含苯并恶嗪单元的双邻苯二甲腈树脂的粘接性能

采用含苯并恶嗪单元的双邻苯二甲腈树脂(BZ-BPH)粘接经过处理表面为新鲜铝合金层及氧化物的铝合金基片,对粘接样的室温及高温热处理后(400℃,30 min)的拉伸性能进行了测试并采用SEM观察了断面的形貌。以上述表面不同的2种铝合金粉体为模型,采用差热扫描(DSC)研究了不同界面对BZ-BPH固化反应的影响。研究结果表明,表面为氧化物的试片室温力学性能远大于表面为铝合金的试片;经过高温热处理后,后者的拉伸剪切强度有较大提高,而前者稍有降低,这表明BZ-BPH具有较好的高温粘接性能。     

含苯并恶嗪及联苯结构双邻苯二甲腈共聚树脂

将联苯结构的双邻苯二甲腈树脂(4,4'-二-3,4-二腈基苯氧基联苯,简称BPH)熔融后与含有苯并恶嗪单元的双邻苯二甲腈树脂(简称BZ-BPH)共混。通过示差扫描量热法(DSC)、流变测试研究了共混树脂的固化工艺性能,通过热重分析(TGA)研究了共混树脂固化物的耐热性能。此外采用SEM观察了浇注样的断面结构。结果表明,通过调节BZ-BPH的加入量可实现对固化工艺的调控。经过240℃/4 h+280℃/4 h+320℃/4 h+375℃/6 h的固化,产物在空气和氮气下5%热失重温度均高于500℃(高于BPH固化物)。BZ-BPH与BPH之间共聚形成了均相的交联网络。     

含苯并噁嗪单元的双邻苯二甲腈树脂及其复合材料的研究

利用4,4'-联苯二酚、4-氨基苯氧基-邻苯二甲腈及多聚甲醛采用熔融法制备了一种含有苯并噁嗪单元的新型双邻苯二甲腈树脂单体(BZ-BPH),1H NMR、13C NMR及DSC的分析结果证实了所合成单体的结构.采用溶液浸渍法制备了玻璃纤维布预浸料,热压方式制备了玻纤增强BZ-BPH树脂复合材料,测试了复合材料的力学性能,吸水率;利用TGA及DMA分析了材料的热性能;同时采用SEM对复合材料的断面进行了表征.结果表明,该复合材料具有优良的热稳定性,在氮气和空气中的5%分解温度分别是,400℃处理30 min后弯曲强度的保持率为97%,沸水中处理24 h的吸水率为1.4%.     

苯并恶嗪树脂的合成及其改性的研究进展

综述了近年来国内外在苯并恶嗪树脂基础研究与应用领域内的最新进展情况;介绍了苯并恶嗪树脂的合成及其改性方法,并对苯并恶嗪树脂的发展趋势进行了展望.     

含氟双氨基邻苯二甲腈树脂合成及性能研究

采用2,2-双（3-氨基-4-羟基苯基）六氟丙烷和4-硝基邻苯二甲腈为原料,通过亲核取代反应制备了一种含氟元素的双氨基邻苯二甲腈树脂（FPN-p）。通过傅里叶红外光谱（FT-IR）和核磁氢谱（1H-NMR）对其化学结构进行表征,通过差示扫描量热法（DSC）和FT-IR考察了树脂的固化行为,并研究了树脂的热稳定性、热机械性能以及耐湿热性能。研究结果表明：FPN-p树脂在不加促进剂的情况下可实现自催化聚合,产物结构以三嗪环和酞菁环为主;树脂的玻璃化转变温度和质量分数5%热分解温度均超过400℃,耐温等级较高;树脂的耐湿热性能良好,高温水煮168 h后吸水率小于1%。该树脂有望用于耐高温涂层、树脂基复合材料以及高性能胶粘剂等领域。     

取代基对苯并恶嗪树脂合成及性能的影响

苯并恶嗪树脂具有灵活的分子结构设计性,可采用不同原料合成各种特定结构的苯并恶嗪以满足不同应用的性能要求。文中分别对酚、胺、醛上的取代基对苯并恶嗪的合成反应、聚合反应和固化物结构与性能的影响进行了综述,以期为苯并恶嗪树脂的分子结构设计提供参考。     

苯并恶嗪二苯醚树脂耐热胶粘剂的研究

合成了苯并恶嗪改性二苯醚树脂耐热胶粘剂（DPO-H）。研究了合成条件,胶粘剂的耐热性能和粘接金属铝板的性能。结果表明：该胶粘剂质量损失5%的温度为399℃,粘接金属铝板的剪切强度28.5MPa。     

