Novel Interacting Blends of Unsaturated Polyester-s-Triazine and Epoxy Resin

2-(4-ethyl-1-piperazinylo)-4,6-bismaleatedethylamino-1,3,5-triazine (EBT) was prepared by the reaction of 2-(4-ethyl-1-piperazinylo)-4,6-bishydroxyethylamino-1,3,5-triazine and maleic anhydride. The EBT derivative was characterized by elemental analysis, acid value and spectral studies.

EBT was then polycondensed respectively with three commercial epoxy resins, namely diglycidyl ether of bisphenol-A (DGEBA), diglycidyl ether of bisphenol-F (DGEBF) and diglycidyl ether of bisphenol-C (DGEBC). The resultant polymers are designated as unsaturated polyester-s-triazine (UPETs) and were characterized by elemental analysis, spectral study, molecular weight determination, differential scanning calorimeter (DSC)and thermogravimetry. The interacting blends of UPETs with DGEBA epoxy resin was made at stoichiometric ratio. The blending of these systems was monitored on a differential scanning calorimeter (DSC), and based on DSC data the glass-reinforced composites (GRC_s) were prepared and characterized by physical and mechanical properties.     

The Synthesis and Characterization of Melamine Based and [Fe/CrSalen] or [Fe/CrSalophen] Capped Polimer Schiff Base Complexes

In this study, by using previously reported monomer complexes [(2-(4-carboxybenzimino)-4,6-diamino-1,3,5-triazine)(salen/salophenFeIII)], [(2-(4-carboxybenzimino)-4,6-diamino-1,3,5-triazine)(salen/salophenCrIII)], [(2-(3,4-dihydroxybenzimino)-4,6-diamino-1,3,5-triazine)(salen/salophenFeIII)] and [(2-(3,4-dihydroxybenzimino)-4,6-diamino-1,3,5-triazine)(salen/salophenCrIII)] obtained by Uysal and Uçan (J Inc Phenom Macrocycl Chem, in press), sixteen new polimer Fe(III) and Cr(III) complexes involving tetradentate Schiff bases N,N′-bis (salicylidene)ethylenediamine-(salenH₂) or bis(salicylidene)-o-phenylenediamine-(salophenH₂) with 2-(4-carboxybenzimino)-4,6-diamino-1,3,5-triazine or 2-(3,4-dihydroxybenzimino)-4,6-diamino-1,3,5-triazine (Uysal and Uçan, J Inc Phenom Macrocycl Chem, in press) and terephthaldehyde or glutaraldehyde have been synthesized and characterized by means of elemental analysis, ¹H N.M.R., FT-IR spectrscopy, MS, thermal analyses and magnetic susceptibility measurements. The complexes have also been characterized as low-spin distorted octahedral Fe(III) and Cr(III) bridged by catechol and/or COO^? groups.     

活性酯法合成来氟米特

2-氯-4,6-二甲氧基-1,3,5-三嗪和N-甲基吗啉反应得到氯化4-(4,6-二 甲氧基-1,3,5-三嗪-2-基)-4-甲基吗啉,其与5-甲基异(噁)唑-4-甲酸反应制备2-(5-甲基异(噁)唑-4-甲酰氧基)-4,6-二甲氧基-1,3,5-三嗪,所得化合物与4-三氟甲基苯胺反应合成标题化合物,总收率约72％(以...     

A comparison of some imidazoles in the curing of epoxy resin

An epoxy-imidazole resin system was used to form an anisotropic conducting film (ACF) for electronic equipment applications. In this study, the curing behaviors of an epoxy resin with imidazole, 2-methylimidazole, 2-ethylimidazole, 2-phenylimidazole, 1-methylimidazole, 2-ethyl-4(5)-methylimidazole, and 1-(2-cyanoethyl)-2-ethyl-4(5)-methylimidazole were investigated using differential scanning calorimetry (DSC), and the curing times were determined at 150 and 180 °C. The polymerization mechanism for the epoxy resin with imidazoles was examined, and the DSC results matched the mechanism. 2-Methylimidazole exhibited the fastest reaction time among the imidazoles used in this study.     

