盖布瑞尔合成法制备N-(2-羟乙基)-邻苯二甲酰亚胺

报道了通过盖布瑞尔合成法制备N (2 羟乙基) 邻苯二甲酰亚胺。以DMF为溶剂,邻苯二甲酰亚胺钾盐与氯乙醇在90℃下反应12h,N (2 羟乙基) 邻苯二甲酰亚胺的收率为86%。讨论了反应温度、反应时间、物料比例以及不同溶剂对反应收率的影响。该方法操作简便,实验条件温和,后处理简便,适合N (2 羟乙基) 邻苯二甲酰亚胺的实验室制备。     

N-(2-溴乙基)-邻苯二甲酰亚胺的合成研究

西他沙星是一广谱喹诺酮类抗菌药,N-(2-溴乙基)-邻苯二甲酰亚胺是其重要的中间体,以自制N-(2-羟乙基)-邻苯二甲酰亚胺和氢溴酸为原料,硫酸为脱水剂合成研究,探讨了原料配比、反应温度、反应时间等反应条件,结果表明合成的最佳条件为原料N-(2-羟乙基)-邻苯二甲酰亚胺与HBr的投料比为2∶9,HBr与浓硫酸的用量比为27∶10,反应温度72℃,反应时间12 h,反应收率可达82%,产品经红外图谱和质谱分析,结果证明产品为目标产物。     

一种新型热致性液晶聚酯酰亚胺的合成与表征

在Higashi直接缩聚法的基础上,利用分步投料法,以N,N-己二撑-1,6-双苯偏三酸酰亚胺二胺(IA6)、对羟基苯甲酸(PHB)和对苯二酚二对羟基苯甲酸酯(PHQ)为主要原料,合成了一种新型三元共聚液晶聚酯酰亚胺(IA6PP)。采用FTIR、DSC、TGA、POM和WAXD等方法研究了单体种类对所合成的聚合物结构和性能的影响。结果表明:IA6PP呈现出典型的向列型液晶的特征,液晶温度区间为252~365℃,热稳定性明显高于由4,4-二羟基二苯甲酮(DHBP)、IA6和PHB合成的液晶聚酯酰亚胺(IA6PD)。     

一种简便的松果腺素的合成方法

以邻苯二甲酰亚胺钾、１,３二溴丙烷、对甲氧基苯胺为主要原料,经５步化学反应合成了松果腺素：邻苯二甲酰亚胺钾和１,３－二溴丙烷在１５５～１６０℃下反应６ｈ,得到Ｎ－（３－溴丙基）,邻苯二甲酸亚胺（Ⅱ）,产率７７％;Ⅱ在乙醇钠存在下和乙酰乙酸乙酯作用得到２－乙酸基－５－邻苯二甲酰亚氨基戊酸乙酯（Ⅲ）,产率７２％;Ⅲ与对甲氧基苯胺重氮盐偶联后发生环化作用,生成Ｔ２－羧乙基－３－（２－邻苯二甲酰亚氨乙基）－５－甲氧基吲哚（Ⅳ）,产率７４％;Ⅳ经碱皂化、水解、脱羧反萃取纯化,得到５．甲氧基色胺（Ｖ）,产率６６％;Ｖ经乙酸化后得到松果腺素（Ⅵ）,产率８２％。     

N-(2-氯乙基)邻苯二甲酰亚胺的合成条件研究

采用盖布瑞尔合成法合成N-(2-氯乙基)邻苯二甲酰亚胺。以N,N-二甲基甲酰胺(DMF)为溶剂,四丁基溴化铵为催化剂,邻苯二甲酰亚胺钾盐与二氯乙烷在70℃下反应2 h,收率为87.3%。     

1,8-萘酰亚胺类荧光剂的合成

采用苊的氧化-卤化法,以4-溴-1,8-萘酐和乙醇胺为原料,经过亚胺化合成4-溴-N-羟乙基-1,8-萘酰亚胺,再进行取代反应,最终合成4-羟乙基胺-N-羟乙基-1,8-萘酰亚胺,通过单因素实验确定了反应的最佳条件,对合成的化合物进行了荧光光谱测定,比较了4-溴-1,8-萘酐和4-羟乙基胺-N-羟乙基-1,8-萘酰亚胺的激发光谱和发射光谱。结果表明,所合成的4-羟乙基胺-N-羟乙基-1,8-萘酰亚胺具有较好的荧光特性,可用作荧光指示剂。     

N-乙基-N',N'-二甲基-N-苯基乙二胺的合成研究

介绍了N－乙基－N‘,N‘-二甲基－N－苯基乙二胺的合成方法,确定了以N－乙基－N－氯乙基苯胺和二甲胺水溶液为原料合成N－乙基－N‘,N‘-二甲基－N－苯基乙二胺的工艺条件,得到收率97％、纯度98％以上的产品。     

