastic poly(ester-ether) (PEE) elastomer containing imide units was prepared from poly(tetramethylene glycol) (PTMG1000), 1,4-butanediol (BD) and a new imide dicarboxylic acid based on pyromellitic dianhydride (PMDA) and glycine through a traditional chemical two-step method. The structures of the synthesized imide dicarboxylic acid and novel PEE were confirmed by FT-IR spectroscopy. The mechanical properties of the novel PEE were investigated. Thermal stability and thermal degradation kinetics of the novel PEE were investigated by thermogravimetric analysis (TGA) under different heating rates. The kinetic parameters of the degradation process were determined by using Kissinger, Flynn–Wall–Ozawa and Friedman methods. The Coats–Redfern method was also used to discuss the probable degradation mechanism of this PEE. The results showed that introduction of the imide units into the poly(ester-ether) endowed the PEE with excellent thermal stability and good mechanical properties. The activation energy obtained by using the Kissinger method was in agreement with that using the Flynn–Wall–Ozawa method. The reaction order (n) and pre-exponential factor (A) were obtained by using the Friedman method. Analysis of the experimental results suggests that the decomposition reaction mechanism of the PEE was a F3 type (random nucleation with three nuclei on the individual particle). 相似文献
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Jiangnan Peng Scott G. Franzblau Fangqiu Zhang Mark T. Hamann 《Tetrahedron letters》2002,43(52):9699-9702
Two novel sesquiterpenes, styxone A (1) and styxone B (2), and a novel lactone, styxlactone (3), were isolated from the Jamaican sponge Myrmekioderma styx. Their structures were elucidated by detailed 1H, 13C and 2D NMR data and the absolute stereochemistry of styxone A and B was determined by CD spectra. Styxone A represents a novel sesquiterpene skeleton. (S)-(+)-Curcuphenol (4), (S)-(+)-curcudiol (5), and abolene (6) were also isolated. An activity enhancement by cyanthiwigin B (7) to curcuphenol was observed in the antimicrobial assays when the two compounds were administered together. 相似文献
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《中国化学快报》1999,(5)
Pci}linlidesareac'ellknownasolleofthe"lostinlportalltclassesof1llgh-perf'ornlance.pci}'nlers.Ilo-c'lever.thed'utilizationisgreatl}'limitedduetotheirpoorhandlingandprocessingcharacteristics'.Anulllberofmethodsincludingincorporationtlexibleornons}l'mmetricallinkagesinpolymerbackboneorusingmollonlersfaithbulkysubstituents.havebeenusedtoilllprovetheirsolubility.Poly(anlide-ilnide)shavealsobeenprovidedatbvorablebalancebetweellprocessability'andperforlllance'.illtillsletter.Wesynthesizedanovelnlonom… 相似文献
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新型树状单分子磷-氮膨胀阻燃剂的合成及阻燃性能研究 总被引:1,自引:0,他引:1
以六氯环三磷腈、对羟基苯甲醚、新戊二醇以及三氯氧磷等为原料, 合成一种新型树状单分子磷-氮膨胀阻燃剂六(4-(5,5-二甲基-1,3-二氧杂环己内磷酸酯基苯氧基))环三磷腈(Ⅵ). 标题化合物结构经IR、MS 及1H NMR 证实. 热失重分析表明标题化合物具有较高的热稳定性和良好的成炭性, 氮气氛下的起始分解温度为270 ℃, 600 ℃时炭残余量达45.2%. 实验表明, 标题化合物对环氧树脂呈现出良好的阻燃效果. 相似文献