含异氰脲酸酯基环氧树脂的合成

为了改善环氧树脂的耐热性与韧性 ,以三羟乙基异氰脲酸酯 (THEIC)为原料 ,与环氧氯丙烷 (ECH)合成了氯化聚醚多元醇 (CPP) ,CPP与氢氧化钠反应制备了一种新型的含异氰脲酸酯基和醚键的液体环氧树脂 (EP) ,并通过IR确定了结构。CPP与氢氧化钠的摩尔比为 1∶3.2 5,在 2 50ml乙醇 ( 0 .1molCPP)中 ,室温反应 3h ,产率 87.7% ,环氧值 0 .36 87。     

新型脂肪族超支化环氧树脂的制备及其改性作用

采用一步法合成了新型脂肪族超支化环氧树脂HTPE-3,利用FT-IR对其结构进行了表征。研究了双酚A型环氧树脂E-51/HTPE-3杂化树脂的力学性能和热性能。结果显示,杂化树脂的韧性和强度随HTPE-3含量的增加先增加后降低,具有极大值;当HTPE-3质量分数为12%左右时,与纯E-51树脂相比,杂化树脂的冲击强度和断裂韧性分别提高了169.8%和35.2%,拉伸强度和弯曲强度分别提高了6.5%,10.0%,维卡软化点温度、玻璃化转变温度和热分解温度略有下降。     

Toughening of epoxy resins with thermoplastics. Ii. Tetrafunctional epoxy resin-polyetherimide blends

A series of blends has been prepared by adding a polyetherimide (PEI), in varying proportions, to a tetrafunctional epoxy resin, tetraglycidyl-diaminodiphenylmethane (TGDDM), cured with 4,4′-diaminodiphenylsulphone (DDS). All the materials exhibited two-phase morphologies which were characterised by dynamic mechanical thermal analysis and scanning electron microscopy. Addition of the thermoplastic gave a modest improvement in fracture properties (K_1c and G_1c), as determined by three-point bending experiments, although no obvious correlation with the marked morphological changes was observed.     

笼型倍半硅氧烷环氧树脂的合成与表征

以3-缩水甘油丙氧基三甲氧基硅烷(GTMS)为原料在异丙醇(IPAP)中水解缩合制成笼型倍半硅氧烷环氧树脂(POSSEP),用红外光谱(FTIR)、~1H-NMR、热重分析(TGA)和液相色谱-质谱联用仪(LC/MS)对其结构进行了表征。LC/MS分析结果表明,合成的笼型倍半硅氧烷环氧树脂以T_(10)为主,另外还含有一定量的T_8以及少量的T_9。热重分析结果表明,笼型倍半硅环氧树脂具有良好的耐热性。在失重5%时的温度为364．5℃,在444．7℃时降解速率最快,800℃以后笼型硅环氧树脂质量基本不变,900℃时的剩余质量为40%。     

含金刚烷结构新型环氧树脂的合成

以1,3-二(4-羟苯基)金刚烷(BPAD)和环氧氯丙烷(ECH)为原料,采用一步法合成了1,3-二(4-羟苯基)金刚烷二缩水甘油醚(DGEBAD),并优化了中间体BPAD的合成工艺。研究了原料配比,反应温度以及反应时间对DGEBAD的合成反应及产物的影响。结果表明,DGEBAD最优合成反应条件如下:BPAD与ECH物质的量比为1∶15,反应温度80℃,反应时间6 h,所得DGEBAD具有较高的环氧值和产率(分别为0.376 mol/100 g和147.1%)。     

环氧树脂改性PUA乳液的合成及性能研究

以异佛尔酮二异氰酸酯（IPDI）、聚醚二元醇（N220）、二羟甲基丙酸（DMPA）、1,4-丁二醇（BDO）和甲基丙烯酸甲酯（MMA）为主要原料合成了脂肪族聚氨酯-丙烯酸酯复合乳液（PUA）,并用环氧树脂对其进行了改性。研究了nNCO／nOH比、DMPA添加量、环氧添加方式及添加量对其性能的影响,结果表明,当nNCO／nOH为1．35-1．4、DMPA为6％～7％时,以环氧和BDO一起加入,环氧添加量在2％～3％时能获得综合性能较好且贮存稳定的聚氨酯丙烯酸酯复合乳液。     