微波固相法合成苯并恶嗪及其共混树脂的性能

邻位二烷基取代苯胺与苯酚和多聚甲醛经100 W微波辐照20 min反应得到了5种苯并恶嗪单体,将其中邻位为甲基和乙基取代的苯胺型苯并恶嗪与双酚A型苯并恶嗪(BAF)共混,采用红外光谱(FT-IR)、核磁共振氢谱(1H-NMR)、示差扫描量热仪(DSC)、动态机械分析(DMA)、热失重分析仪(TGA)、粘度仪和介电阻抗仪研究了共混树脂的粘温性、热性能及介电性能。结果表明,邻二甲基苯胺型苯并恶嗪(2m6m-BZ)与BAF以物质的量比3∶7共混的体系100～250℃下粘度<500 mPa.s,其固化后热性能接近固化后的纯BAF树脂,且介电常数<3.9,介电损耗低于0.003 5,优于其它共混树脂。     

苯并恶嗪树脂固化收缩行为及热稳定性能研究

对熔融法合成的苯并恶嗪树脂的固化收缩行为及热稳定性能进行了研究。结果表明,苯并恶嗪树脂固化时体积几乎不收缩,甚至略有膨胀,而且具有较高的热稳定性,是一类很有发展前途的新型耐热树脂。     

Polymeric prodrugs containing neridronate and ferrocene: Synthesis,characterization, and antimalarial activity

Polyamidoamine prodrugs containing ferrocene derivatives and neridronate were successfully synthesized and characterized by NMR, FTIR, SEM, and EDX analyses. Appearance of characteristic peaks in ¹H and ³¹P NMR or EDX spectra were used to confirm the presence of neridronate or ferrocene in the conjugates and co-conjugates. In vitro evaluation of the new materials revealed improved antimalarial activity, especially for conjugate 5 and corresponding co-conjugate 8, when compared with chloroquine and quinine. Hemolysis studies revealed that synthesized prodrugs had no effect on the integrity of the host red blood cell membrane; a direct effect on the intra-erythrocytic parasite was, however, noted.     

Synthesis,characterization, and properties of a novel epoxy resin containing both binaphthyl and biphenyl moieties

A new epoxy resin containing both binaphthyl and biphenyl moieties in the skeleton (BLBPE) was synthesized and confirmed by electrospray ionization mass spectroscopy, ¹H‐nuclear magnetic resonance spectroscopy, and infrared spectroscopy. To evaluate the combined influence of two moieties, one epoxy resin containing binaphthyl moiety and another containing biphenyl moiety were also synthesized, and a commercial biphenyl‐type epoxy resin (CER3000L) was introduced. Thermal properties of their cured polymers with phenol p‐xylene resins were characterized by differential scanning calorimetry, dynamic mechanical, and thermogravimetric analyses. The cured polymer obtained from BLBPE showed remarkably higher glass transition temperature and lower moisture absorption, as well as comprehensively excellent thermal stability. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Synthesis and characterization of liquid crystalline polymers containing aromatic ester mesogen and a nonmesogenic ferrocene unit in the spacer

A new series of liquid crystalline polymers containing aromatic triad ester mesogen and 1,1′‐disubstituted ferrocene as a nonmesogenic unit along with polymethylene spacer was synthesized. The polymer was synthesized by a room temperature polycondensation reaction between bis(4‐chloroformyl phenyloxy alkyl ferrocene dicarboxylate) and quinol. The alkyl groups have been varied by an even number of methylene groups with a range from two to ten groups. All the polymers were found to possess liquid crystalline properties. The identification of the mesophase is more transparent with an increase in the spacer. The thermal characteristics were studied using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The results reveal that the thermal stability of the polymers was decreased with increasing spacer length. The T_g, T_m, and T_i of the polymers decreased with increasing methylene groups. The incorporation of the ferrocene moiety also has a considerable effect on the glass transition temperature. The char yield of the polymer decreases with an increasing methylene chain length. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 3494–3501, 2002     

二茂铁甲酸封端不饱和聚酯的固化及热性能研究

以乙二醇、反丁烯二酸为原料合成的不饱和聚酯作为主链,二茂铁甲酸(FCA)作为封端剂,合成了含二茂铁基的不饱和聚酯(RFc),采用红外光谱对产物结构进行了表征。采用DSC及TGA研究了不同二茂铁甲酸含量对不饱和聚酯树脂固化性能和热稳定性的影响。结果表明,随着二茂铁甲酸含量的增加,RFc树脂固化反应活性减弱,热稳定性下降。其最高放热峰温度在171～173℃,且具有比较宽的加工温度范围(152～195℃),符合模塑料固化工艺要求。树脂的耐热性较好,初始热分解温度约为340℃,N2气氛下600℃残炭率可达19.76%。     

