马来酸酐扩链端羟基聚丁二烯表征

用马来酸酐在常温条件下对端羟基聚丁二烯进行扩链,通过黏度法测定了扩链前后端羟基聚丁二烯的相对平均分子质量,并用傅立叶变换红外光谱、核磁共振谱对扩链前后端羟基聚丁二烯的结构进行了表征。结果表骐,扩链后相对平均分子质量增大至原来相对平均分子质量的1．46倍,在傅立叶变换红外光谱图上显示出较强的酯基伸缩振动吸收峰（1735cm^-1）,同时也用核磁共振谱排除了乙醇的酯化,这说明端羟基聚丁二烯的扩链不是简单的端羟基转变为端羧基,而是酯化反应。     

几种N-取代苯基马来酰亚胺单体的合成与表征

以马来酸酐、苯胺及其衍生物为主要原料合成了N-对甲苯基马来酰亚胺(NM PM I)、N-对氯苯基马来酰亚胺(NCLPM I)、N-对甲氧苯基马来酰亚胺(NM OPM I),产率可达85%以上。采用1H-NM R,13C-NM R和FT-IR等仪器对产物及中间产物马来酰胺酸的结构进行详细的表征。研究发现马来酰胺酸和马来酰亚胺苯环上不同的取代基,在1H-NM R谱图中,对HC=CH上质子峰的影响不大,而对苯环上质子峰却有影响,吸(供)电子基使苯环质子的化学位移向低(高)场移动;在13C-NM R谱图中,含强电负性(O、N、C l)的取代基使苯环上δc1低场移动,邻对位δc略向高场移动,取代基的电负性越大,位移也越大。     

端烯化合物改性双马来酰亚胺树脂

BMI(DDM型双马来酰亚胺)经VE(环氧丙烯酸酯)改性,两者重量比为1:1时,加适当促进剂,可以在改善BMI成型工艺性同时保持基体优良的耐热性和耐湿/热性能。基体热变形温度285℃。T300增强单向板干态250℃下层剪强度和弯曲强度保持率分别为60％和63％。沸水煮24小时后,室温下层剪和弯曲强度保持率分别为90％和94％,150℃、200℃层剪强度保持率分别为71％和61％。     

双马来酰亚胺树脂扩链增韧改性研究

研究了采用腰果壳油增韧改性双马来酰亚胺树脂的方法，双马来酰树脂虽具有突出的耐热性，良好的机能及加工性能，但其最大不足是固化物脆性大，因此必须引进长链的柔性分子或分合物对双马来酰亚胺树脂加以改性，增加其韧性，改善其机械性性能，扩大其应用邻域，腰果壳油具有柔性长链分子，而且还有不饱和双键，能与双马来酰亚胺树脂的不饱和双键反应，它是一种良好的改性剂，本篇论文探讨了双马来酰亚胺树脂与腰果壳油长链分子反应机理，考察了改性树脂的力学性能和热学性能，对其工艺和配方也作了初步探讨。     

耐高温涂料用新型双马来酰亚胺树脂的合成及性能研究

用烯丙烯酚二苯醚树脂与双马来酰亚胺按不同配比进行预聚合，制得系列韧性双马来酰亚胺预聚树脂，其特点是：预聚树脂稳定，溶解性好，成型加工性优良，熔体粘度小和流动性好，固化物具有聚酰亚胺的耐热性，耐潮湿，耐腐蚀和耐辐射等性能，同时具有优良的电绝缘和机械性能，适宜作耐高温粉末涂料或高固体分涂料。     

含芳酰胺键的液晶双马来酰亚胺的合成与表征

通过对马来酰亚胺基苯甲酸及其酰氯化路线合成了两种含芳酰胺键的液晶双马来酰亚胺Ⅰ b和Ⅱ b;制备了二苯甲烷二胺与液晶双马来酰亚胺Ⅱ b的扩键其聚物Ⅲb。经FTIR、~1H-NMR谱对合成产物的结构进行了表征,表明1710cm~(-1)的酰亚胺羰基和1646cm~(-1)酰胺键,交联反应或扩链反应发生在双马来酰亚胺的双键上。经热分析DTA/DSC及热台偏光显微镜表征了其热性能及液晶相变特征,相变过程是一个非平衡不可逆过程。     

耐205℃的改性双马来酰亚胺树脂

经改性的双马来酰亚胺树脂可在205℃下工作,并具有良好的韧性和成型工艺性。该树脂的研制成功为复合材料向较高使用温度的零件与结构领域推广创造了条件。     

双烯丙基联苯醚/双马来酰亚胺共聚物的制备与液晶行为

本文以联苯二酚为原料,制备了双烯丙基联苯醚与双马来酰亚胺的共聚物。经DSC、WAXD和热台偏光显微镜表征,该共聚物具有较强的热固化性能和液晶特征。经等温固化研究表明,交联密度越大液晶聚合物网络的清亮点越低,而且将近晶型液晶态保留在网络中。这为制备新型的改性双马来酰亚胺另辟新径。     

