用红外光谱法对热固性酚醛树脂固化过程的研究

用红外光谱法研究了四种热固性酚醛树脂在固化过程中的化学变化。结果表明热固性酚醛树脂的固化过程,首先是羟甲基发生缩合反应,缩合反应形成醚键是主要的。热固性酚醛树脂在进一步固化时(150—200°)出现了羰基,它的出现不是亚甲基氧化所致,而是部分醚键断裂形成了醛羰基。对热固性酚醛树脂的固化过程的机理进行了讨论。     

吸水过程对环氧树脂的动态松弛行为的影响

以酚醛树脂和乙酸、正丁酸和苯乙酸酯化的酚醛树脂固化邻甲酚环氧树脂.应用称重法、示差扫描量热法(DSC)和动态机械分析法(DMA)等手段研究吸水过程对环氧树脂的动态松弛行为的影响.结果表明,吸水过程对酚醛树脂和酯化酚醛树脂固化体系的动态松驰行为有显著的影响,这是由于两种体系中侧基对吸水过程及与水分子的相互作用不同所致.     

硼酚醛树脂热分解动力学及其耐热性

用热重法研究了固化硼酚醛树脂的热分解动力学。并用红外光谱法跟踪硼酚醛树脂的固化过程；结果表明，热分解过程为一级反应，由于硼酯键代替了醚键和次甲基键使得热氧化裂解速率常数随硼含量的增加而减小。     

硼酚醛树脂的合成与固化机理的研究

本文研究了硼酚醛树脂的合成与固化反应过程的机理, 结果表明, 甲阶段的硼酚醛树脂主要是硼酸苄酯, 固化过程中形成硼酸苯酯, 反应过程中有醚键生成, 醚键断裂产生羰基。     

吸水过程对环氧树脂的动态松驰行为的影响

以酚醛树脂和乙酸、正丁酸和苯乙酯化的酚醛树脂固化邻甲醛环氧树脂，应用称重法，示差扫描量热法（DSC）和动态机械分析法（DMA）等手段研究吸水过程对环氧树脂的动态松驰行为的影响。结果表明，吸水过程对酚醛树脂和酯化酚树脂固化体系的动态松驰行为有显著的影响，这是由于两种体系中侧基对吸水过程及与水分子的相互作用不同所致。     

硼酸钠/甲阶酚醛树脂配合物的热固化过程和耐热性

硼酸钠/甲阶酚醛树脂配合物的热固化过程和耐热性     

FTIR研究不同固化程度SiO_2/酚醛杂化材料官能团的变化

采用FTIR光谱吸收峰的波数位移、A/A1612表示的吸收强度和半峰宽Δ1/2(O—H)/Δ1/2(C C)表示的谱带宽度,比较不同固化程度SiO2/酚醛树脂杂化材料官能团的变化.在相同固化条件下(120℃,2 h),杂化材料的氢键作用比酚醛树脂的强得多,羟基含量更高,而且杂化材料发生邻位取代缩合反应的比例特别高.正是因为杂化材料中未反应的官能团多,作为底漆使用时能与面漆中的官能团反应,实现无层间界面交联,获得层间结合力.过固化过程(160℃,1 h)能够有效降低杂化材料中的羟基含量,但醚键含量比酚醛树脂的高得多,而且过固化过程中酚环主要发生对位取代缩合反应.杂化材料固化后的颜色比热固性酚醛树脂的淡得多,与热塑性酚醛树脂的相当.在相同氧化程度下,杂化材料中无游离酚,比酚醛树脂更环保.     

酚醛树脂/蒙脱土纳米复合材料的制备及固化反应动力学研究

利用自制的有机蒙脱土 ,采用浇模固化成型法制备酚醛树脂 /六次甲基四胺 /蒙脱土纳米复合材料 ,并用XRD观察有机蒙脱土分别在热塑性和热固性酚醛树脂中复合行为 .研究发现 ,由于两种树脂的固化反应机理不同 ,热固性酚醛树脂与蒙脱土复合 ,可得插层型纳米复合材料 ;而采用热塑性酚醛树脂进行固化 ,则得到部分剥离的纳米复合材料 .通过DSC进一步研究热塑性酚醛树脂 /蒙脱土复合体系的固化反应动力学 .运用Kissinger ,Flynn Wall Ozawa ,Crane方法求出活化能和反应级数等动力学参数 .结果发现 ,加入蒙脱土使固化反应活化能下降 ,反应级数减小 ,从而有利于固化工艺的实现 ,便于纳米复合材料实际应用 .     