多面齐聚倍半硅氧烷改性环氧的制备及表征

以八苯基多面齐聚倍半硅氧烷为原料通过溴代,格氏试剂与丙酮加成等反应制备了八多羟基苯基多面齐聚倍半硅氧烷,并对产物进行了FTIR表征。采用该产物改性环氧树脂,并通过热失重分析仪、示差扫描量热仪对其固化物的热性能进行了研究。结果表明:该合成具有活性官能团的多面齐聚倍半硅氧烷的方法可行。在环氧树脂中加入八多羟基苯基多面齐聚倍半硅氧烷对其固化物热稳定性影响不大,但可以显著提高材料的玻璃化转变温度,当其质量分数为5.13%时,Tg可达183.2℃。     

聚氨酯-环氧树脂复合乳液的合成与性能研究

以六亚甲基二异氰酸酯(HDI)、聚醚二元醇(Diol-1000)、二羟甲基丙酸(DMPA)、乙二胺(EDA)和环氧树脂(E-20)等为主要原料制备了聚氨酯-环氧树脂复合乳液。研究了聚醚二元醇含量、羧基含量对复合乳液的稳定性及涂膜柔韧性和耐水性等的影响,用电化学阻抗技术研究了涂层的耐腐蚀性能。     

Synthesis and characterization of petroleum and biobased epoxy resins: a review

Petroleum based epoxy resins exhibit various excellent properties such as adhesion, mechanical performance, electrical insulation and chemical resistance. There is wide concern towards depletion of non‐renewable resources, climate change and finding renewable alternatives for petroleum based materials to reduce the emission of greenhouse gases. This review mainly draws attention towards the utilization of renewable resource based epoxy resin derived from lignocellulosic biomass, furan, tannins, itaconic acid, rosin acid and bio‐oil etc. Without altering the mechanical and thermal properties much, epoxy resins derived from renewable materials have been widely investigated. The last two decades have witnessed an exponential growth in using bio‐derived products, which has been driven by the need to replace petroleum based materials, reduce fuel consumption and lower the overall environmental impact. © 2018 Society of Chemical Industry     

Synthesis and characterization of epoxy based nanocomposites

Epoxy‐clay nanocomposites were synthesized to examine the effects of the content and type of different clays on the structure and mechanical properties of the nanocomposites. Diglycidyl ether of bisphenol‐A (epoxy) was reinforced by 0.5–11 wt % natural (Cloisite Na⁺) and organically modified (Cloisite 30B) types of montmorillonite. SEM results showed that as the clay content increased, larger agglomerates of clay were present. Nanocomposites with Cloisite 30B exhibited better dispersion and a lower degree of agglomeration than nanocomposites with Cloisite Na⁺. X‐ray results indicated that in nanocomposites with 3 wt % Cloisite 30B, d‐spacing expanded from 18.4 Å (the initial value of the pure clay) to 38.2 Å. The glass transition temperature increased from 73°C, in the unfilled epoxy resin, to 83.5°C in the nanocomposite with 9 wt % Cloisite 30B. The tensile strength exhibited a maximum at 1 wt % modified clay loading. Addition of 0.5 wt % organically modified clay improved the impact strength of the epoxy resin by 137%; in contrast, addition of 0.5 wt % unmodified clay improved the impact strength by 72%. Tensile modulus increased with increasing clay loading in both types of nanocomposites. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 1081–1086, 2005     

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     

高折射率含硫环氧树脂PTETE的合成与表征

以苯硫酚、氯乙醇和环氧氯丙烷为原料,通过直接法合成高折射率苯硫基乙基-2,3环氧1丙硫醚（PTETE）环氧树脂。研究了原料配比、温度和氢氧化钠的用量等因素对产物产率的影响。得出最佳反应条件为：反应温度为0～10℃,环氧氯丙烷、MEPS与NaOH摩尔比为1．25：1：1,产率91．50％,产物的折射率1.6016。并通过FT-IR对合成的原料和产物进行表征。     

低电子阻抗环氧树脂的合成

采用金属钙络合离子中间体与双酚A型环氧树脂合成了低电子阻抗的环氧树脂,通过多元胺固化剂交联制备了低电子阻抗的环氧树脂固化物。用差示扫描量热法和热重分析法分别测试了低电子阻抗环氧树脂的固化过程与固化产物的热稳定性,考察了金属钙络合离子中间体与环氧树脂的用量比及反应时间对固化物的体积电阻率的影响。结果表明,引入金属钙络合离子中间体后,环氧树脂E-51固化物的冲击强度为12.1kJ/m2,弯曲强度为78.9MPa。     

