DCPD酚型环氧/DCPD苯酚树脂的固化及应用研究

通过DSC分析研究了不同软化点的双环戊二烯(DCPD)酚型环氧与DCPD苯酚树脂在溴化阻燃树脂体系中的固化反应特性并测试了其FR-4覆铜板的性能。结果表明:体系固化反应温度范围较大,DCPD酚型环氧软化点为50,80、90℃时,树脂体系反应活化能分别为98.3,82.3与74.2 kJ/mol。其制成板材的Tg在150℃以上,介电性能良好。随着DCPD酚型环氧树脂软化点的提高,板材玻璃化温度明显提高,高温高压下其吸水率降低,而热分解温度、粘接性及介电性能无明显变化。     

DCPD环氧树脂的合成及在IC封装中的应用

制备了DCPD苯酚树脂，利用该树脂与环氧氯丙烷反应，制备出了DCPD环氧树脂，采用红外光谱分析对所生成的DCPD环氧树脂结构进行了表征，测定了DCPD环氧树脂的羟基值、环氧值、相对分子质量和氯含量。同时采用自制的DCPD环氧树脂作为基体树脂，制备了集成电路（IC）封装用DCPD环氧树脂模塑料。结果表明，制得的DCPD环氧模塑料的吸水率低（0．22％），玻璃化温度高（175℃），热变形温度高（282℃），可用于大规模集成电路IC的无铅封装。     

双酚A型活性酯的环氧固化行为及其性能研究

以双酚A型活性酯(H7070)为双环戊二烯环氧树脂(DCPD)和酚醛环氧树脂(638S)的固化剂,采用傅里叶红外光谱(FTIR)对两种环氧体系固化前后的结构进行了表征,发现固化后环氧基伸缩振动峰几乎消失。通过非等温示差扫描量热法研究两种环氧体系的固化行为,分别得到两种体系的表观活化能、反应级数、表观指前因子和动力学方程。对两种体系进行热重分析,发现H7070/DCPD体系有2个热失重峰,H7070/638S体系有1个热失重峰,H7070/DCPD的热稳定性略优于H7070/638S。两种环氧体系的介电指标相近,介电性能良好。试样H7070/DCPD的弯曲强度,冲击强度分别为92 MPa和60 k J/m2,略优于H7070/638S。     

硅烷单体改性环氧树脂的固化及性能

分别用苯基三甲氧基硅烷(PTMS)和3-缩水甘油醚氧丙基三甲氧基硅烷(KH560)单体对环氧树脂进行了化学改性,通过红外(FT-IR)、核磁(1H NMR)对其化学结构进行了表征。以聚酰胺650为固化剂,用差示扫描量热仪(DSC)研究了固化物的固化动力学。此外还研究了涂膜的热失质量(TGA)、吸水率、附着力等性能。结果表明:苯基三甲氧基硅烷和3-缩水甘油醚氧丙基三甲氧基硅烷接枝上环氧树脂,与纯环氧树脂相比,改性后的树脂具有更好的热稳定性和更低的吸水率。改性环氧树脂固化后形成两面性质不同的涂层,与底材接触的涂层底面保留了环氧树脂原有的附着力,而涂层表面则具有高憎水性,起到防腐等作用。     

含有联萘基团的环氧树脂的合成与固化

合成了一种具有联萘结构的环氧树脂(BEBN)。通过红外光谱、核磁共振氢谱以及元素分析对其结构进行了表征。以双酚A型环氧树脂(E-51)作为参照,采用二氨基二苯基甲烷为固化剂,通过差示扫描量热法(DSC)研究了BEBN,E-51的固化反应性;采用DSC,热重分析对固化物的热学性能进行测试,比较了固化物的力学性能、热性能以及吸水率;探讨了BEBN的结构与性能之间的关系。结果表明,同E-51相比,BEBN的固化反应平缓：BEBN固化物的玻璃化转变温度升高29℃,吸水率降低0．31％,热失重5％和50％的温度分别升高15℃和13℃。     

二甲苯型氰酸酯/环氧树脂固化体系介电性研究

通过介电性能和吸水率测试研究了二甲苯型氰酸酯(DMBPCN)与环氧树脂(EP)不同配比对其共混体系固化物性能的影响。结果表明,随着DMBPCN用量增加,DMBPCN/EP固化物中极性基团减少,介电性能提高。当DMBPCN添加质量分数为90%时,DMBPCN/EP固化物在沸水中浸泡100 h后吸水率仅为0.64%。MBPCN/EP固化体系的耐水性能和介电性能较常用的双酚A氰酸酯/环氧树脂体系高。     

环氧树脂/DMP30体系的微波固化及性能研究

针对目前环氧树脂/固化剂体系微波固化的研究现状,通过预凝胶处理和间歇固化相结合的方法,初步研究了环氧树脂/DMP30[2,4,6-三(二甲胺基甲基)酚]体系的微波固化条件,利用红外光谱研究了微波固化过程,并表征了产物的结构和力学性能。实验结果表明,与传统热固化相比,微波固化可以明显缩短固化时间、降低能耗;微波固化产物和热固化产物具有相同的产物结构;微波固化产物具有更高的弯曲模量和弯曲强度,热固化产物的冲击强度略高一些。     

