1,8-二羟基-9,10-二氢蒽的合成

以1,8-二羟基蒽醌为原料,经甲醚化,锌粉和金属钠还原,去甲基等4步反应合成1,8-二羟基-9,10-二氢蒽,总产率为37.1,8-二甲氧基蒽醌用NaBH₄/CF₃COOH还原生成二聚产物,并测定了其单晶结构.     

Generation of Singlet Diatomic Sulfur from 9,10-Epidithio-9,10-dihydroanthracene

The novel 9,10-epidithio-9,10-dihydroanthracene ( ) was formed as an intermediate in the reaction of 9,10-dihydro-9,10-(1,3-epidithio-2-methano- 2-p-methoxyphenyl-1-oxide)propanoanthracene ( ) with perchloric acid. Singlet diatomic sulfur was generated from endodisulfide and trapped with conjugated dienes.     

含联苯结构聚醚醚酮酮共聚物和共混物的制备及性能研究

聚醚醚酮（PEEK）是八十年代初投入市场的全芳香结构热塑性耐高温特种工程塑料，它的7’。一143“C，Tm一334C“‘，最大结晶度为48％，典型制品结晶度为20％～30％［”．PEEK可用通常的设备成型，其制件、纤维、涂料及复合材料在电子电器、机械设备、交通运输、宇航、原子能工程、军事等领域有广泛的用途［’j．聚醚醚酮酮（PEEKK）是继PEEK之后，由德国Hoechst公司开发出来的又一种全芳香结构热塑性耐高温特种工程塑料［‘j．为了研究该类聚合物的结构和性能的关系，我们在实验室中合成了PEEKK和含联苯结构聚醚醚酮酮（PE－＊…     

聚醚醚酮醚酮的合成与表征

聚醚醚酮（ＰＥＥＫ）自工业化以来［１］，由于其优异的性能已在机械、航天等领域得到广泛应用．各种聚芳醚酮类聚合物相继被开发出来．但以亲电缩聚路线制备聚醚醚酮醚酮（ＰＥＥＫＥＫ）的报道较少［２］．本文以二苯醚和４－氟苯甲酰氯为主要反应试剂，采取付氏酰基化...     

Synthesis of photoreactive poly(ether ether ketone)s containing alkyl groups

Poly(ether ether ketone)s containing alkyl groups were prepared by nucleophilic substitution reaction of alkyl-substituted difluoro diaryl ethers with hydroquinone or by electrophilic substitution reaction of alkyl-substituted diaryl ether with 4,4′-oxydibenzoic acid in PPMA. Polycondensations proceeded smoothly and produced polymers having inherent viscosities up to 0.5-–1.6 dL/g. The polymers were quite soluble in strong acid, dipolar aprotic solvents, and chloroform at room temperature. Thermogravimetry of the polymers showed excellent thermal stability, indicating that 10% weight loses of the polymers were observed in the range above 450°C in nitrogen atmosphere. The glass transition temperatures of the polymers ranged from 128 to 146°C. Furthermore, Polymer 3b functioned as a photosensitive resist of negative type for UV radiation. The resist had a sensitivity of 42 mJ/cm² and a contrast of 2.5, when it was postbaked at 100°C for 10 min, followed by development with THF/acetone at room temperature. © 1996 John Wiley & Sons, Inc.     

Structure of a 1:1 molecular complex of trans-9,10-dihydroxy-9,10-diphenyl-9,10-dihydroanthracene with ethanol

X-ray analysis of the title complex revealed hydrogen-bonded chains comprising two crystallographically independent types of $\text{trans}$-9,10-dihydroxy-9,10-diphenyl-9,10-dihydroanthracene molecules, in which the central 1,4-cyclohexadiene rings are respectively flat and very slightly puckered, with the ethanol molecules attached exclusively to the latter type.     

聚芳醚酮醚酮酮类聚合物的结晶与多晶型

晶体结构;聚芳醚酮醚酮酮类聚合物的结晶与多晶型     

聚醚醚酮/聚醚醚酮酮共混体系的熔融和等温结晶行为

采用熔融共混方法制备了聚醚醚酮和聚醚醚酮酮的共混物,用DSC对共混物的熔融行为和等温结晶行为进行了研究.结果表明,共混物熔点随聚醚醚酮含量增加而降低,但与聚醚醚酮酮有相同的平衡熔点,二者共混没有改变其结晶的成核与生长机制.     

聚醚酮醚酮酮/含萘环聚醚酮醚酮酮无规共聚物的合成与性能

在无水AlCl3及N－甲基吡咯烷酮（NMP）存在下，以4,4′-二（α－萘氧基）二苯酮（DNBP）作为第三单体，将其与4，4′－二苯氧基二苯酮（DPBP）和对苯二甲酰氯（TPC）在1，2－二氯乙烷（DCE）中进行低温溶液共缩聚反应，合成了一系列聚醚酮醚酮酮／含萘环聚醚酮酮醚酮酮无规共聚物，用IR、DSC、TG及WAXD等方法对其结构和性能进行了表征与测试。研究结果表明共聚物的玻璃化转变温度（Tg)要比纯PEKEKK的高，而其熔融温度（Tm)和结晶度（Xc)则随共聚物中含萘环PEKEKK结构单元含量的增加而逐渐降低。共聚物具有优异的耐热性能及抗腐蚀性能。     

Complexation with diol host compounds. Part 18. Structures and thermal analysis of trans-9,10-dihydroxy-9,10-di-p-tolyl-9,10-dihydroanthracene and its inclusion compounds with acetone,diethyl ether and pyridine

Abstract

The structure of the host compound trans-9,10-dihydroxy-9,10-di-p-tolyl-9,10-dihydroanthracene and those of its inclusion compounds with acetone, diethyl ether and pyridine have been elucidated. The non-porous α-phase of the host has a structure in which the molecules are packed in layers parallel to the (100) plane, but exhibit no intermolecular hydrogen bonding. The host:guest stoichiometry of each inclusion compound is 1:2, and the structures are each stabilised by O-H…O or O-H…N hydrogen bonds between host and guest. The thermal decompositions of the acetone and diethyl ether compounds are characterised by single endotherms of the guest-release reaction, but the pyridine inclusion compound has a more complex decomposition, characteristic of similar pyridine inclusion compounds.     