2-苯基-4,6-二[2-羟基-4-(甲基哌啶氧基羰基甲氧基)苯基]-1,3,5-三嗪的合成与表征

以三聚氯氰为起始原料,通过格氏反应、Friedel-Craft反应、醚化反应及酯交换反应合成了两个含受阻胺结构的新型三嗪类双功能光稳定剂——2-苯基-4,6-二[2-羟基-4-(2,2,6,6-四甲基哌啶氧基羰基甲氧基)苯基]-1,3,5-三嗪(Ⅳa)及2-苯基-4,6-二[2-羟基-4-(1,2,2,6,6-五甲基哌啶氧基羰基甲氧基)苯基]-1,3,5-三嗪(Ⅳb),收率分别为37.6%和38.1%;用MS、1HNMR和IR确定了目标产物的结构;测试了其紫外吸收性能。结果显示,目标产物在270~400 nm有较强吸收,Ⅳa和Ⅳb最大摩尔吸收系数分别为6.651 3×104L.mol-1.cm-1(276nm),2.837 4×104L.mol-1.cm-1(339 nm);6.435 9×104L.mol-1.cm-1(276 nm),2.648 3×104L.mol-1.cm-1(339 nm)。     

阴离子瓜尔胶合成新工艺

以对氨基苯磺酸钠、三聚氯氰为原料合成了阴离子瓜尔胶改性剂2-（4-磺基）苯胺基-4，6-二氯-1，3，5-均三嗪，改性剂与瓜尔胶反应制得了阴离子瓜尔胶（AGG），采用IR对改性剂及AGG进行了表征。采用正交实验得出制备AGG的较佳工艺条件，测定了AGG水溶液（质量浓度为1％）的粘度。     

2,4-二(4-联苯基）-6- (2-羟基-4-烷氧基苯基)-1,3,5-均三嗪紫外线吸收剂的合成与性能

以三聚氯氰为原料,通过格氏反应、Friedel-Craft反应合成了2-氯-4,6-二(4-联苯基)-1,3,5-均三嗪(Ⅳ);化合物Ⅳ在碱性条件下与溴代烷反应合成了3种2,4-二(4-联苯基)-6-(2-羟基-4-烷氧基苯基)-1,3,5-均三嗪(Ⅴ1～3)。用FTIR、MS、1HNMR对化合物Ⅴ1～3结构进行了确证,用TGA、UV-Vis对化合物Ⅴ1～3的热稳定性、紫外吸收及光稳定性进行了测定。结果表明,与市售商品化紫外线吸收剂UV-1577相比,化合物Ⅴ1～3的T5(质量损失5%时的温度)提高了40～60℃;具有更宽的吸收范围和更高的最大摩尔吸收系数(εmax)。化合物Ⅴ1～3的εmax分别为:79 448.28 L/(mol.cm)(λmax=318.5 nm),80 873.51 L/(mol.cm)(λmax=319 nm),76 774.7 L/(mol.cm)(λmax=319 nm)。     

三嗪型紫外线吸收剂的合成及性能

用格氏试剂偶联法合成了4个有代表性的三嗪型紫外线吸收剂:2,4-双(2,4-二羟基苯基)-6-(4-甲氧基苯基)-1,3,5-三嗪、2,4-双(2,4-二羟基苯基)-6-苯基-1,3,5-三嗪、2-(2,4-二羟基苯基)-4,6-二苯基-1,3,5-三嗪和2,4,6-三(2,4-二羟基苯基)-1,3,5-三嗪,测定了它们的紫外光谱。其中,2,4-双(2,4-二羟基苯基)-6-(4-甲氧基苯基)-1,3,5-三嗪在UVB和UVA都有较强吸收,εmax=36000L/(mol.cm)(λmax=313nm),εmax=36333L/(mol.cm)(λmax=344nm),是其中最好的紫外线吸收剂。     

固化促进剂对环氧树脂固化物性能的影响

借助透光率/雾度仪、DSC和SEM比较了四乙基溴化铵(TEABr)、二甲基苄胺(DBMA)、2-乙基-4-甲基咪唑(2,4-EMI)、2,4,6-三(二甲基胺基甲基)苯酚(DMP-30)以及有机膦/溴络合物(AO-4)对E-51环氧树脂/酸酐固化体系性能的影响。结果表明,固化促进剂的加入可不同程度地提高环氧树脂的固化速率,改善固化物的透明度和耐热稳定性。AO-4质量分数为0.5%～1.0%,120℃下反应得到的环氧/酸酐固化物无色透明,综合性能最佳。     

Composites of Poly(Keto-Sulfide)–Epoxy Resin Systems and Their Thermal and Mechanical Properties

A novel matrix resin system, poly(keto-sulfide)–epoxy resin, has been developed. The poly(keto-sulfide)s (PKS), based on various ketones, formaldehyde, and sodium hydrogen sulfide (NaSH), were prepared by the reported process. These (PKS) having terminal thiol (–SH) groups were used for curing commercial epoxy resin (i.e., diglycidyl ether of bisphenol A – DGEBA), to fabricate crosslinked epoxy-poly(keto-sulfide) resin glass fiber-reinforced composites (GRC). Various epoxy/hardener (PKS) mixing ratios were used, and the curing of epoxy-PKS has been monitored using differential scanning calorimetry (DSC) in dynamic mode. Based on DSC parameters the GRC of epoxy-PKS were prepared and characterized by thermal and mechanical methods. The variation in resin/hardener ratio led to variations in thermal and mechanical properties.     