E-51环氧树脂改性双酚A型氰酸酯树脂的研究

采用示差扫描量热法(DSC)、傅里叶变换红外光谱(FTIR)研究了E-51环氧树脂改性双酚A型氰酸酯树脂(BADCy)体系的反应活性、反应机理及固化工艺,通过TGA分析了不同含量E-51环氧树脂改性BADCy后固化物的热性能,并测定了体系的吸水率及力学性能。结果表明,随着E-51环氧树脂用量的增加,BADCy改性体系的反应活性逐渐提高,固化温度逐渐降低;用环氧树脂改性BADCy生成了恶唑烷酮等芳杂环结构,降低了氰酸酯树脂体系的三嗪环交联密度,增加了体系的韧性;改性后材料的起始热分解温度均在380℃以上,吸水率均低于2%。     

新型含磷环氧树脂的合成及性能研究

合成了一种新型含磷环氧树脂,采用化学分析和红外光谱研究了其结构及反应特性。采用DSC、UL-94垂直燃烧试验和氧指数法表征了含磷环氧树脂/4,4′-二氨基二苯砜(DDS)固化体系的玻璃化温度和阻燃性能,并测定了其拉剪性能及吸水率等。结果表明,含磷环氧树脂的最佳合成反应条件为:反应温度150℃,反应时间150 min,最佳固化工艺为130℃/1 h+160℃/2 h+180℃/2 h+200℃/2 h。磷质量分数为2%时,阻燃效果可达到UL-94-V-0级,同时具有较高的力学强度;固化物玻璃化温度为126℃,吸水率0.24%。该树脂可用于覆铜板等电子产品制造中,可操作性强,成本低。     

高折光指数含硅环氧树脂的合成与性能研究

将二苯基二氯硅烷经过氢化铝锂还原为二苯基硅烷,再与4-乙烯基环氧环己烷进行硅氢加成后合成了1种新型含硅环氧树脂二[2-(3,4-环氧环己基)乙基]二苯基硅烷(EODPS)。该树脂的折光指数达到1.567,并具有较好的透明度。采用甲基六氢苯酐和乙酰丙酮铝-二苯基硅醇组合物分别对EODPS进行固化。通过红外光谱,DSC分析表征了EODPS的结构,研究了其固化活性,并对固化后产物的热稳定性、力学性能和吸水性进行了测试,且与脂环族环氧树脂CEL-2021P性能进行了比较。结果表明,与CEL-2021P相比,EODPS具有更高的热稳定性和更低的吸水率,可用于LED封装。     

用二环戊二烯合成气干型不饱和聚酯树脂

用二环戊二烯,顺丁烯二酸和乙二醇合成不饱和聚酯,这种不饱和聚酯既可浇铸,也可以在空气中固化。     

环三磷腈基多官能液体脂环族环氧树脂的合成

以双环戊二烯、乙二醇和六氯环三磷腈为原料合成一种新型环三磷腈基多官能脂环族环氧化合物（PCNEP）。采用傅里叶变换红外光谱、核磁共振、质谱分析和测定环氧值等方法对PCNEP及其中间体的化学结构进行了表征。合成的脂环族环氧树脂用甲基四氢邻苯二甲酸酐固化,并通过热重分析将PCNEP固化物的热性能与商品化脂环族环氧树脂ERL-4221进行了比较。结果表明：PCNEP固化物的起始热分解温度低于ERL-4221固化物,但在500℃和700℃的高温下,PCNEP固化物的残炭量分别为28．87％,24．73％。     

浅谈双环戊二烯改性不饱和聚酯树脂的生产工艺

采用双环戊二烯改性不饱和聚酯树脂,使得不饱和聚酯树脂具有很多独特的优异性能。主要介绍以双环戊二烯与顺丁烯二酸酐合成双环戊二烯马来酸单酯为基础,经进一步扩链（加入多元醇酯化）之后得到不饱和聚酯树脂的合成过程。剖析了生产设备、生产工艺流程。     

二环戊二烯双酚型环氧树脂及环氧酯漆的合成研究

本文用二环戊二烯和苯酚合成二环戊二烯双酚,再用它与环氧氯丙烷合成二环戊二烯双酚型环氧树脂,并用这种环氧树脂与亚麻油酸合成气干型环氧酯漆,测试了漆膜的性能。实验证明,适当的酚超量和较低的滴加二环戊二烯的反应温度可控制二环戊二烯的自聚反应。     