Synthesis of copolymers of poly(ether sulfone ether ketone ketone) and poly(ether ketone diphenyl ketone ether ketone ketone) by electrophilic Friedel–Crafts solution polycondensation

A new monomer, 4,4′‐bis(4‐phenoxybenzoyl)diphenyl(BPOBDP), was synthesized via a two‐step synthetic procedure. A series of novel poly(ether sulfone ether ketone ketone)/poly(ether ketone diphenyl ketone ether ketone ketone) copolymers were prepared by electrophilic Friedel–Crafts solution copolycondensation of isophthaloyl chloride (IPC) with a mixture of 4,4′‐diphenoxydiphenylsulfone (DPODPS) and 4,4′‐bis(4‐phenoxybenzoyl)diphenyl (BPOBDP), in the presence of anhydrous aluminum chloride and N‐methylpyrrolidone (NMP) in 1,2‐dichloroethane (DCE). The copolymers with 10–50 mol% DPODPS are semicrystalline and have remarkably increased T_gs over commercially available PEEK and PEKK. The copolymers with 40–50 mol% DPODPS had not only high T_gs of 170–172°C, but also moderate T_ms of 326–333°C, which are extremely suitable for melt processing. These copolymers have tensile strengths of 96.5–108.1 MPa, Young's moduli of 1.98–3.05 GPa, and elongations at break of 13–26% and exhibit excellent thermal stability and good resistance to acidity, alkali, and common organic solvents. Copyright © 2009 John Wiley & Sons, Ltd.     

聚醚醚酮酮和含联苯聚醚醚酮酮共聚物的熔融热

根据Ｆｌｏｒｙ热力学统计理论和比容－熔融热作国法，由ＤＳＣ结果得到了不同联苯含量的聚醚醚酮酮－含联苯聚醚醚酮酮（ＰＥＥＫＫ－ＰＥＢＥＫＫ）共聚物的熔融热，两种方法获得的结果吻合。在此基础上给出了ＰＥＥＫＫ－ＰＥＢＥＫＫ共聚物不同联苯含量的熔点计算表达式。结果还表明，随着联苯含量ｎＢ，的变化，明显改变；当ｎＢ＝０．３５时，ＰＥＥＫＫＰＥＢＥＫＫ共聚物的值最小。     

Synthesis and properties of poly(aryl ether ether ketone) copolymers with pendant methyl groups

Polyether ether ketone and polyether ether ketone copolymers were prepared by the nucleophilic substitution reaction of 4,4′-difluorobenzophenone with hydroquinone and with varying mole proportions of hydroquinone and methyl hydroquinone using sulfolane solvent in the presence of anhydrous K₂CO₃. The polymers were characterised by different physico-chemical techniques. The crystallinity of the polymers was found to decrease with increase in concentration of the methyl hydroquinone units in the polymer. Thermogravimetric studies showed that all the polymers were stable upto 430 °C with a char yield above 49% at 900 °C in N₂ atmosphere. The glass transition temperature was found to increase and the crystalline melting temperature and activation energy were found to decrease with increase in concentration of the methyl hydroquinone units in the polymer.     

Steric effects in the electroreduction of 9-anthryl styryl ketone and 9,10-anthryl bis(styryl ketone)

The electrochemical behavior of 9-anthryl styryl ketone (ASK) and 9,10-anthryl bis(styryl ketone) (ABSK) in acetonitrile and N,N-dimethylformamide at a Pt electrode was investigated by cyclic and rotating ring disk electrode (RRDE) voltammetry and controlled potential coulometry. ASK is reduced in a reversible one-electron step to form the radical anion which rapidly couples (k₂=10⁵M^?1 s^?1) to form the dimeric dianion. The dimer can be reoxidized to form ASK. ABSK is reversibly reduced to the stable dianion which shows no tendency to couple. The cyclic voltammogram wave shape suggests that the styryl-keto groups in the 9-and 10-positions are non-interacting so that the reduction occurs in two steps whose standard potentials differ by the statistically predicted 36 mV.     

含三苯基膦聚醚醚酮酮的结构与性能

以双[4-(对氟苯甲酰基)苯基]苯基氧化膦和对苯二酚(HQ)为单体, 合成了新型主链含三苯基膦结构的聚醚醚酮酮, 并对聚合物的结构和性能进行了表征.     

含氟聚醚醚酮酮的制备及其性能

以邻氟对苯二酚和4,4′-二氟三苯二甲酮为原料通过亲核缩聚反应,合成含氟聚醚醚酮酮(FPEEKK)材料。 用FTIR、1H NMR和WAXD进行了结构表征,用DSC、TGA测试了热性能,并研究了聚合物的溶解性、吸水性、介电性能及光学性能。 结果表明,含氟聚醚醚酮酮具有较好的热性能（N2气气氛中,5%热分解温度为505 ℃）;能溶于氯仿、四氢呋喃和N,N-二甲基甲酰胺等有机溶剂;具有较低的吸水率(0.24%)和介电常数（ε=3.0）;在近红外区1300和1550 nm处吸收非常弱。