N-苯基马来酰亚胺的合成与表征

以顺丁烯二酸酐和苯胺为原料,研究在催化剂作用下合成N_苯基马来酰亚胺（N—PMI）的新工艺,在N-苯基马来酰胺酸合成时采用乙酸已酯作溶剂,在N-PMI合成时采用乙二胺四乙酸（EDTA）钠盐作为催化剂、醋酐作为脱水剂、丙酮作为溶剂,考察了原料配比、催化剂的选择及用量、反应温度与反应时间等因素对反应结果的影响,合成N-PMI的最佳工艺条件为：顺酐与苯胺质量比为1．06：1,0,催化剂用量为O．35g／g中间体,反应温度为55℃,反应时间为4h。在最佳工艺下产品收率可达92％以上,产品纯度可达99％（质量分数）以上,并通过气相色谱检测了产品纯度,通过红外光谱对产品结构进行了表征。     

Synthesis and thermal behavior of some brominated bismaleimides and polyaspartimides

Brominated bismaleimides were synthesized by the reaction of brominated bisphenols with 3‐ or 4‐maleimidobenzoyl chloride. The reaction of these maleimides with various aromatic diamines yielded brominated polyaspartimides. The monomers and polymers were characterized by Fourier transformed infrared and proton nuclear magnetic resonance spectroscopy. Thermal behavior of these brominated polyaspartimides was studied and compared with that of related polyaspartimides having other substituents instead of bromine or other bridges in the bisphenolic segment. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Syntheses of bismaleimides with ester units and their polymerization with diamines

Five structurally different bismaleimides were synthesized by reaction between 3(4)‐maleimidobenzylchloride with various diphenols. They were characterized by infrared (IR) and proton nuclear magnetic resonance (¹H‐NMR) spectroscopy. Thermal characterization of monomers and their polymers was accomplished by differential scanning calorimetry (DSC) and dynamic thermogravimetric analysis (TGA). Polyaminobismaleimides having inherent viscosities of 0.1–0.4 dL/g were prepared by Michael addition of diamines to bismaleimides. The polymers are soluble in solvents as DMF, NMP, and DMSO, and afforded film from their solutions. © 2002 John Wiley & Sons, Inc. J Appl Polym Sci 84: 750–757, 2002; DOI 10.1002/app.10294     

Preparation and characterization of metal-containing bismaleimides from divalent metal salts of p-aminobenzoic acid

A series of novel metal-containing bismaleimides monomers BMI(M) (M = Ca, Sr, Ba, Pb, Co, Ni) were prepared by reacting maleic anhydride with diaminodiphenyl carboxylate to form bismaleamic acid precursors, and subsequently by imidizing them chemically or thermally to form bismaleimides. The samples were characterized by IR, ¹H-NMR, and TG-DTA. The results of thermal analysis show that the BMI(M) have high thermo-oxidiative stability and their temperatures of initial decomposition have a relationship with metals introduced and the imidization methods. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 63: 1827–1831, 1997     

二烷基酰亚胺萃取剂的合成与表征

以丙酰氯、正戊酰氯、正庚酰氯为酰化试剂,在温度≤10℃下分别与氨水反应生成丙酰胺、正戊酰胺和正庚酰胺. 以吡啶作缚酸剂,将生成的酰胺与含相同碳链长的酰氯在温度≤0℃下反应,得到3种具有对称结构的含直链烷基的二烷基酰亚胺(二丙酰亚胺、二正戊酰亚胺和二正庚酰亚胺),对终产物进行了表征. 结果表明,以乙醇为良溶剂、水为不良溶剂,经多次重结晶后其最终产率分别为30%, 35%, 33%,终产物的熔点分别为153.7~154.0, 91.5~91.7, 89.0~89.5℃,二烷基酰亚胺纯度大于99%.     

Synthesis and characterization of bisitaconimides. I

This article describes the synthesis and characterization of bisitaconimides on the basis of 4,4′‐diaminodiphenylether, 2,2′‐bis[4‐(4‐aminophenoxy)phenyl]propane, 1,3‐bis(4‐aminophenoxy)benzene, and 1,4‐bis (4‐aminophenoxy)benzene. Isomerization of the itaconimides to citraconimides (varying in the range of 25–40%) was observed during synthesis. The curing exotherm and thermal stability of the cured resins depended on the backbone structure of itaconimides. The curing exotherm immediately followed the melting endotherms. These resins cured at lower temperatures than bismaleimides but thermal stability of cured bismaleimides was higher than bisitaconimides. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 2277–2282, 2002     

Synthesis and characterization of novel chain‐extended bismaleimides containing fluorenyl cardo structure

