双酚A改性甲阶酚醛树脂的合成和表征

利用双酚A、苯酚、甲醛水溶液为原料,在KOH的催化下,合成了一种含有羟甲基的双酚A改性甲阶酚醛树脂,研究了反应温度、反应物配比、催化剂用量、反应时间对合成的影响,并用红外光谱分析了产品的结构。结果表明,在反应温度为80℃,反应时间为3 h条件下,各反应物物质的量比的适宜范围:n(甲醛):n(苯酚)为(3.0～3.5):1,n(氢氧化钾):n(苯酚)为(0.085～0.15):1;n(双酚A):n(苯酚)为(0.1～0.35):1。     

双酚A改性甲价酚醛树脂的合成和表征

利用双酚A、苯酚、甲醛水溶液为原料，在KOH的催化下，合成了一种含有羟甲基的双酚A改性甲阶酚醛树脂，研究了反应温度、反应物配比、催化剂用量、反应时间对合成的影响，并用红外光谱分析了产品的结构。结果表明，在反应温度为80℃，反应时间为3h条件下，各反应物物质的量比的适宜范围：n(甲醛)：n(苯酚)为（3.0-3.5）:1;n(氢氧化钾)：n(苯酚)为（0.085-0.15）:1;n(双酚A)：n(苯酚)为（0.1-0.35）:1。     

5-氨基-1-（2-羟乙基）吡唑合成工艺条件优化

以3-乙氧基-2-氰基丙烯酸乙酯和羟乙基肼为原料,经环合、水解等一锅法合成5-氨基-1-(2-羟乙基)-4-甲酸吡唑,然后加热脱羧得到5-氨基-1-(2-羟乙基)吡唑.考察了环合反应反应物物质的量比对收率的影响,确定了最佳物质的量;通过正交设计优化了水解反应的工艺条件.产物收率73.8%,高于文献报道值57%.     

二步法合成固体环氧树脂工艺研究

以低分子质量液体双酚A型环氧树脂E-54及固体双酚A为原料,分别选用三苯基膦、乙基三苯基醋酸膦、乙基三苯基氯化膦、乙基三苯基溴化膦、四苯基溴化膦为催化剂,采用二步法合成了固体环氧树脂E-12。研究了不同催化剂、原料配比对产物性能的影响以及反应转化率随时间及温度的变化趋势。结果表明,采用乙基三苯基溴化膦为催化剂,催化剂最佳用量为原料树脂质量的1/900。反应过程平稳,产物透明,软化点适中。     

环氧树脂新型固化剂—双酚A线性酚醛树脂的合成反应研究

本文介绍了一种环氧树脂新型固化剂－双酚Ａ线性酚醛树脂的合成方法,探讨了醛酚比、反应时间、反应温度、催化剂种类及加入量对产物软化点、分子量、残留ＢＰＡ含量的影响。     

线型双酚A酚醛树脂的合成

对线型双酚A酚醛树脂的合成工艺及催化剂浓度、种类、反应时间、醛酚比等影响因素进行了研究。结果表明,随着反应物醛酚比的增大,产物中残留的BPA量呈下降趋势,软化点先上升后下降,在1.2左右出现峰值;随反应时间延长,产物的软化点升高,分子质量增大,残留BPA量减少,分子质量分散性增加;催化剂用量增大,分子质量增大,软化点增高,残留BPA含量降低。合理的催化剂用量为m(BPA)∶m(催化剂)=100∶20。以合成的BPAN代替双氰胺(D ICY)作环氧树脂EB454A80的固化剂,在相同的固化工艺条件下,固化物的Tg提高近12℃。     

含硅化合物改性聚酯的合成与性能研究

为制备疏水性聚酯,在缩聚阶段将含硅化合物双羟甲基硅油加入聚酯反应体系进行缩聚反应,合成含硅改性聚酯。利用傅里叶红外光谱(FT-IR)对改性聚酯结构进行表征,采用接触角测量仪测定水的静态接触角,分析双羟甲基硅油的添加量与改性聚酯表面疏水性的关系。采用差示扫描量热仪(DSC)和热重分析仪(TGA)对改性聚酯的结晶性能和热稳定性进行了测试。结果表明,双羟甲基硅油的加入量为2%时可使聚酯表面接触角提高33°,随着双羟甲基硅油添加,改性聚酯结晶速率变慢,热稳定性略有提升。     

固体双酚A型环氧树脂的合成与表征

以液体环氧树脂和高纯度双酚A为原料,加入季铵类催化剂,通过加成聚合法制备了高分子质量固态环氧树脂。通过环氧值,软化点,折光系数和透光率的测定,研究了双酚A加入量对环氧当量与软化点的影响以及合成树脂的光学性质。结果表明,产物的环氧当量随着双酚A加入量的增加而提高,软化点与双酚A的加入量呈线性增长关系。产物的转化率在94%以上。树脂样品在可见光区无明显的吸收,400nm透光率接近70%,在近紫外区透光率随波长减小出现明显衰减,双酚A用量对折射率几乎没有影响。     

