两步催化法制备异松油烯的工艺研究

【作者】 谢惠定；

【导师】 王亚明；

【作者基本信息】 昆明理工大学 ， 应用化学， 2002， 硕士

【摘要】 异松油烯是一种价格昂贵的精细化学品，制备高收率的异松油烯有着重要的意义。 本论文是以松节油为原材料，采用两步催化制备异松油烯。第一步催化是松节油在13X钠型分子筛的催化下，获得较高收率的双戊烯和部分异松油烯；通过考察不同条件处理的13X钠型分子筛催化剂的活性，发现分子筛-C-d催化剂的活性最佳。第二步催化是以SO₄^2-/ZrO₂固体超强酸为催化剂，使第一步产物中的双戊烯向异松油烯转化，从而获得高收率的异松油烯；不同条件下制备的SO₄^3-/ZrO₂固体超强酸有着不同的活性，根据实验知，SO₄^2-/ZrO₂-Ⅱ-C-3、SO₄^2-/ZrO₂-Ⅱ-D-3催化剂的活性和选择性最佳。 第一步催化反应适宜的工艺条件为：催化剂为分子筛-C-d，催化剂用量为4%，催化剂粒径为30-100目，反应温度为150℃，反应时间为30-60分钟。第二步催化反应适宜的工艺条件为：催化剂为SO₄^2-/ZrO₂-Ⅱ-D-3，催化剂用量为4%，反应温度为80℃，反应时间8-12小时。松节油在以上工艺条件下经两步催化后，异松油烯的收率可达35.24%。更多还原

【Abstract】 Terpinolene is a kind of fine chemicals, and its price is very expensive.lt is important to abtain the high-yield terpinolene.This paper prepared terpinolene using turpentine as raw material by two-stage catalyze. First, turpentine was inverted to high-yied dipentene and part terpinolene using 13X molecular sieve as catalyst.lt was found that catalyst , Molecular sieve-C-d, had optimum activity by inspecting the activity of 13X molecular sieve with different handling conditions. Second,dipentene in the first-stage products was inverted to terpinolene using SO427ZrO2 solid superacid as catalyst.so as to obtain the high-yield terpinolene.The SO42YZrO2 solid superacid catalyst which was prepared in different conditions had different activity.According to experiment ,the SO42YZrO2 - n -C-3 solid superacid catalyst and the SO42YZrO2-II-D-3 solid superacid catalyst had both optimum activity and optimum selectivity.The appropriate technology conditions in the first-stage reaction were as follows: catalyst was Molecular sieve-C-d, the ratio of catalyst and raw material was 4: 100, the diameter of catalyst was 30-100 cohorts, the reaction-temperature was 150, the reaction-time was 30-60 minutes. The appropriate technology conditions in the second-stage reaction were as follows: catalyst was SO427ZrO2-II-D-3 solid superacid catalyst, the ratio of catalyst and raw material was 4: 100, the reaction-temperature was 80, the reaction-time was 8-12 hours. Under the techonology conditions as the above, the yield of terpinolene can reach 35.24% by two-stage catalyzing turpentine.更多还原