Syntheses of novel macrocyclic polyarylate oligomers based on phenolphthalein and m-phthaloyl-dichloride

Novel macrocyclic oligomers were synthesized through the condensation of phenolphthalein and m-phthaloyl-dichloride with triethylamine as catalyst in the mixed solution of methylene chloride and THF via pseudo-high-dilution technique. The oligomers were characterized by IR, H-1 NMR, MS, WAXD, TGA and DSC. It was found that the 3 : 3 adduct (molar ratio of phenolphthalein to m-phthaloyl-dichloride) and the 4 : 4 adduct were the main products and there was a small amount of crystalline in the macrocyclic mixtures. When the mixtures were heated to 360 degrees C, the crystalline disappeared.

Preparation and characterization of doped polyaniline films

Stable monolayer of the polyaniline doped with camphor sulfonic acid at the air-water interface has been obtained, of which multilayers have been successfully deposited by Langmuir-Blodgett technique onto CaF2 substrate. The limiting mean molecular area and collapse pressure are found to be 0.294 nm(2) and 41 mN/m, respectively. The multilayers were characterized by IR and W-Vis-NIR spectroscopies. X-ray small-angle diffraction data show that the multilayer was periodic layer structure with the layer spacing of 1.60 nm. The comparisons are also made with characterization of the casting film. (C) 1999 Elsevier Science S.A. All rights reserved.

Luminescence of unusual bismuth in barium berates BaB8O13 : Bi)

The luminescence of unusual divalent bismuth (Bi2+) in BaB8O13 is reported. The emission band with maximum peak at 592 nm corresponds to the P-2(3/2)-->P-2(1/2) transition of Bi2+ in the matrix and the excitation spectrum with two bands peaked at 470 and 580 nm respectively corresponds to two split crystal-field levels of P-2(3/2) state. The small Stokes shift (similar to 350 cm(-1)) reflects the rigid structure of the host for the Bi2+ ions.

Synthesis and characterization of thermotropic liquid crystalline poly(ester imide)s

Two closely series of poly(ester imide)s had been synthesized by solution polycondensation of p-phenylenebis(trimellitate) dianhydride with aliphatic diamines. The differential scanning calorimetry (DSC) traces of the most poly(ester imide)s exhibited two endotherms representing the solid state to anisotropic phase transition (T-m1) and the anisotropic to isotropic melt transition (T-m2), respectively. Observation under polarizing microscope and wide-angle X-ray diffraction (WAXD) measurements suggested that the anisotropic phase formed above the melting paints (T-m1) had a smectic character. The thermogravimetric analyses (TGA) revealed that the thermal stabilities of the poly(ester imide)s were up to 350 degrees C. (C) 1999 John Wiley & Sons, Inc.

聚苯胺在防腐领域的应用

综述导电聚苯胺用于金属防腐蚀领域的最新进展，并且探讨了其相关的防腐机理。

Synthesis and investigation of monoesters of polymaleic acids with azo-group

A series of amphiphilic polymers, monoesters of polymaleic acid containing ate-side groups (PMAN-A(n)Me) was synthesized by the reaction of alcohol(A,Me) with polymaleic anhydride (PMAN) for Langmuir-Blodgett assembly. The effects of the length of flexible spacer in the side chain on the pi-A isotherms and LB films were investigated. The UV-Vis and infrared linear dichroism spectra showed that the ate-side groups were highly oriented in PMAN-A(6)Me LB film deposited on silica or CaF2 substrate.