桐油改性双环戊二烯不饱和树脂的合成及其性能研究

采用催化水解加成法合成了桐油改性双环戊二烯不饱和聚酯,通过对桐油滴加前后不饱和聚酯的凝胶色谱及红外表征,证实了桐油与不饱和聚酯分子链中的双键发生了Diels-Alder反应。研究了桐油加入量对树脂涂膜的气干性、附着力、柔韧性、硬度、耐磨性及树脂耐热性能的影响,并确定了桐油的最佳加入量。结果表明:较未改性的双环戊二烯不饱和聚酯(DCPD-UPR),桐油基DCPD-UPR的涂膜具有更好的气干性、柔韧性、粘接性和耐磨性,并且桐油基DCPD-UPR的耐热性也优于未改性的DCPD-UPR。     

Characterization and application of propylene grafted hydrogenated dicyclopentadiene hydrocarbon resin

Hydrocarbon resins, which are defined as low molecular weight, amorphous, and thermoplastic polymers, are widely used as tackifiers for various types of adhesives, as processing aids in rubber compounds, and as modifiers for paint and ink products, and for use in plastics polymers such as isotactic polypropylene. Recently, the quantities of the hydrocarbon resin׳ raw materials which are the side products from naphtha cracking process have decreased because of light-feed cracking such as gas cracking, so new raw materials for hydrocarbon resin production are essential. To be satisfied with the previously mentioned factors, the substitution of hydrocarbon resin raw materials with renewable resources is a worthy consideration. Moreover, new hydrocarbon resin having high adhesion performance, low specific gravity, and good compatibility with various polymers has been requested in various adhesives.To meet those requests, in this study, propylene instead of side product from naphtha cracking as main raw material of hydrocarbon resin were partially used. The propylene serves as a new, sustainable raw material and was successfully grafted onto dicyclopentadiene. The reaction of the propylene with dicyclopentadiene was confirmed because, according to NMR and FT-IR analyses, a pendant methyl-propylene group exists in the structure of the propylene-grafted, hydrogenated dicyclopentadiene hydrocarbon resin. To establish an optimal production condition regarding the propylene-grafted, hydrogenated dicyclopentadiene hydrocarbon resin, numerous experiments were conducted according to the mole ratio of the raw materials and the polymerization temperature. The propylene-grafted, hydrogenated dicyclopentadiene hydrocarbon resin that was manufactured according to optimal conditions results in a lower specific gravity and a high molecular weight, whereby the advantages of the adhesion properties of an SIS-based pressure-sensitive-adhesive are exploited. When the propylene-grafted, hydrogenated dicyclopentadiene hydrocarbon resin was formulated with the SIS-based pressure-sensitive-adhesive, both the heat stability and the shear-adhesion strength are sound.     

我国双环戊二烯改性不饱和聚酯树脂的研究进展

综述了双环戊二烯改性不饱和聚酯树脂的生产技术,重点介绍了我国近年来双环戊二烯改性不饱和聚酯树脂的研究进展,并指出了双环戊二烯改性不饱和聚酯树脂的发展方向。     

Synthesis and thermal stability of a novel cycloaliphatic epoxy resin system

A novel cycloaliphatic epoxy resin was synthesized from dicyclopentadiene, ethylene glycol, and nadic anhydride. The chemical structures of the resultant epoxy resin and its precursor were characterized with Fourier transform infrared spectroscopy, ¹H‐NMR, and mass spectrographic analyses. The thermal stability of the cured polymer was investigated with differential scanning calorimetry and thermogravimetric analysis. Compared with the thermal stability of the commercial cycloaliphatic epoxy resin 3,4‐epoxy cyclohexyl methyl‐3′,4′‐epoxy cyclohexyl carboxylate, a higher thermal stability for the cured polymer of the novel epoxy resin was observed. The results imply that the novel cycloaliphatic epoxy resin has good potential applications in electronic encapsulation. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

油改性涂料用双环戊二烯型不饱和聚酯树脂的合成及应用研究

介绍了油改性双环戊二烯(DCPD)型涂料用不饱和聚酯树脂的合成工艺以及调漆性能测试。试验结果表明,油与多元醇在210～220℃下先醇解,然后与顺酐反应形成半酯,剩余顺酐水解成顺丁烯二酸,然后与DCPD加成,合成的树脂具有优良的空干性;同时油的使用极大地提高了涂膜的柔韧性和抗绿化性,得到的树脂性能上可满足涂料用不饱和聚酯树脂的要求。     

Synthesis and characterization of a novel epoxy resin containing naphthyl/dicyclopentadiene moieties and its cured polymer

A new epoxy resin containing both naphthalene and dicyclopentadiene (DCPD) groups was synthesized to produce a highly heat-resistant network, and the curing behavior was investigated using diaminodiphenylsulfone (DDS) as curing agent. The chemical structures were characterized with FTIR spectroscopy, NMR, MS, and GPC analyses. Dynamic curing behavior was investigated using differential scanning calorimetry (DSC). The physical properties of the resulting polymers were evaluated with dynamic thermal mechanical analyses (DMTA) and thermogravimetric analyses (TGA). The cured polymer showed great improvement in heat-resistant property including remarkably higher glass transition temperature (T_g) and thermal stability. Such properties make this new epoxy resin highly promising for heat-resistant applications.