硫酸-离子液体复合催化剂催化松香聚合反应工艺的研究

STUDIES ON SYNTHESIS OF POLYMERIZED ROSIN CATALYZED BY SULFURIC ACID-IONIC LIQUID

首次将3种硫酸-离子液体复合催化剂[H2SO4-(C2 mim)BF4、H2SO4-(C4 mim)BF4和 H2SO4-(C8 mim)BF4]用于催化松香聚合反应中,H2SO4-(C4 mim)BF4和H2SO4-(C8 mim)BF4均显 示出很好的催化活性。以H2SO4-(C8 mim)BF4为代表,详细考察了不同溶剂、H2SO4用量、反应温 度和反应时间等因素对反应结果的影响。得到较佳的工艺条件:松香和甲苯质量比1:1。催化剂用量为松香质量的 30％。反应温度70℃,反应时间4h。在该条件下,得到的聚合产物软化点为13℃,酸值为142mg/g。并时H2SO4- (C8 mim)BF4复合催化剂的重复使用性能进行了考察,该复合催化剂克服了传统催化剂的一些缺点,既简化了产物 的分离,又可以重复使用。

Several kinds of catalysts of sulfuric acid-ionic liquid were first used in the synthesis of polymerized rosin. Sulfuric acid-l-n-butyl-3-methylimidazolium tetrafluorobate [ H2SO4-（ C4 mim ） BF4 ] and sulfuric acid-l-n-octyl-3- methylimidazolium tetrafluorobate [ H2SO4-（ C8 mim） BF4 ] have high catalytic activities. For H2SO4-（ C8 mim） BF4, effects of the kinds of solvents, amount of H2 SO4, reaction temperature and reaction time were studied. The optimum reaction condition was as followed： m（rosin） and m（toluene） = 1 ： 1 ,catalyst dosage 30 % （based on rosin mass）, reaction temperature 70 ℃, reaction time 4 h, sofening point of the polymerized rosin could reach 135 ℃, and acid value could be 142 mg/g. The regeneration of H2SO4-（ C8 mim ） BF4 was investigated. The results showed that H2SO4-（C8 mim）BF4 could be excellently reused. By using this catalyst, some defects of traditional catalysts were overcome, and the product could be conveniently separated by decantation.