Study on the Adsorption and Activation of NO and CO over Mixed Oxide Catalysts Containing Cu by Means of TPSR

Adsorption and activation of small molecules NO, CO and CO+ NO on LaSrCuO4, La2CuO4 and La1.7Th0.3CuO4 which are typical samples in the sence of nonstoichiometric oxygen(lambda) anrong the series of La2-x(SrTh)(x)CuO4 +/-lambda mixed oxide catalysts were studied by means of MS- TPD (TPSR ), XRD, chemical analysis and so on. It was shown that the adsorption amount of NO can be correlated with the content of oxygen vacancy while the types and strength of adsorption of NO could be related to the oxidation state of the metallic ion. It was also found that CO molecule was first converted into CO32- and then desorbed in the form of CO2 at high temperature during the adsorption and desorption of CO on the mixed oxide with oxygen vacancy. The fact that the profiles of TPD(TPSR) of NO in co-adsorption of NO+CO and in single NO adsorption are similar shows that the adsorption of NO molecule not only has some priority to that of CO but also is stronger than that of CO. It seems that the adsorption of NO plays a dominate role in the activation and decomposition of NO.

含Cu复合氧化物对NO和CO吸附和活化的TPSR研究

利用MS－TPD法并结合XRD、化学分析等对催化剂进行了表征，探讨了K2NiF4结构La2-x(Sr，Th)xCuO4±λ系催化剂中三个典型样品LaSrCuO4、La2CuO4和La1.7Th0．3CuO4对NO、CO及CO＋NO等小分子的吸附性能和活化规律。结果表明：NO吸附量的大小与催化剂中氧空位含量有关，吸附强度和脱附峰种类与金属离子氧化态有关。CO在氧缺陷复合氧化物催化剂上的吸附是首先变为碳酸根，并在高温以CO2物种脱出．在NO和CO的共吸附过程中，有关NO的吸、脱性能与单独NO－TPD中NO的吸脱附规律相似，表明NO在NO＋CO共吸附的竞争吸附过程中，优先吸附起决定作用，而受CO的影响较小．NO的吸附是NO活化分解的必要条件.

稀土催化合成反式、环化和顺反立构嵌段聚异戊二烯

采用新型稀土催化体系Ｌ＿３－ｎＬｎＸ＿ｎ－Ｒ＿３Ａｌ－Ｒ｀Ｘ，研究了催化体系各组分、室温下再陈化时间、ＲＸ和Ｒ＿３Ａｌ种类及用量、溶剂种类等因素对异戊二烯聚合的影响。在此基础上，经环化聚合合成出环化聚异戊二烯，并尝试了异戊二烯的立构嵌段聚合，用ＩＲ、ＮＭＲ及动态力学测试等方法表征了聚合物的结构。合成出含１，４－结构６８．２％含环化结构约２８．９％，顺－１，４和反－１，４链段的Ｔｇ分别为－２９℃和７０℃的顺反立构嵌段聚异戊二烯。

活性炭的表面化学性质及对CuO/C催化剂上NO还原性能的影响

活性炭是一种十重要的吸附剂和催化剂载体.它属于微晶结构,主要在低衍射角处产生一个比较大的弥散峰,因而人们尚不能够获得关于活性炭的清晰的空间结构特征.一般认为,活性炭的含氧量是影响其化学性质的一个重要因素.而含氧量和含氧基团分布与活化方式有关.遗憾的是,也还不能通过活化方式控制含氧量和含氧基团分布.目前,关于这些基团的组成和分布在催化剂制备的某些关键步骤中和催化反应中的行为都还知道得很少.本工作选取了4种市售国产活性炭:椰壳炭、山楂核炭、山桃核炭和煤质炭.实验表明,当活性炭本身做催化剂时,含氧基团起到了活性中心作用;在制备负载催化剂的浸渍阶段,含氧基团起着成核中心作用,含氧基团的分布可以影响金属离子的分散度.1 实验部分1.l 反应性能评价以等体积浸渍法制备担载量6.25%质量分数硝酸铜/活性炭催化剂.首先室温下真空干燥24h,然后烘箱中65℃下烘4h,再120℃下烘6℃.性能评价在连续流动微型反应装置上进行.石英反应管内径8mm,催化剂用量500mg(20～35目).反应前催化剂在He气中200℃下处理0.5h,然后350℃下热分解1h.反应气NO浓度1.5%摩尔分数(配在He气中),F/W=50mL/...