不饱和聚酯和环氧树脂嵌段共聚物的研究

本文利用环氧基功能团与羟基反应,使聚酯分子扩链,合成了A—B—A型嵌段共取物,其耐酸碱性比普通型不饱和聚酯强可与3301双酚A型不饱和聚酯媲美,提高了聚酯的耐碱性。     

柠檬酸三乙酯的新催化合成

实验首次采用中孔分子筛MCM-41为催化剂,直接用反应物乙醇作带水剂,用乙醇和柠檬酸为原料合成了柠檬酸三乙酯.考察了催化剂用量、反应物物质的量比、反应温度和反应时间对柠檬酸三乙酯收率的影响.通过实验得出该反应最佳的合成条件是:柠檬酸和乙醇的物质的量配比为1:8,催化剂的量为柠檬酸质量的1.5％,反应时间为6h,反应在剧...     

D-33单体中的游离双酚A含量对3301不饱和聚酯树脂凝胶时间的影响

本文对D-33单体中的游离双酚A含量对3301不饱和聚酯树脂凝胶时间的影响进行了诸方面的讨论,并最终提出了D-33单体中的游离双酚A含量不能阻止苯乙烯单体与聚酯交联,也就是说D-33单体中的游离双酚A不能影响3301不饱和聚酯树脂的凝胶时间。     

用废PET醇解制墨粉树脂的研究

本实验主要研究了回收PET瓶片在催化剂和二元醇存在下,进行醇解和酯交换转化为各种不同组成具有端羟基低分子链段和二醇,进而醇解产物与反丁烯二酸酯化缩聚为用于墨粉树脂的聚酯。探索了从原料配比到反应工艺条件等多方面因素合成聚酯树脂的条件。利用聚酯回收料为原料醇解后直接合成墨粉用聚酯树脂的工艺简单、产品质量稳定、具有良好的经济效益和环保效应。     

Characterization of imidazole-cured epoxy–phenol resins

The physical and chemical properties of the diglycidyl ether of bisphenol A (DGEBA) cured with different concentrations of bisphenol A (BPA) and 2-ethyl-4-methylimidazole (EMI-24) were examined using Fourier transform infrared spectroscopy, differential scanning calorimetry, dynamic mechanical and dielectric analyses, and solvent extraction studies. The effects of the phenol-epoxide and the secondary hydroxyl (R-OH)-epoxide reactions on the network formation process were analyzed using a recursive modeling technique to obtain expressions for the weight-averaged molecular weight, the weight fraction solubles, and the gel point as a function of the extent of cure and the epoxide-phenol reactant ratio. The sol fraction and the gel point predictions from recursive modeling studies of the network formation process agreed with the results obtained from the extraction studies. The results from the network modeling studies were also related to the thermal and rheological properties of the resin during cure.     

高分子网络凝胶法制备纳米氧化锌的工艺控制

以乙酸锌[Zn(Ac)2]为原料,丙烯酰胺(AM)为单体,N,'N'-亚甲基双丙烯酰胺(MABM)为网络剂,采用高分子网络凝胶法制备了纳米ZnO粉体,研究了其制备过程中反应物浓度、引发剂(NH4)2S2O8含量、溶液的pH值及备反应条件对纳米ZnO晶粒尺寸的影响.X射线衍射分析结果表明:纳米ZnO颗粒的平均晶粒大小随Zn2+起始浓度引发剂含量的增加而增加,随溶液pH值的增加而减小.确定了用高分子网络凝胶法制备纳米ZnO粉体的最佳工艺参数为:反应温度80℃;反应时间2h:干燥温度100℃:干燥时间4h.     

特种氢化双酚A型环氧树脂合成研究

氢化双酚A和环氧氯丙烷在催化剂作用下开环反应生成了氯醇醚,而后加碱进行闭环反应,制备了低分子质量氢化双酚A型环氧树脂,再将其进一步与氢化双酚A等进行加聚反应,得到高分子质量环氧树脂。通过对产物的环氧值、力学性能和电性能的测试,研究了环氧氯丙烷用量、碱用量、环化反应温度、时间、溶剂及催化剂对合成反应的影响。结果表明,最佳反应条件为:环氧氯丙烷与醇羟基的物质的量比为3.0~3.5∶1,n(NaOH)∶n(醇羟基)=1∶1.1~1.2,环化反应温度25~30℃、时间4 h,甲苯为溶剂,催化剂为自制EH-10。所得氢化双酚A环氧树脂质量稳定,可替代进口。     

Studies on curing and thermal behavior of diglycidyl ether of bisphenol‐A and benzoxazine mixtures

