新型3(4)-噻吩甲氧基邻苯二甲腈的合成

3-硝基邻苯二甲腈或4-硝基邻苯二甲腈分别与噻吩甲醇反应合成了两个新化合物——3-(2-噻吩甲氧基)邻苯二甲腈或4-(2-噻吩甲氧基)邻苯二甲腈,其结构经UV,1H NMR,13C NMR,IR和MS表征.     

耐高温邻苯二甲腈树脂研究进展

邻苯二甲腈树脂是以邻苯二甲腈结构封端的高性能耐高温热固性树脂,具有优异的热氧稳定性、阻燃性、力学强度、低吸水率、低热膨胀系数和介电常数,可用于制备先进复合基体材料、涂料、粘接剂等,在航空技术、电子、机械、军事等领域得到广泛应用.本文综述了邻苯二甲腈树脂结构、邻苯二甲腈单体类型、邻苯二甲腈的固化剂、自催化邻苯二甲腈、生物...     

4-溴-5-硝基邻苯二甲腈的合成及晶体结构

以邻苯二甲酸酐为原料,经溴化、脱水、亚胺化、硝化、酰胺化、脱水6步反应合成了一种易调变的酞菁前驱体——4-溴-5-硝基邻苯二甲腈,并测定了其晶体结构。     

3-硝基邻苯二甲腈的合成

以邻苯二甲酸酐为原料,经过硝化、脱水、亚胺化、氨解、脱水5步反应,高产率地合成了3-硝基邻苯二甲腈,研究了邻苯二甲酸酐的硝化反应、3-硝基邻苯二甲酰胺的脱水条件对产率的影响。目标化合物的结构用元素分析,IR和^1H NMR表征。     

四氟邻苯二甲腈的合成及其晶体结构

四氟邻苯二甲腈是合成氟代酞菁类有机光电子材料及含氟药物的重要中间体。以四氟邻苯二甲酸酐为起始原料,经亚胺化、氨化及脱水3步反应,合成了四氟邻苯二甲腈,总收率41.67%,其结构经FT-IR, MS(ESI)和X-射线单晶衍射确证。     

邻苯二甲腈基联苯酚醛树脂中空微球的制备与性能研究

以苯酚及4,4′-二氯甲基联苯为单体,盐酸作催化剂经Friedel-Crafts烷基化反应,合成了联苯酚醛(BN)树脂,并在此基础上通过BN树脂和4-硝基邻苯二甲腈发生亲核反应合成了邻苯二甲腈基联苯酚醛(PBN)树脂,采用高温发泡法制备了邻苯二甲腈基联苯树脂中空微球.利用红外吸收光谱(FTIR)、核磁氢谱(~1H-NMR)、凝胶渗透色谱(GPC)、热失重(TG)以及扫描电子显微镜(SEM)等对制备的PBN树脂以及PBN中空微球进行了结构与性能表征.研究结果表明,采用自固化和固化剂固化的PBN树脂中空微球均已完全固化,2种固化产物中都形成了异吲哚啉和酞菁环结构,固化剂固化产物中还有三嗪环结构的形成.PBN树脂的自固化产物和固化剂固化产物固化物在1000°C氩气氛围残炭率分别为67%和70%,在600°C空气氛围残炭率分别为70%和47%.PBN树脂中空微球粒径分布范围为350~800μm,数均粒径和体积平均粒径分别为562和583μm,单分散指数为1.04.     

含酰亚胺环酞菁聚合物性能的研究

双邻苯二甲腈单体在催化剂作用下通过熔融聚合得到酞菁聚合物。以IR、DTA、TG等对单体和酞菁聚合物的结构和热性能进行了表征和研究。此外,还进行了单体和聚合物的溶解性试验。结果表明,含酰亚胺环的酞菁聚合物具有优良的热和热氧稳定性,化学惰性和高的成碳率(64.6～65.6％,N_2,>800℃)。这类聚合物可望作为高性能材料应用于宇航等部门。     

含芳基均三嗪环耐高温低聚酰亚胺的合成与性能

通过调控聚合单体的摩尔配比,合成了一系列新型的不同分子链长度的邻苯二甲腈封端含二氮杂萘酮联苯结构低聚酰亚胺,通过FTIR、1H-NMR、WAXD和元素分析对其结构进行表征.以4,4′-二氨基二苯砜为催化剂,低聚物经常压下固化交联后,得到含芳基均三嗪环结构的热固性聚酰亚胺.低聚物表现了良好的溶解性能,可溶于N-甲基-2-...     