MAK—04型粘弹分析仪温控系统的改进

对MAK-04型粘弹分析仪的温控系统作了改进,将其温度控制范围从-70～+180℃扩展到-200～+450℃,远远超出同类型仪器-100～+350℃的技术指标。改进后的仪器已用于多样品测试,均获得满意结果。

SPIN AND VALENCE STATE EQUILIBRIA OF COBALT AND MAGNETIC-PROPERTIES OF LACOO3

On the basis of the spin and valence state equilibria and superexchange interaction of the various cobalt ions in LaCoO3, an approximate semiempirical formula has been proposed and used to calculate magnetic susceptibilities of LaCoO3 over a wide temperature range (100-1200 K). The results indicate that there are thermodynamic equilibria between the low spin state Co(III) (t2g6e(g)0) ion, the high spin state Co3+ (t2g4e(g)2) ion, the Co(II) (t2g6e(g)1) ion and the Co(IV) (t2g5e(g)0) ion in LaCoO3. The energy difference between the low spin state Co(III) and the high spin state Co3+ is about 0.006 eV. The content of the low spin state Co(III) ion is predominant in LaCoO3 and the content of the high spin state Co3+ ion varies with temperature, reaching a maximum at about 350 K, then decreasing gradually with increasing temperature. At low temperature the contents of the Co(II) ion and the Co(IV) ion in LaCoO3 are negligible, while above 200 K the contents of both the Co(II) ion and the Co(IV) ion increase with increasing temperature; however, the content of the Co(II) ion always is larger than that of the Co(IV) ion at any temperature. These calculated results are in good agreement with experimental results of the Mossbauer effect, magnetic susceptibility and electrical conductivity of LaCoO3.

PEK-C/PPS共混体系的相容性和结晶行为

结晶-非晶高聚物共混体系的相容性和结晶行为的研究已有许多报道。本工作研究了含酞侧基聚芳醚酮(PEK-C)与聚苯硫醚(PPS)共混物的相容性和结晶行为。 PEK-C为徐州工程塑料厂产品,未作封端处理,η?p/c=0.70;PPS为日本东丽产品。两者用双螺杆挤出机在320～350℃制成共混物。仪器为Perkin-Elmer DSC-7型差示扫描量热仪,升温速率10℃/min;DDV-Ⅱ-EA型全自动动态粘弹谱仪和理学D/max-ⅡBX-射线衍射仪。

酞侧基聚芳醚砜和聚芳醚酮的相容性

本文报道注射级酞侧基聚芳醚砜(PES-C)和聚芳醚酮(PEK-C)共混试样的玻璃化转变行为和部分力学性能的研究结果。并讨论共混工艺对相容性的影响。 PES-C和PEK-C树脂均由中国科学院长春应用化学研究所徐州工程塑料厂合成,在三氯甲烷中的比浓粘度ηsp/c(20℃)分别为0.45和0.47。将粉状树脂在GH-100Q高速搅拌器内按配方混合,并在烘箱内干燥后,用SHJ-30双螺杆挤出机在320～350℃(物料温度)挤出造粒。

Bi系中2212相的超导电性研究

已知在Bi系高Tc超导体中存在三个超导相:2223相的Tc～110k,c～37(?);2212相的Tc～85k,c～30.6(?);2201相的Tc～10k。在实验过程中,我们注意到还可能有另外的超导相存在,通过改变元素名义配比和制备工艺观察到一个具有2212相结构,但Tc却表现为～105k的新现象存在。 实验部分 样品制备采用固相反应方法将Bi_2O_3、PbO、Sb_2O_3、SrCO_3、CaCO_3、CuO(均为A.R.级)混匀、碾磨,于～810℃在刚玉坩埚中预烧20h;再碾,压片后于～870℃在磁舟中烧结60-240h,然后作测试分析。