高折射率含硫环氧树脂的合成与表征

利用间接法以巯基乙醇和环氧氯丙烷 (ECH)为原料通过 3步反应得到 2 ,3 二 (2 ,3 环氧丙硫乙硫基 )丙基·2 ,3 环氧丙基硫醚型环氧树脂 (TGEBES) ,其折射率和环氧值分别达 1.5 85 0和 0 .5 3;在没有任何催化剂的条件下 ,按以三元硫醇 (BES)和ECH物质的量比为 1∶3.6、在温度为 0～ 5℃下反应 3～ 4h ,环氧化反应的产率达到84 .5 %。并利用红外光谱和核磁共振对含硫高折射率环氧树脂的结构进行了表征 ;利用高效液相色谱对TGEBES和BES的纯度进行了测定 ,结果表明TGEBES和BES纯度分别达 96 %和 97.7%以上。     

新型含磷阻燃环氧树脂的合成与表征

以2-(5,5-二甲基-4-苯基-2-氧代-1,3,2-二氧磷杂环已烷膦酸酯基)-对苯二酚和双酚A 二缩水甘油酯合成了一新型的含环状膦酸酯结构的阻燃环氧树脂(DPODB-EP).采用元素分析、红外光谱(FTIR)和凝胶渗透色谱(GPC)对该含磷环氧树脂的结构和相对分子质量分布进行了表征.采用示差扫描量热法(DSC))和热失重法(TG)对DPODB-EP/PN固化物热性能进行了测试,发现该固化物具有较高的玻璃化转变温度(165℃)和较高的燃烧残炭率(700℃,31%).阻燃性能测试表明该固化物具有较好的阻燃效果,在磷的质量分数为2.25%时其极限氧指数可达29.5%.     

低黏度浅色环氧丙烯酸酯的合成

讨论比较了环氧丙烯酸酯合成过程中温度、催化剂、阻聚剂、投料方式等因素对生成产品性能与外观的影响。研究表明,最优的反应工艺条件为：环氧基与丙烯酸摩尔比1.00∶1.02,采用E-51作原料,四乙基溴化胺作催化剂,对羟基苯甲醚作阻聚剂,催化剂与阻聚剂一同均匀地分散于丙烯酸中,将丙烯酸混合物滴入E-51;采取分步控温的方式：...     

硫醇-烯烃点击反应制备含硫环氧树脂及其性能研究

硫醇-烯烃点击反应是反应速度快、产率高、产品结构可控的高效环保合成技术。以三羟甲基丙烷-三巯基丙酸酯和甲基丙烯酸缩水甘油酯为原料,通过巯基和双键的点击反应制备了一种新型的含硫环氧树脂,产率达99．16％,利用红外光谱和氢核磁其振谱图对含硫环氧树脂的化学结构进行了表征。采用甲基六氢苯酐固化含硫环氧树脂。用差热和热重分析测得玻璃化转变温度（Tg）和表现热分解温度分别为72．0℃和310．9℃。     

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。     

DDS型多官能环氧树脂的合成及其胶粘剂的研制

在催化剂TCAT-172作用下,以4,4'-二氨基二苯砜DDS与环氧氯丙烷ECH为主要原料开环反应生成氯代中间产物,再在碱性环境下闭环生成DDS型多官能环氧树脂,并对其进行红外表征及环氧值、挥发分、产率测试;此外,以其为基体树脂制备环氧胶粘剂,并对该胶粘剂进行性能研究。结果表明,合成的DDS型多官能环氧树脂综合性能较好,其环氧值高达0.70~0.71,挥发分为0.95%左右,产率为90%~92%;制备出的DDS型环氧胶粘剂的综合性能优异,室温下拉伸剪切强度为23.8 MPa,180℃时仍有14.5 MPa,相对介电常数在3.83~3.95之间,吸水性在1.22%左右。     

双酚F/间苯二酚共聚型环氧树脂的合成

为提高双酚F环氧树脂的综合性能,以双酚F、间苯二酚与环氧氯丙烷反应制得双酚F／间苯二酚共聚型环氧树脂。研究了催化剂用量、反应温度、反应时间以及闭环时的加碱速度等因素对产物性能的影响,并对产物进行了表征。结果显示,其最佳合成工艺条件是:间苯二酚与双酚F质量比为20:80,催化剂摩尔分数为2．0％．醚化温度为80℃,醚化时间为5 h,闭环时加碱速度为0．4g/min。