增粘树脂对湿固化聚氨酯热熔胶性能的影响

针对湿固化聚氨酯热熔胶,考察增粘树脂中松香树脂、萜烯树脂和萜烯酚醛树脂的加入对湿固化聚氨酯热熔胶初粘强度、终粘强度、熔融粘度、开放时间等性能的影响。结果表明,萜烯酚醛树脂作为增粘树脂所得的湿固化聚氨酯热熔胶熔融粘度低,粘结强度大,热稳定性高,增粘效果显著。     

FD-MS表征酚醛树脂结构

酚醛树脂是常用合成高分子材料,主要分两大类,即Novolak型和Resolve型.前者又称为线型酚醛,本身不能固化,需加固化剂方可固化.后者亦称可溶性酚醛,自身加热即可固化.表征这类聚合物方法很多.近几年随先进质谱仪出现,场解析-质谱(FD-MS)方法用来表征这一类化合物[1].本文尝试用FD-MS表征酚醛树脂结构.     

Preparation of porous/hollow particles of phenolic resin

Porous/hollow polymer microparticles were prepared by suspension polymerization from a resol, water‐soluble phenolic resin in a multiple emulsion system oil‐in‐water‐in‐oil(O/W/O). The porous/hollow structures of phenolic resin microparticle were characterized by optical microscopy (OM) and scanning electron microscopy (SEM). It is shown that the porous/hollow structure is related to a dispersion and curing process of the resol resin. It was indicated that it is low‐cost and simple to prepare porous/hollow phenolic resin micr‐particles from resol in an O/W/O system. Copyright © 2007 John Wiley & Sons, Ltd.     

掺磷酚醛树脂炭嵌锂性能研究

以添加不同含量五氧化二磷的热塑性酚醛树脂为前驱体 ,经热固化后升温至 70 0℃裂解制备掺磷树脂裂解炭 .X射线衍射考察了裂解炭的微晶结构变化 ;恒电流技术研究了裂解炭的充放电性能 .实验表明 ,五氧化二磷的加入使树脂裂解炭微晶结构发生了很大改变 ,随着磷含量的增加微晶层间距减小 ,而且更加无序 ;其放电可逆容量随五氧化二磷掺杂量的增加先增而后减 ,当P2 O5含量为 9wt%时 ,可逆容量达到最大值 (5 2 8mA·h·g- 1) ,是未掺杂 (2 30mA·h·g- 1)的 2倍多     

Preparation of Phenolic Resin/Silver Nanocomposites via in-situ Reduction

Polymer/metal nanocomposites have attracted considerable interest because of their potential application in catalysts, electronics, electromagnetics and nonlinear optics1-3. They have been prepared by blending polymer with nanometer metal particles4, reducing polymer-metal ion complexes with reducing agents5, and reducing metal ions in the polymer matrix by high-energy radial irradiation3. In this paper, we report a new approach to phenolic resin/silver nanocomposites, which have potential a…     

摩阻材料用亚麻油改性酚醛树脂的制备及耐热性研究

利用亚麻油改性酚醛树脂,得到高性能的摩阻材料用树脂基体.推导了改性机理和结构特征,并进行了耐热试验和分析.结果表明,亚麻油参与了反应并成为聚合物的一部分,亚麻油改性酚醛树脂固化后的结构特征是互穿聚合物网络(IPN),与普通酚醛树脂相比,亚麻油改性酚醛树脂的耐热性能显著提高,可望用作耐高温磨阻材料树脂基体.     

Adhesives and coatings based on phenolic/epoxy resins

Low molecular weight epoxy resin based on bis (4‐hydroxy phenyl) 1,1 cyclohexane was prepared and modified with various types of the prepared phenolic resins. Phenol–, cresol–, resorcinol–and salicylic acid–formaldehyde resins were used. The optimum conditions of formulation and curing process were studied to obtain modified wood adhesives characterized by high tensile shear strength values. This study indicated that the more suitable conditions are 1:2 weight ratio of phenol–or cresol–formaldehyde to epoxy resin in the presence of phthalic anhydride (20 wt%) of the resin content as a curing agent at 150°C for 80 min. Resorcinol–or salicylic acid–formaldehyde/epoxy resins formulated at 1:2 weight ratio were cured in the presence of paraformaldehyde (20 wt%) at 150°C for 60 min. The effect of the structure of phenolic resins on the tensile shear strength values of formulated resin samples, when mixed with the epoxy resins and cured under the previously mentioned optimum conditions for different times, was investigated. Metallic and glass coatings from the previous resins were also prepared and evaluated as varnishes or paints. Copyright © 1999 John Wiley & Sons, Ltd.     

