一种双官能度环氧树脂乳化剂的合成与应用的研究

Study on the Synthesis and Application of Bifunctional Epoxy Emulsifier

摘要:

以环氧树脂(E-44)、偏苯三酸酐（TMA）及聚乙二醇（PEG4000）为原料，在催化剂三氟化硼乙醚作用下，合成出一种含羧基和羟基双亲水基团的多嵌段环氧乳化剂，再利用相反转法制备出水性环氧乳液。乳化剂的结构通过FTIR、1HNMR和GPC等手段进行分析。探讨了催化剂用量、反应温度和反应时间对乳化合成过程中的酯化率及环氧转化率的影响，并研究了乳化剂用量及乳化温度对所制乳液稳定性的影响。结果表明，合成乳化剂的最佳条件是：催化剂用量（占反应物总质量）为0.36 %，酯化反应2 h，温度70 ℃，酯化率达到96.6 %；环氧开环反应时间为5 h，温度95 ℃，环氧转化率达到94.2 %。当乳化剂用量（占E-44质量）为15 %，乳化温度为60 ℃时，所制得的乳液平均粒径约为312 nm，并且具有良好的稳定性能。

Abstract:

A multiblock epoxy emulsifier with bifunctional group (Hydroxyl and Carboxyl) was synthesized by a series of raw materials, including epoxy resin (E-44), trimellitic anhydride (TMA) and polyethylene glycol (PEG4000) in the presence of the catalyst boron trifluoride etherate. Then waterborne epoxy emulsion was prepared by phase inversion method with the above emulsifier. The chemical structure of emulsifier was characterized by FTIR、1HNMR and GPC. The effects of the amount of catalyst, reaction temperature and time on the esterification epoxy conversion rate in the emulsifier synthesis process were studied. Simultaneously, the effects of the amount of emulsifier and emulsifying temperature on Emulsion stability were explored. The optimum conditions of synthesis emulsifier: catalyst dosage was 0.36 % (the total reactant mass), esterification reaction time was 2 h and temperature was 70 ℃, esterification rate reached 96.6 %. Epoxy ring-opening reaction time was 5 h and temperature was 95 ℃, ethylene conversion reached 94.2 %. Moreover, the emulsion with small average particle size (about 312 nm) and good stability was obtained when emulsifiers dosage was 15 % (the mass of E-44) and temperature was 60 ℃.