摘要
用几种稀土元素对单一型固体超强酸SO24-/TiO2进行改性。结果表明,用Ce4+改性效果较好,且当Ce4+质量分数为7.5%、经500℃焙烧3h后催化剂SO24-/TiO2-Ce4+的催化活性最佳,并用TEM、XRD和IR对其结构进行了表征。该改性催化剂属于纳米级材料,粒径为32nm,粒度均匀。并以该固体超强酸SO24-/TiO2-Ce4+为催化剂,松油醇和乙酸酐为原料合成乙酸松油酯。利用正交试验得到适宜的合成条件为:反应温度70℃、催化剂用量3%、松油醇与乙酸酐物质的量之比为1∶1.5、反应时间6h。在此条件下,松油醇转化率达99%,产物中乙酸松油酯含量达90%。与普通型固体超强酸进行比较,SO24-/TiO2-Ce4+具有更高的催化活性和选择性。
Common solid superacid SO~ 2- _4/TiO_2 was modified by several rare earth elements. The results showed that Ce~ 4+ was the best modifying agent among these rare earth substances. Ce~ 4+ -modified solid surperacid SO~ 2- _4/TiO_ 2 -Ce~ 4+ displayed excellent activity when superacid SO~ 2- _4/TiO_2 was impregnated by 7.5 % Ce~ 4+ and then calcined at 500 ℃ for 3 h. The structure of SO~ 2- _4/TiO_ 2 -Ce~ 4+ was characterized by TEM, XRD and IR methods. The catalyst was a nanomaterial with uniform granularity of 32 nm. Synthesis of terpinyl acetate from terpineol and acetic anhydride with solid superacid SO~ 2- _4/TiO_ 2 -Ce~ 4+ as catalyst had been studied for the first time. By orthogonal test, the optimum condition was obtained as follows: reaction temperature 70 ℃, reaction time 6 h, catalyst dosage 3 %, ratio of terpineol to acetic anhydride 1 ∶1.5. Under this condition, the conversion of terpineol was over 99 %, and the content of terpinyl acetate in the product was 90 %. Compared with common superacid SO~ 2- _4/TiO_2, the modified SO~ 2- _4/TiO_ 2 -Ce~ 4+ had higher catalytic activity and selectivity.
出处
《林产化学与工业》
EI
CAS
CSCD
2006年第4期73-77,共5页
Chemistry and Industry of Forest Products
基金
云南省教育厅科研基金资助项目(5Y0091A)
关键词
固体超强酸
稀土元素
乙酸松油酯
催化合成
solid superacid
rare earth element
terpinyl acetate
catalytic synthesis