不同胺取代三嗪衍生物对高密度聚乙烯阻燃性能的影响

以三聚氯氰、甲胺和二甲胺水溶液为原料,合成了2,4,6-三甲胺基-1,3,5-均三嗪(TMM)和2,4,6-三二甲胺基-1,3,5-均三嗪(HMM),并用FT-IR和DSC对其进行了表征。研究了用多聚磷酸胺(APP)和季戊四醇(PER)作为酸源和炭源,分别用三聚氰胺(MEL)、TMM和HMM作为气源的膨胀型阻燃剂对高密度聚乙烯(HDPE)力学性能和阻燃性能的影响。结果表明:含TMM的HDPE复合材料的阻燃性能和力学性能都优于含MEL或HMM的HDPE复合材料。     

Nonisothermal cocuring behavior and kinetics of epoxy resin/3‐glycidyloxypropyl‐POSS with MeTHPA

3‐Glycidyloxypropyl‐polyhedral oligomeric silsesquioxanes (G‐POSS) was prepared from 3‐glycidyloxypropyl‐trimethoxysilane (GTMS) by hydrolytic condensation. The cocuring behavior and kinetics of G‐POSS with bisphenol‐A epoxy resin (BPAER) using 3‐methyl‐tetrahydrophthalic anhydride (MeTHPA) as curing agent were investigated by nonisothermal differential scanning calorimetry (DSC) and torsional braid analysis (TBA). The face distribution of silicon in the cured products was characterized by energy dispersive X‐ray spectrometry (EDS). The results show that the compatibility of G‐POSS with BPAER is very well and can cocure. The curing mechanism was proposed. The relationship of E_a and conversion α can be obtained by the isoconversional method of Kissinger. These curing reactions can be described by the Šesták–Berggren (S–B) equation and can be depicted by the following equation: . TBA analysis indicated that T_g was decreased when the contents of G‐POSS is over to 30 wt%. POLYM. COMPOS., 2010. © 2009 Society of Plastics Engineers     

Synthesis,characterization, and curing of {2,6–bis‐[2‐(bis‐oxiranylmethyl‐amino)‐methylbenzyl]‐phenyl}‐bis‐oxiranylmethylamine (BPBOMA)

The curing behavior of epoxy resin prepared by reacting epichlorohydrin with amine functional aniline acetaldehyde condensate (AFAAC) was investigated using AFAAC as a curing agent. The epoxy resin, {2,6‐bis‐[2‐(bis‐oxiranylmethyl‐amino)‐methylbenzyl]‐phenyl}‐bis‐oxiranylmethylamine (BPBOMA), was characterized by FTIR and ¹H‐NMR spectroscopy, viscosity measurement, and determination of epoxy content. Analysis of the curing reaction was followed by differential scanning calorimetry (DSC) analysis. To investigate the curing kinetic with AFAAC, dynamic DSC scans were made at heating rates of 5, 10, 15, and 20°C/min. The activation energy and frequency factor of the AFAAC formulation were evaluated. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 3168–3174, 2006     

阴离子瓜尔胶的制备及其稀溶液性质

在碱催化剂作用下,用改性剂2-氨基乙磺酸钠-4,6-二氯-1,3,5-均三嗪与瓜尔胶反应制得新型阴离子瓜尔胶(AGG),采用IR对AGG进行了表征。借助乌氏黏度计研究了AGG的稀溶液性质,考察了温度和外加盐浓度对AGG的影响。结果发现,随着温度的升高,其特性粘度先增大后减小;而其特性粘度则随着NaCl溶液浓度的增加先减小后增大。     

咪唑促进双氰胺固化环氧树脂体系固化动力学

采用差示扫描量热(DSC)法研究了2-乙基-4-甲基咪唑(2E4MI)的含量对双氰胺(DICY)固化环氧树脂体系固化动力学的影响。非等温DSC测试结果表明,2E4MI能大幅度降低DICY固化环氧树脂所需要的温度和活化能,从而加快反应的进行。当2E4MI用量为0.2份时,活化能最低为84.2 kJ/mol且整体活化能随固化度的变化较小、固化更均匀。在2E4MI最佳用量(0.2份)下对固化体系进行等温DSC以及潜伏性测试,结果表明,该体系在160℃下20 min内可完成固化,室温储存15 d的固化度仅为0.146,说明其适合用作快速固化环氧树脂储存体系。     