Fabrication and Characterization of Diatomite-supported Activated Carbon Functional Ceramic

Using porous diatomite ceramic as carrier and phenolic resin as carbon precursor, the activated carbon functional ceramic with the activated carbon fixed into porous ceramic was prepared by the impregnation load phenolic resin, carbonization and activation isolated air. The influences of impregnation, curing, carbonization, activation etc. on the material property were discussed. The iodine value, SEM, elemental analyzer, BET and spectrum analysis chart were used to characterize the microstructures and performance of material at different conditions. The results showed that the excellent comprehensive property of activated carbon functional ceramic was gained when it adsorbed phenolic resin in 4 h under vacuum condition at curing temperature of 150 ℃ for 0.5 h and carbonization temperature of 600 ℃ for 1.0 h, and then put into 25wt% KOH for 4.0 h at activation temperature of 700 ℃ for 1.5 h. The iodine value is 176.9 mg/g, the specific surface area can reach 86.3 m2/g and the yield of carbonization is 50.48%.     

Synthesis and application of phenolic resin internally toughened by chain extension polymer of epoxidized soybean oil

A novel epoxidized soybean oil (ESO) internally toughened phenolic resin(ESO-IT-PR) with both good toughness and excellent thermal stability was prepared as the matrix resin of copper clad laminate (CCL). FTIR was adopted to investigate the molecular structure of modified phenolic resins and SEM was used to observe the micro morphology of their impacted intersections. The properties of CCLs prepared with these modified phenolic resins were studied to determine the optimal process and investigate the toughening mechanism. The main modifying mechanism is the etherification reaction between phenol hydroxyl and ESO catalyzed by triethanolamine and the chain extension polymerization between ESO and multi-amine gives the long-chain ESO epoxy grafting on the phenolic resin prepolymer. when the ESO content is 30% and the curing agent content is 7%, the ESO toughened phenolic resin possesses optimal performance. The flexible ESO epoxy shows significant toughening effect and it crosslinks with the phenolic resin to form an internally toughened network, which is the key factor for improving the solderleaching resistance of CCL prepared with this modified phenolic resin. __________ Translated from Journal of South China University of Technology (Natural Science Edition), 2007, 35(7): 99–104 [译自: 华南理工大学学报(自然科学版)]     

Chemorheological study of the curing kinetics of a phenolic resol resin gelled

The changes in the resin viscosity, conductivity, mass, and enthalpy during curing reactions have been studied to obtain kinetic parameters that allow modeling of the resin behavior throughout its industrial application. In this work, isothermal rheological tests of a phenolic resol resin were performed in order to study its complex viscosity during crosslinking reactions. Samples were prepared by a precuring treatment in a heated plate press to reach gel point of the resin. Rheological analyses of resol resin curing were carried out at five different temperatures (80-100 °C), and the kinetic models of Arrhenius and Kiuna were applied. The resol resin curing presented an activation energy of 72.1 kJ/mol according to the Arrhenius model. The Kiuna model was proposed to fit the non-linear evolution of the resin’s complex viscosity at the highest temperatures. This kinetic model was suitable for predicting the changes in the complex viscosity of the resol resin after its gelation, and the process activation energy obtained for the second order polynomial applied in this model was 88.1 kJ/mol. In addition, the profile for the degree of curing of resol resin was determined from measurements of the material’s elastic modulus.     

Phenolic materials via ring-opening polymerization: Synthesis and characterization of bisphenol-A based benzoxazines and their polymers

Compounds with bifunctional benzoxazine groups in their molecular structures form crosslinked structures characteristic of phenolic materials through a ring-opening reaction mechanism. This family of compounds offers greater flexibility than conventional novolac or resole resins in terms of molecular design. It is also superior to conventional phenolic resin in process control since it releases no by-product during curing reactions. The materials thus obtained exhibit excellent mechanical integrity with glass transition temperatures over 200°C. The synthesis, composition, and structural analysis of precursors based on bisphenol-A are discussed herein. © 1994 John Wiley & Sons, Inc.     

Synthesis and properties of a deuterated phenolic resin

A highly deuterated novolac‐type phenolic resin was prepared by polycondensation of deuterated phenol and formaldehyde using oxalic acid as an acid catalyst. The polycondensation of deuterated monomers and the formation of the highly deuterated phenolic resin were confirmed by the gel permeation chromatography, IR, and ¹H NMR analyses. With the exception of hydroxyl groups, the degree of deuteration was estimated to be more than 98%. The polymer conformation in THF solution was evaluated by the scaling exponent of the Mark–Houwink–Sakurada equation. The exponent of the deuterated phenolic resin is 0.26 in THF at 40 °C and is close to that of a nondeuterated phenolic resin, which suggests that phenolic resins behave like a compact sphere irrespective of deuteration. The curing behavior of the deuterated phenolic resin with hexamethylenetetramine was confirmed by differential scanning calorimetry analysis. The cured highly deuterated phenolic resin exhibits a lower incoherent neutron scattering background than that of the nondeuterated phenolic resin, which suggests that the former is suitable for matrix resins with low incoherent backgrounds for small‐angle neutron scattering studies of thermosetting resins. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2011.