结晶聚酯型墨粉主体树脂的合成与性能研究

合成了一种软化点范围适合作墨粉的结晶聚酯,该聚酯以反丁烯二酸和羟乙基双酚A为原料采用熔融缩聚的方法制备而成;探讨了单体羟乙基双酚A的合成方法并研究了反应物物质的量比和催化剂对合成羟乙基双酚A的影响;考查了反应物物质的量比以及反应温度对结晶聚酯合成的影响,对其流变性和软化点作了测试并与商用墨粉用树脂进行比较。     

荧光黄颜料的合成

本文以苊为原料经硝化、氧化、缩合、还原等工序合成了４－氨基－Ｎ－间甲苯基－１,８－萘二甲酰亚胺和４－氨基－Ｎ－邻甲苯基－１,８－萘二甲酰亚胺两种荧光黄颜色的荧光体,并对影响合成反应的诸因素进行了讨论。制得的两种化合物经光谱测定,证明有很好的荧光性能。     

4，4＇－二氨基二苯醚的合成

４，４＇－二氨基二苯醚的合成赵继全，贾志祥，任连生（河北工学院化工系，天津３００１３０）４，４＇－Ｍ氨基二苯醚是生产耐热性塑料聚酰亚胶树脂、聚马来酰亚胺树脂、聚酰胺－酰亚胶树脂、聚酯－酰亚胺树脂等的原料。还用于耐热性环氧树脂高分子化合物的交联剂。这些...     

Synthesis of a novel polyesterimide

A new polyesterimide has been synthesized from trimellitic acid anhydride, diaminodiphenylsulfone, and bisphenol-A following three different routes. Solubility behavior in different solvents, solution viscosity, density, crystallinity, and thermal and electrical properties of the polyesterimide have been discussed. Results indicate that the polyesterimide thus prepared has medium thermal stability.     

Synthesis and properties of polyesterimides and their isomers

A new type of polyesterimide has been synthesized by polycondensation of a dicarboxylic acid containing an internal imide group with ethylene glycol. The dicarboxylic acid was synthesized by reacting aminobenzoic acid with trimellitic acid anhydride in N, N-dimethylformamide solution. Three isomeric (ortho, meta, and para) polyesterimides were prepared from the respective isomer of the dicarboxylic acid. The solubility characteristics, solubility parameters, solution viscosity behavior, density, crystallinity, and thermal properties of these three isomeric polyesterimides were discussed. Some generalizations about structure–property relationship in polyesterimides were also made. It was found that while the ortho and meta isomers of the polyesterimide are amorphous, the para isomer tends to be somewhat crystalline and consequently less soluble, even in polar solvents. The thermal behavior of the meta isomer resembles closely that of the para isomer. The thermal stability of these isomers follows the order para ≥ meta > ortho.     

Investigation in thermal endurance of polyesterimide used in electrical machines

The purpose of this investigation is to evaluate thermal lifetime of polyesterimide using Weibull statistics. Thermal aging was performed on twisted pair specimens of copper wire insulated by a polyesterimide layer. The study shows that breakdown voltage varies versus aging time. Its increase is allotted to a crosslinking inducing a diminution of mean‐free path of charge carriers leading thereby to a mobility decrease, whereas its decrease is attributed to the viscosity diminution expressing a weakening of molecular bonds and a mobility increase of charge carriers. Shape parameter changes in function of aging time. Its increase is ascribed to an arrangement of the molecular structure, whereas its decrease is due to an augmentation in the size of defects. The thermal endurance graph is a straight line indicating that the degradation is governed by a first‐order chemical reaction. Activation energy and temperature index were determined. The degradation is governed by the dissolution of copper into the polymer and accelerates its degradation occurring at the polyesterimide–copper interface. Oxygen can diffuse into the insulation and attack copper resulting in the formation of copper oxide. The degradation is caused by the scission of imide and ester bonds. The process is followed by a change in color and a presence of cracks. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Thermal transition behaviors in a liquid crystalline polyesterimide

The crystallization and melting behaviors of the polyesterimide, derived from N,N′-hexane-1,6-diylbis(trimellitimides), 4,4′-dihydroxybenzophenone and p-hydroxybenzoic acid, were investigated by using polarized light microscopy (PLM), differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD). The nematic texture of the polyesterimide was observed on raising temperature to 265 °C, and the nematic phase was found to convert to isotropic melt beginning from about 300 °C, the ordered nematic micro-domains still surviving after 320 °C. Isothermal crystallization of the samples was performed at 180 °C after heating samples at various temperatures in the range of 265-360 °C, and a completed crystallization peak can appear on DSC curves up to the heating temperature of 360 °C in the presence of the nematic phase and the ordered nematic micro-domains. Non-isothermal crystallization of the samples at different cooling rate was carried out, and the melting of the resulting crystals exhibits double endotherms. It is indicated that a fast crystallization in the nematic phase forms relatively more ordered crystals, which melt at higher temperature, and a slow crystallization in the isotropic phase or in the biphasic melt produces poor crystals, which melt at lower temperature. The crystallized polyesterimide was annealed, which has a minor effect on the high-melting peak but leads to a continual shifting of the low-melting peak to higher temperature with increasing annealing temperature or annealing time. WAXD patterns indicated that the structural transform was not found during annealing process.     