双氨基邻苯二甲腈/环氧树脂固化物的制备及性能研究

本文合成出了一种双氨基邻苯二甲腈(DPN)单体,采用红外和核磁共振表征了DPN及其中间体含双氨基的酚类单体(DHTM)的分子结构,利用差示扫描量热证明了DPN的自催化性能及其对环氧树脂(EP)的固化作用。将DHTM与DPN分别与EP制得共混体系,然后将其固化。热失重和动态热机械性能测试表明,DPN-EP固化物的各项性能都要优于DHTM-EP固化物。其在氮气和空气下的初始分解温度(T_(5%))分别提高了27和68℃,计算得到的极限氧指数达到36.36,提高了9.12,其玻璃化温度为202℃,展现出了良好的耐热和阻燃性能。     

四磺酸酞氰锌四钾盐的合成与表征

四磺酸酞氰锌四钾盐的合成与表征;四磺酸酞氰锌四钾盐;磺酸邻苯二甲酸单钾盐;磺酸邻苯二甲腈单钾盐;     

枸杞子糖缀合物LbGp4糖链的结构及其免疫活性的研究

枸杞子糖缀合物LbGp4经β--消除、柱层析分离后得到一条分子量高达180800的分支多糖化合物LbGp4-OL.LbGp4-OL糖基组成为n(Rha):n(Ara):n(Gal)=0.05:1.33:1.根据甲基化、部分酸水解及¹HNMR、¹³CNMR分析,确定了其主要的结构,并对LbGp4和LbGp4-OL的免疫活性进行了研究.     

杯芳烃钕/二正丁基镁/六甲基磷酰胺催化4-乙烯基吡啶的均聚及其与苯乙烯的共聚

聚4-乙烯基吡啶[P（4-VP）]是一种功能高分子,由于在吡啶环上有一个碱性的氮原子,它能进一步与酸反应生成各种盐,与卤代烃生成季铵盐以及与金属离子生成配合物,可用作高分子电解质,高分子试剂,高分子功能材料等,因此有不少文献对它的合成进行了报道,合成聚4-乙烯基吡啶及其与苯乙烯（St）的共聚物,除了用丁基锂作引发剂外,过渡金属的Ziegler-Natta催化剂,以及烷基铝和烷基锌等也常被用作催化剂,但用这些催化剂催化所得的聚4-乙烯基吡啶及其与苯乙烯的共聚物产率低,分子量小。     

聚丙烯酸钠吸收释放氮肥性能

研究了聚丙烯酸钠(PAANa)吸液率及其对氮肥的吸收释放性能。结果表明,尿素对PAANa吸液率没有影响,氯化铵使其吸液率大大降低,且浓度越大吸液率越小;PAANa对不同浓度尿素溶液的吸液率均为370 g/g,对质量浓度为5、10、15和20 g/L氯化铵溶液的吸液率分别为82、62、56和55 g/g。在尿素溶液中,分配系数(mkd)约为1,而在氯化铵溶液中,mkd>1,随着氯化铵浓度增大mkd减小;PAANa对尿素没有富集作用,对NH4 有富集作用;但PAANa对尿素的吸收容量约为NH4 的10倍。PAANa对吸收的尿素和NH4 均具有缓慢释放性能,在水中经4次浸泡(24 h/次),尿素和NH4 累积释放率分别在80%和60%左右;FT-IR分析表明,NH4 与树脂中阳离子发生了离子交换。     

The conjugative metabolism of 4-methylumbelliferone and deconjugation to the parent drug examined by isolated perfused liver and in vitro liver homogenate of rats