This article describes the synthesis and characterization of benzoxazine monomers prepared by reacting the mixture of amine (aniline [A], 3‐chloroaniline [C], o‐toluidine [T]) and phenol (bisphenol‐A [B], phenol [P]) with formaldehyde [F]. The benzoxazine monomers prepared by reacting B and F with A, C, and T have been designated as BAF, BCF, and BTF, respectively. Structural characterization of benzoxazines was done using FTIR, ¹H NMR, and elemental analysis. The curing behavior of benzoxazine monomers was investigated by differential scanning calorimetry in the presence of diglycidyl ether of bisphenol‐A (DGEBA). In all the samples, the molar ratio of benzoxazine monomer:DGEBA, was varied as 1 :0, 3 : 1, 1 : 1, and 1 :3. The peak exotherm temperature (T_p) was lowest in all the samples having molar ratio of 3 : 1 benzoxazine:DGEBA and highest in samples having molar ratio of 1 : 3. The heat of polymerization (ΔH) was found to be maximum during curing of mixture of DGEBA and benzoxazine monomer prepared from phenol, aniline and formaldehyde (PAF). Thermal stability of benzoxazines:DGEBA mixture cured isothermally was evaluated by recording thermogravimetric traces in nitrogen atmosphere. The char yield was highest for a mixture having benzoxazine : DGEBA in the ratio of 3 : 1. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

低温固化型水性聚酯的合成及其水性烤漆应用

基于功能性组分羟乙基化双酚A,间苯二甲酸-5-磺酸钠以及多元醇/酸合成聚酯共聚物,并以硅烷偶联剂改性获得适合低温固化型水性烤漆的水性聚酯;研究了羟乙基化双酚A,间苯二甲酸-5-磺酸钠,支化组分以及硅烷偶联剂,与水性聚酯水溶性、贮存稳定性以及合成过程黄变的关系,确定了上述组分对水性低温固化涂层的耐化学性、耐溶剂性以及光泽...     

墨粉低温定影性能的影响因素分析

介绍了复印机、打印机墨粉的组成及其定影性能评价方法,探讨了不同分子质量分布的聚苯乙烯树脂、聚酯树脂、低分子蜡对墨粉定影性能的影响。结果表明,在墨粉树脂组分中同时加入低分子质量组分和高分子质量组分的聚苯乙烯丙烯酸树脂可降低墨粉的定影温度、扩大定影温度范围并改善定影性能;低分子质量聚酯树脂更适应低温定影要求并提供良好的耐久性和保存性;低分子蜡的使用有利于改善offset性能。     

双酚F的合成及其应用研究综述

本文介绍了目前国内外双酚F生产的技术路线,以及双酚F在环氧树脂、PC树脂、酚醛树脂、聚酯树脂等合成材料中的应用,并重点对双酚F型和双酚A型环氧树脂的性能进行了比较。     

Synthesis and characterization of 3,3′‐disulfonated‐4,4′‐dichlorodiphenyl sulfone (SDCDPS) monomer for proton exchange membranes (PEM) in fuel cell applications

A systematic study of the synthesis and characterization of 3,3′‐disulfonated‐4,4′‐dichlorodiphenyl sulfone (SDCDPS) monomer was conducted by varying reactant stoichiometries (molar ratios of 4,4′‐dichlorodiphenyl sulfone (DCDPS) to SO₃ 1 : 2.2, 1 : 2.9, and 1 : 3.3), reaction temperature (90–120°C), and reaction time (4–6 h). The optimum synthesis batch process variables were 1 : 3.3 reactant molar ratio (DCDPS : SO₃) at 110°C for 6 h. In earlier studies, recrystallization of the “crude” disulfonated monomer from alcohol–water mixture was necessary to remove the monosulfonated and DCDPS impurities that lowered yield. However, in the current research, SDCDPS was successfully synthesized at nearly 100% conversion, which effectively eliminated the need for recrystallization. Recrystallization of SDCDPS from several alcohol–water mixtures (methanol–, ethanol–, and isoproponal–water mixtures) was investigated to compare product purities. Several characterization methods including proton NMR, HPLC, UV–visible, and fast atom bombardment mass spectroscopy confirmed that the crude SDCDPS was completely disulfonated and identical to recrystallized SDCDPS, without having any monosulfonated or starting material DCDPS impurities. Hence, it was demonstrated that the crude SDCDPS monomer by the current one‐step process and the recrystallized SDCDPS monomer were identical. This optimized monomer synthesis has been used to scale up the SDCDPS and poly(arylene ether sulfone) random and statistical copolymers at controlled disulfonation (35 and 45 mol %) levels, which were then used to fabricate proton exchange membranes for fuel cell applications. The intrinsic viscosity data confirmed that high molecular weight film forming copolymers were synthesized. The calculated degree of disulfonations by proton NMR was in close agreement with target disulfonations. It may be concluded that this optimized SDCDPS synthesis eliminates the need for recrystallization, which would be expected to improve process economics. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 4595–4602, 2006