N-(carboxymethyl) trimellitimide–based polyesterimides as film formers for air-drying protective coatings

N-(carboxymethyl) trimellitimide, the imidodicarboxylic acid, was prepared by the reaction between trimellitic anhydride and glycine. This was subsequently condensed in N-methyl-2-pyrrolidone with the alcoholysis products obtained from linseed oil and glycerine to get different oil length polyesterimide resins. The drying characteristics of the resins and the physicochemical properties of the clear and the iron oxide pigmented coatings were evaluated. The results indicate that these materials form a promising class of film—formers for coatings of good durability and protective properties.     

Tribological properties of polyesterimide and its composites

Polyesterimide (PEI) and phenol formaldehyde (PF) samples were synthesized, and composites of the two polymers, as well as composites with carbon, were prepared. Using a pinon-disc machine, the friction and wear properties of the following samples were studied in the load range of two to eight bars:

• Phenolformaldehyde vs. steel
• Phenol formaldehyde cured with hexamethylenetetramine vs. steel
• Polyesterimide vs steel
• Polyesterimide and carbon composite vs steel
• Phenol formaldehyde vs polyesterimide
• Phenol formaldehyde and polyesterimide composite vs. phenol formaldehyde
• Phenol formaldehyde and polyesterimide composite vs. steel.

The data obtained from these experiments were compared with literature data on poly(tetrafluoroethylene) and nylon, conventionally used for tribological applications. It is seen that, in terms of thermal stability, friction, and wear, PEI and PF are promising for tribological applications.     

Weibull statistics in electrical aging of polyesterimide under AC voltage

This article is aimed at the investigation of electrical aging of polyesterimide under AC voltage using Weibull statistical analysis. It's shown that the time to breakdown characteristic (V–t) of polyesterimide includes two zones (segments of straight line). The first zone characterizes a statistical dispersion of the intrinsic defects of material. The second zone expresses the real aging of polymer. The variation of the slope of lifetime curve is attributed to the change in the degradation mechanism. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Thermal decomposition kinetics of thermotropic liquid crystalline polyesterimides

We investigated the thermal decomposition behavior of three groups of polyesterimides that had been synthesized from different compositions of monomers that were added in different. We characterized these polymers with thermogravimetric analysis (TGA) and calculated the apparent activation energy (E_a) associated with the thermal decomposition process by the Ozawa method. The results showed that the E_a of the polyesterimides was correlated with the length of the methylene spacer and the content of the 4,4′‐dihydroxybenzophenone monomer. The polyesterimide with four methylene spacers in the main chain had a higher E_a than that with six methylene spacers. The polyesterimide with a higher 4,4′‐dihydroxybenzophenone content provided better thermal stability. The E_a of the polyesterimides also depended on the sequence in which the monomers were added during the copolycondensation process. The E_a of these polyesterimides followed the order: p‐hydroxybenzoic acid added first > p‐hydroxybenzoic acid mixed 4,4′‐dihydroxybenzophenone adding > 4,4′‐dihydroxybenzophenone added first. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 2467–2472, 2005     

聚酯酰亚胺及其应用

本文介绍了聚酯酰亚胺树脂的基本合成方法。重点介绍了其在柔性印刷电路领域的应用。以及在液晶显示、新型绝缘电线涂料、太阳能电池与感光树脂中的应用。阐明为了适应高速发展的现代经济与科技发展的需要,信息记录材料与现代影像技术领域应加速对上游产品中相关基础材料与技术的研发与应用。     

超支化聚酯改性聚酯亚胺不饱和树脂

合成了一种带柔性链的芳醚型聚酯亚胺不饱和树脂(AEPUR),采用红外光谱技术对其结构进行了表征。研究了端羧基超支化聚酯(HTM-4)对AEPUR/环氧树脂E-44共混体系的弯曲性能、冲击性能和热性能的影响。结果表明,HTM-4能显著提高AEPUR/E44共混物的冲击强度和弯曲性能,表现出明显的增韧/增强作用,体系的热分解温度变化不大,残碳率明显增加。