We examined the disposition of 4-methylumbelliferone (4-MU) and its conjugative metabolites, glucuronide (4-MUG) and sulfate (4-MUS), using a single-pass rat liver perfusion system. When 4-MU was delivered, the steady-state hepatic extraction ratio for 4-MU was very high (approximately 1.0) and its conjugative metabolites, 4-MUG and 4-MUS, appeared to a large extent in the effluent perfusate. The biliary excretion rate of the 4-MUG conjugated from 4-MU was 44% of the infusion rate at the steady-state, whereas those of 4-MU and 4-MUS were less than 1% of the infusion rate. When 4-MUG was delivered, the steady-state hepatic extraction ratio for 4-MUG was very low (less than 0.05) and the removal rate of 4-MUG from the perfusate was almost identical to the excretion rate of 4-MUG into the bile, while 4-MU and 4-MUS were slightly excreted into the bile (1% of the total biliary excretion rate), suggesting that a little deconjugation of 4-MUG to 4-MU occurred in the liver. Similarly, 4-MU and 4-MUS were not detectable in the effluent perfusate. The apparent extraction ratio (Eapp) for the intracellularly conjugated 4-MUG was approximately twenty times higher than that for the pre-conjugated 4-MUG. This discrepancy between the values of Eapp for the intracellularly conjugated and pre-conjugated 4-MUG might be attributed mainly to the diffusional barrier for the metabolite between the blood and hepatocytes, as suggested in the previous simulation (J. Pharmacokin, Biopharm., 15, 399 (1987].(ABSTRACT TRUNCATED AT 250 WORDS)     

Accurate-mass identification of chlorinated and brominated products of 4-nonylphenol, nonylphenol dimers, and other endocrine disrupters

LC/ToF-MS was used to identify new chlorination and bromination products of 4-nonylphenol (4-NP), such as 4-NPBr2, 4-NPBrCl, 4-NP dimer (2 isomers), 4-NPCl dimer (2 isomers), 4-NPBr dimer, and a series of methoxy bromo and chloro 4-NPs from a laboratory study of nonylphenol chlorination. The identification procedure used the exact mass, exact mass of the isotope cluster, and their relative intensities, at an average mass accuracy of approximately 1 ppm. The products were produced by a simulated study of industrial cleaning procedures where 4-NP, nonylphenol ethoxylate (NPEO-1 and 2), and nonylphenol carboxylate (NPEC-1) were in contact with sodium hypochlorite solutions (with and without bromide) of various strengths (possible environmental scenarios) at neutral pH. The formation of the products was measured as a function of chlorine concentration, and it was found that 4-NP was the most reactive, producing 4-NPCl, 4-NPCl2, 4-NP (dimers), and the 4-NPCl (dimers). In the presence of bromide ions, a mixture results with products of 4-NPBr2, 4-NPCl, 4-NPCl2, 4-NPBrCl, 4-NPBr, and a 4-NPBr dimer. Less reactive to halogenation was NPEO, which formed only the monochloro and monobromo products, and the least reactive was NPEC. A simple stereochemical model is used to explain halogenation reactivity for the family of 4-NPs and NPEOs at neutral pH. The presence of halogenated 4-NP dimers (bromo and chloro diphenyl ethers) is discussed as a possible source of new endocrine disrupters.     

微晶碳电活化过程中离子尺寸效应研究

以石油焦基微晶碳作为电极材料,并由N2吸附,X射线衍射(XRD)表征其孔结构和微晶结构.研究了4种电解液Et4NBF4/PC(四乙基铵四氟硼酸盐/碳酸丙烯酯)、Et4NBF4/AN(四乙基铵四氟硼酸盐/乙腈)、Bu4NBF4/PC(四丁基铵四氟硼酸盐/碳酸丙烯酯)和Bu4NBF4/AN(四丁基铵四氟硼酸盐/乙腈)的微晶碳电容器特性.结果表明:电解质离子与溶剂AN的溶剂化半径较小,容易嵌入类石墨微晶碳层,其于AN的电活化电位比在PC中的低,致使电活化程度更深,材料的表面利用率更高,电容量较大.电解质阳离子(Et4N+,Bu4N+)大小对电活化影响不大.电活化使材料类石墨微晶层间距(d002)变大,离子尺寸越大,层间距增加越明显.     

