松香基磷酸酯地合成及性能研究.docVIP

松香基磷酸酯的合成及性能研究 Study on Synthesis and Properties of Rosin-based Phosphate 摘 要 本论文是以歧化松香和环氧乙烷反应生成的松香聚氧乙烯醚（PA）为原 料，使用 P2O5 为磷酸化剂进行磷酸酯化反应合成磷酸酯类阴离子表面活性 剂。红外光谱表明，合成产物为松香基聚氧乙烯醚磷酸酯(PPA)。 本论文先在催化剂作用下以歧化松香为起始原料与环氧乙烷(EO)发生加成 反应合成松香聚氧乙烯醚（PA）。研究了反应温度、催化剂用量对反应的影 响，得到适宜的反应条件为：反应温度为 180℃，催化剂用量为总投料量 （mol）的 3.6%。红外光谱表明，歧化松香的羧基与环氧乙烷发生了加成反 应。考察了环氧乙烷聚合度(n)对产物 PA 物性的影响：随着环氧乙烷聚合度 （n）增大，产物色泽加深，粘度先减小后增大，聚乙二醇含量增加，单酯得 率下降，产物羟值呈减小趋势。 在惰性气体保护下,将 PA 与磷酸化剂 P2O5 进行酯化反应合成松香基聚氧 乙烯醚磷酸酯(PPA)，再进行适当的后处理。研究了投料比、反应温度、时间 及投料方式对酯化反应的影响，得到适宜的磷酸酯酯化条件：PA/P2O5 =2:1 （mol/mol）、酯化温度 80℃、酯化反应时间 6 小时，采用分批进料方式。研 究了水解时间、温度以及加水量对磷酸酯收率的影响，得到适宜的水解条件： 加水量为 4%（g/g），水解温度 60℃ 研究了不同 EO 聚合度（n）的 PPA 的乳化及破乳应用试验，结果表明 PPA-15, PPA-20(n=15, 20)的乳化效果较好，而 PPA-10(n=10)的脱水率较大, 因而有较好的破乳效果。 关键词： 松香; 聚氧乙烯醚; 磷酸酯 ;表面活性剂 ; 合成 ABSTRACT In this dissertation phosphate anionic surfactant was synthesized by phosphorylating polyoxyethylene abietate(PA). Phosphorylating agent was P2O5 there. PA was prepared from disproportionated rosin and ethylene oxide(EO). The structures of phosphate polyoxyethylene abietate (PPA) was identified by IR. PA was first synthesized: Addition reaction of disproportionated rosin and EO was performed in the condition of catalyst. Through the study of the influence of reaction factors such as temperature, calalyst amount. The suitable synthetic conditions were as follow: reaction temperature was 180℃, calalyst amount was 3.6%(based on total materials(mol)). Reaction between carboxyl of the disproportionated rosin and EO had taken place, which was confirmed by IR. The relations between physical properties of polyoxyethylene abietate(PA) and polymerization degree of EO(n) were also studied. With the increasing of polymerization degree of EO, the color of the products be darken gradually; the viscosity was lowering first, then rising; The content of polyglycol was increasing; the yield of monoester and the hydroxyl value of products were dropping. PA was esterified by phosphorus pentoxide and created PPA under nitrogen atmo