双酸型离子液体[HO_(3)S(CH_(2))_(3)NEt_(3)]Cl-ZnCl_(2)(x(ZnCl_(2))=0.60)催化合成松香甘油酯

Synthesis of Rosin Glyceride Catalyzed by Double Acidic Ionic Liquid [HO_(3)S(CH_(2))_(3)NEt_(3)]Cl-ZnCl_(2)(x(ZnCl_(2))=0.60)

制备并表征了Bronsted-Lewis双酸型离子液体3-磺酸丙基三乙基铵氯锌酸盐[HO_(3)S(CH_(2))_(3)NEt_(3)]Cl-ZnCl_(2)(x(ZnCl_(2))=0.60),并用于催化合成松香甘油酯。考察了原料配比、催化剂用量、反应时间和反应温度等条件对反应结果的影响。结果表明:所合成的离子液体具有可调变的Bronsted与Lewis酸性特征,且两酸性间兼有的协同催化效应显著提高了反应的催化性能;在n(松香)∶n(甘油)=1∶0.8、松香15.0 g和催化剂0.3 g、反应温度230℃、反应时间5 h、真空度40 kPa的较佳实验条件下,产物松香甘油酯的软化点为104.5℃、酸值(KOH)为9.2 mg·g^(-1)、色泽为10~11(Fe-Co)。且反应后分离所得催化剂重复使用6次后,其催化性能未见降低,具有较好的可重复使用性。

Bronsted-Lewis double acidic ionic liquid[HO_(3)S(CH_(2))_(3)NEt_(3)]Cl-ZnCl_(2)(x(ZnCl_(2))=0.60)was prepared,characterized,and used for catalytic synthesis of rosin glyceride.The influences of reaction conditions,such as kinds of catalysts,amounts of catalyst,reaction time and temperature were examined.The optimum reaction conditions for esterification were obtained as follows:n(rosin)∶n(glycerinum)=1∶0.8,rosin 15.0 g,catalyst 0.3 g,reaction temperature 230℃,reaction time 4 h,and vacuum degree 40 kPa.Under the above reaction conditions,the softening point of rosin glyceride was 104.5℃,the acid value(KOH)was 9.2 mg·g^(-1),the color was 10—11(Fe-Co).The recyclability of the catalyst was also investigated.When the catalyst[HO3S(CH2)3NEt3]Cl-ZnCl2(x=0.60)was repeatedly used for six times,it′s catalytic performance had not been reduced,so it had good reusability.