Novel fluorenyl cardo chain‐extended bismaleimides (FCCEBMIs) were synthesized by reacting maleic anhydride with fluorenyl cardo diamine and different dianhydrides. FCCEBMIs were characterized by FT‐IR spectra (FT‐IR), ¹H NMR, and elemental analysis. All FCCEBMI monomers were readily soluble in a variety of organic solvents, such as N‐methyl‐2‐pyrrolidinone, N,N‐dimethyl acetamide, chloroform (CHCl₃), methylene chloride (CH₂Cl₂), dimethyl sulfoxide, and tetrahydrofuran when compared with 9,9‐bis(4‐maleimidophenyl) fluorene. Curing process was investigated by differential scanning calorimetry. Thermal properties of the cured FCCEBMIs were characterized by thermogravimetry analysis, the cured products are stable up to 430°C. The results show that the FCCEBMIs with imide structure improve significantly the solubility of bismaleimide (BMI) in organic solvents without sacrificing thermal properties of cured BMIs. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Synthesis and characterization of functionalized thermoplastics as reactive modifiers for bismaleimide resins

The preparation and characterization of a series of chemically functionalized oligosulphones (of approximate M _n 5000–17 000 g mol^?1) bearing propenyl groups substituted into the main aromatic backbone is reported. The thermal characterization of the oligomers using differential scanning calorimetry was carried out and the main features of the thermally‐initiated process are presented. Blends of the oligomers were formed with a commercial bismaleimide and their thermal characteristics are also discussed. © 2001 Society of Chemical Industry     

Synthesis and Properties of Novel Poly(amide-imide)s Derived from 2,4-diaminotriphenylamine and Imide Ring-Preformed Dicarboxylic Acids

2,4-diaminotriphenylamine (2) was synthesized via the cesium fluoride-mediated aromatic substitution reaction of 1-fluoro-2,4-dinitrobenzene with diphenylamine, followed by palladium-catalyzed hydrazine reduction. A series of poly(amide-imide)s (PAIs) with inherent viscosities of 0.38–0.46 dL/g were prepared by triphenyl phosphite-activated polycondensation from the diamine monomer 2 with various monoimide- and diimide-dicarboxylic acids. All of the PAIs were readily soluble in a variety of organic solvents and formed strong and tough films via solution casting. These PAIs have moderately high glass transition temperatures in the range of 168–274 ^○C and 10 % weight loss temperatures in excess of 447 ^○C in nitrogen or in air.     

Reduction and cyclization to form poly(benzimidazole amide imide) copolymers

Poly(amide imide) copolymers were synthesized with different molar ratios of 4,4‐diphenylmethane diisocyanate, two types of aromatic dianhydrides (pyromellitic dianhydride (PMDA) and 3,3′,4,4′‐sulfonyl diphthalic anhydride (DSDA)), and a diacid, which was derived from 3,3′‐dinitrobenzidine and isophthaloyl chloride in a previous work. In this study, the copolymers were further reacted with a reducing agent, and the nitro groups in the copolymers were hydrogenated into amine groups. Then, the amine‐group‐containing poly(amide imide) copolymers were cyclized at 180°C to form the poly(benzimidazole imide amide) copolymers in poly(phosphoric acid), which acted as a cyclizing agent. The resultant copolymers were soluble in sulfuric acid and poly(phosphoric acid) at room temperature and in sulfolane or N‐methyl‐2‐pyrrolidone under heating to 100°C with 5% lithium chloride. According to wide‐angle X‐ray diffraction, all the copolymers were amorphous. According to thermal analysis, the glass‐transition temperature ranged from 270 to 322°C, and the 10% weight‐loss temperature ranged from 460 to 541°C in nitrogen and from 441 to 529°C in air. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 91: 378–386, 2004     

Synthesis,polymerization and thermal properties of bio-based benzoxazine resins containing imide or amide functionality

Two novel bio-based benzoxazine monomers containing imide or amide group (HPIDD-fa and HPBA-fa) were synthesized from raw materials of benzoyl chloride/phthalic anhydride, tyramine, furfurylamine and paraformaldehyde via a two-step reaction. Fourier transform infrared spectroscopy (FT-IR), proton and carbon nuclear magnetic resonance (NMR) spectroscopies were performed to characterize the structures of the benzoxazine monomers. The curing behavior was investigated by using differential scanning calorimetry (DSC) and in situ FT-IR, and the DSC results indicate that the peak curing temperatures of HPIDD-fa and HPBA-fa are centered at 248.5 and 230.1°C, respectively. In addition, thermogravimetric analysis (TGA) suggests that the newly developed bio-based benzoxazine-derived polybenzoxazines present excellent thermal stability with T_d10 (temperature at 10% weight loss) of 385 and 368°C for poly(HPIDD-fa) and poly(HPBA-fa), respectively. The current investigation suggests that our newly obtained bio-based thermosetting resins are promising materials for high-tech applications.