镁合金化学转化膜的制备及其性能研究

在磷酸钠-磷酸二氢铵-高锰酸钾体系中对镁合金进行化学转化处理.研究了磷酸钠、磷酸二氢铵、高锰酸钾、温度、时间和添加剂对转化膜性能的影响.通过对转化膜结构、成分及性能的测试评价,得到了性能较好的化学转化溶液配方:Na3PO4为5g·L-1,NH4H2PO4为15 g· L-1,KMnO4为1g· L-1,添加剂(NH4)6 Mo7O24为0.5g·L-1.由SEM可观察到转化膜的表面成“干枯河床”状.XRD和EDS检测表明,膜层的主要成分是Mg,Al12 Mg17和无定形相,膜层表面主要有Mn,Mg,K,O和Al等元素组成.腐蚀实验和电化学测试表明,添加剂能够降低转化膜的腐蚀率,转化膜较基体的腐蚀电位正移了0.73 V,提高了镁合金的耐蚀性.     

合成聚对苯二甲酸丙二醇酯负载型催化剂钛酸四丁酯/纳米二氧化硅的制备

以钛酸酯偶联剂(TMC-201)为改性剂,采用超声波分散方法对亲水性纳米二氧化硅(nano-SiO2)进行了表面改性。采用浸渍法将钛酯四丁酯(Ti(OC4H9)4)负载于表面改性的nano-SiO2上,制备了纳米级Ti(OC4H9)4/nano-SiO2负载型催化剂。考察了偶联剂用量、温度、时间对纳米SiO2表面改性的影响,研究了负载时间、负载温度和Ti(OC4H9)4用量对表面改性后纳米SiO2负载Ti(OC4H9)4的影响。结果表明,当TMC-201质量分数为35%、反应温度为90℃、反应时间为3.5 h时,纳米SiO2粒子表面接枝的偶联剂量最大;在室温下,负载48 h,Ti(OC4H9)4用量为表面改性纳米SiO2量的1/2时得到的Ti(OC4H9)4/nano-SiO2负载型催化剂负载Ti(OC4H9)4量最大;运用ICP-AES、FESEM等测试技术对修饰后的纳米SiO2及Ti(OC4H9)4/nano-SiO2负载型催化剂进行了表征;将Ti(OC4H9)4/nano-SiO2负载型催化剂用于聚对苯二甲酸丙二醇酯(PTT)聚酯合成的结果表明,与均相Ti(OC4H9)4催化剂相比,Ti(OC4H9)4/nano-SiO2负载型催化剂催化合成PTT聚酯过程中酯化时间177 min,与均相催化剂催化酯化时间相近,在缩聚2 h后得到PTT的特性粘度高达1.05,证明该负载型催化剂具有高的催化活性,既可催化酯化反应又可催化缩聚反应。     

共沉淀法合成稀土正磷酸盐(La,Gd)PO4:RE3+(RE=Eu,Tb)及其真空紫外光谱特性

采用共沉淀法制备了稀土正磷酸盐荧光粉(La,Gd)PO4:RE3+(RE=Eu,Tb).红外光谱分析发现GdPO4的红外光谱吸收峰与LaPO4一致,只是峰位向高波数方向移动.(La,Gd)PO4:RE3+的真空紫外光谱特性研究表明,Gd3+在能量传递过程中起中间体作用.XPS研究揭示,LaPO4的价带由O2-的2p能级构成,而GdPO4的价带则是由O2-的2p能级和Gd3+的4f能级共同构成.     

Synthesis of 4-Aminosalicylglycine

To search for a better prodrug of 4-aminosalicylic acid that is expected to deliver stably parent drug to colon against the inflammatory bowel disease, a novel 4-aminosalicylic acid derivative was designed and synthesized from 4-aminosalicylic acid. 4-Aminosalicylglycine was prepared from 4-aminosalicylic acid by protecting amino and hydroxyl groups with benzyloxycarbonyl and acetyl, respectively, then the carboxylic acid was converted to acyl chloride which was treated with glycine. After removing the protection groups, 4-aminosalicylglycine wasobtained. All the compounds were characterized by FT-IR, ^1H-NMR, ^13C-NMR spectra. In vivo experiment on rats suggested that the curative effect of 4-aminosalicylglycine was more effective than that of 4-aminosalicylic acid.