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SO_4~(2-)/ZrO_2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SO_4~(3-)/ZrO_2固体超强酸有着不同的活性,根据实验知,SO_4~(2-)/ZrO_2-Ⅱ-C-3、SO_4~(2-)/ZrO_2-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SO_4~(2-)/ZrO_2-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%。
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.
引文
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