乙酰二茂铁谷氨酸Schiff碱的合成

由乙酰二茂铁和谷氨酸合成乙酰二茂铁谷氨酸Schiff碱,优化了反应条件。实验结果表明,当原料物质的量比为1∶1.5、反应温度为50℃、反应时间为7h、pH值为7～8时,产品收率最高。     

Synthesis and electrochemical properties of redox active polyurethanes with ferrocene units in polyether soft segments

Electrochemical active segmented polyurethane with ferrocene units in polyether soft segments (PU‐S‐Fc) has been originally synthesized and identified by ¹H‐NMR spectra. Electrochemical behaviors of PU‐S‐Fc blending with lithium perchlorates were investigated by cyclic voltammetry. In N,N′‐dimethyl formide solution, PU‐S‐Fc exhibited normal cathodic and anodic peaks of the ferrocene/ferricinium (Fc/Fc⁺) couple. Compared with that of ferrocene molecules blended in ordinary polyurethane (PU‐B‐Fc), redox peaks of ferrocene units in PU‐S‐Fc were found to be broader, which may be ascribed to the weak adsorption of the polyurethane on the electrode surface. The influence of lithium perchlorate concentration on peak potentials indicated that supporting electrolytes played an important role in electrochemical redox of PU‐S‐Fc. In the solid state, PU‐S‐Fc/Li⁺ showed discernible redox peaks at temperatures higher than 60°C, and an exponential increase curve of electrochemical response with an increase of temperature was found. Temperature variations of the solid‐state ionic conductivity for PU‐S‐Fc/Li⁺ can be interpreted by the Arrhenius equation. The similarity between the temperature dependence of ionic conductivity and electrochemical response revealed that transport mechanism of ionic and redox species in the polyurethane matrix was controlled by the mobility of polyether chains. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 74: 2674–2680, 1999     

新型含硼苯并噁嗪的合成及其与环氧树脂共混热性能

以乙醇胺、硼酸为原料合成硼酸乙醇胺酯（BAE）,再用所得硼酸乙醇胺酯与多聚甲醛、苯酚反应,合成含硼苯并噁嗪（BAE-BOZ）。将所得BAE-BOZ高温固化,BAE-BOZ和环氧树脂E-51按照不同的质量比进行熔融共混,并经高温固化。采用FT-IR,¹H NMR 和¹³C NMR等分析了BAE-BOZ的化学结构,证明了产物为目标产物;采用DSC对BAE-BOZ的固化特性进行研究;采用TG 分析了含硼乙醇胺型苯并噁嗪poly（BAE-BOZ）和BAE-BOZ/E-51共聚物的热稳定性。结果表明：BAE-BOZ在218℃出现了固化峰;BAE-BOZ的硼含量达到8.67%,在N₂条件下,poly（BAE-BOZ）的热分解温度为302℃,在426℃时热分解速率最快,800℃的残炭率为58.08%,与未经硼改性的乙醇胺型苯并噁嗪（E-BOZ）相比,热分解温度提高40℃,残炭率提高了16.28%;BAE-BOZ/E-51共聚物的热分解温度达到343℃,热性能得到进一步提高。     

二茂铁亚胺酯的抑菌活性研究Ⅰ——1-[1-(2-羟基苯基)乙基]- 二茂铁及其酯的合成、表征与抑菌活性

为了增加乙酰基二茂铁缩邻氨基酚席夫碱的酯溶性，对其进行结构修饰。用乙酰基二茂铁与邻氨基苯酚进行缩合，制得席夫碱（二茂铁亚胺），然后再与酰氯反应，得到二茂铁亚胺羧酯酯。对所得产物结构用元素分析，红外光谱和核磁z共振氨谱进行了表征，化合物的抑菌活性试验表明，二茂铁亚胺及其酯显示了较好的抗病原微生物作用。     

两种含二苯膦基二茂铁酮亚胺席夫碱的合成与表征

以二茂铁、醋酸酐和苯甲酰氯为原料,经过傅克反应和酮胺缩合等反应,合成了标题化合物.讨论了催化剂、溶剂、反应时间和投料计量比对目标产物收率的影响.通过红外光谱、核磁共振氢谱与碳谱、质谱及元素分析对产物的结构进行了表征,并研究了其电化学性质.     

1,1′-二(三氟乙酰基)二茂铁的合成研究

以三氟乙酸酐为酰化剂,无水三氯化铝为催化剂,合成了1,1'-二(三氟乙酰基)二茂铁,其结构经IR,1HNMR,MS和元素分析得到确证。用正交实验设计确定的最佳反应条件为:n(FcH):n((CF3CO)2O)=1:2.2,0℃反应6h。产率78.9%,为该产品的深入研究提供了基础数据。