两种新型三嗪类紫外线吸收剂的合成与表现

以三聚氯氰为原料,通过三步取代反应,合成了新型三嗪类紫外线吸收剂2-(2-羟基-4-丙二酸二乙酯基氧基苯基)-4,6-二苯基-1,3,5-三嗪(Ⅲ)和2-(2-羟基-4-丙二酸二乙酯基氧基苯基)-4,6-二(4,-甲基)苯基-1,3,5-三嗪(Ⅵ)。对他们及紫外线吸收剂UV1577的溶液进行了光老化试验,通过对比发现它们的抗光老化性能均比UV1577好。Ⅲ、Ⅵ两种化合物的总收率均为68%,含量均在98%以上。同时,用质谱(MS)及红外(IR),确定了物的结构,测定了化合物(Ⅲ、Ⅵ)的熔点。     

Isothermal and nonisothermal cure kinetics of an epoxy/poly(oxypropylene)diamine/octadecylammonium modified montmorillonite system

The effect of an octadecylammonium‐exchanged montmorillonite on the curing kinetics of a thermoset system based on a bisphenol A epoxy resin and a poly(oxypropylene)diamine curing agent were studied with differential scanning calorimetry (DSC) in isothermal and dynamic (constant‐heating‐rate) conditions. Montmorillonite and the prepared composites were characterized by X‐ray diffraction analysis and simultaneous DSC and thermogravimetric analysis. The analysis of the DSC data indicated that the intercalated octadecylammonium cations catalyzed the epoxy–amine polymerization. A kinetic model, arising from an autocatalyzed reaction mechanism, was applied to the DSC data. Fairly good agreement between the experimental data and the modeling data was obtained. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 1765–1771, 2006     

Hexahydrotriazine derivative containing imidazole for fast curing,improved mechanical strength,and flame retardancy of epoxy

We synthesized a hexahydrotriazine derivative containing imidazole, 1,3,5-tris[4′-(1H-imidazol-1-yl)-(1,1′-biphenyl)-4-yl]-1,3,5-triazinane (HIM) and adapted it as a co-curing agent for epoxy resin (EP). The curing kinetics of HIM were evaluated using elevated differential scanning calorimetry (DSC) analysis, and the curing speed was determined to be accelerated with HIM. Moreover, when 5 phr of HIM was applied to the epoxy system, the tensile strength of cured EP increased to 50.9 MPa. Because of the high nitrogen content of HIM, when the candidate amount of HIM was increased, the char yield increased. HIM (20 phr) showed a char yield of 36.1%, which is about 74% higher than that of the HIM (0 phr) reference (20.7%). The char layer acts as a barrier between oxygen and polymeric decomposition gases, inducing a high flame-retardant property.     

Synthesis, absorption and fluorescence properties of N-triazinyl derivatives of 2-aminoanthracene

N-(4,6-dichloro-1,3,5-triazin-2-yl)-2-aminoanthracene was synthesized by substitution of one chlorine atom of 2,4,6-trichloro-1,3,5-triazine with 2-aminoanthracene. A new series of N-triazinyl-2-aminoanthracenes was prepared by nucleophilic substitution of one or both chlorine atoms on N-(4,6-dichloro-1,3,5-triazin-2-yl)-2-aminoanthracene with electron-donating methoxy or phenylamino groups. The UV/Vis absorption, fluorescence and excitation spectra as well as the fluorescence quantum yields of the prepared compounds were measured in 1,4-dioxane, ethyl acetate, dibutyl ether and acetonitrile; nanosecond kinetics of the fluorescence decay was measured in different solvents. The influence of the character of the substituent on triazinyl ring and of the solvent polarity upon the absorption and fluorescence spectra and fluorescence quantum yields are discussed.     

Amine-terminated oligoimides for epoxy curing

Oligoimides of N,N′,-4,4′-bismaleimidodiphenyl ether (DDEBM) and 4,4′-diaminodiphenylmethane (DDM) were prepared by the Michael addition reaction. The synthesized oligoimides (DDEBM–DDM) were characterized for their molecular structure by elemental analysis and IR spectroscopy. The number-average molecular weight (M _n) was determined by nonaqueous conductometric titration. Thermal characteristics were studied by thermogravimetry. Use of DDEBM–DDM oligomers as a curing agent for epoxy resin was studied by differential scanning calorimetry (DSC). The resin curing of the epoxy was monitored by the change in oxirane spectral band in the IR spectrum. Glass fiber reinforced composites of DDEBM–DDM-epoxy were prepared and evaluated for their physical and chemical properties. © 1996 John Wiley & Sons, Inc.