乙酰丙酸反应分离一体化制α-当归内酯

Preparation of α-Angelica Lactone by Integrated Reaction-Separation Process from Levulinic Acid

以生物质基平台化合物乙酰丙酸为原料,磷酸为催化剂,在较低温度下合成了α-当归内酯。通过对反应规律的考察,发现α-当归内酯在反应工艺条件下不稳定,只有及时将生成的α-当归内酯导出反应体系,才能有效提高反应收率。作者采用反应分离一体化工艺,分别考察了反应温度、磷酸质量分数和体系压力对α-当归内酯收率的影响,确定的最佳反应条件为:反应温度140℃,磷酸质量分数3%,体系压力9kPa。在该反应条件下α-当归内酯的选择性达96%,收率达88%。

α-Angelica lactone （α-AL） was synthesized at rather low temperature from the bio-platform chemical-levulinic acid （LA） with phosphoric acid as catalyst, α-AL was found to be unstable under the reaction conditions through the research of reaction process. To increase the yield of α-AL, the separation of α-AL in situ from the reaction system was necessary. The integrated reaction-separation process was proposed to increase the yield of a-AL. The effects of reaction temperature, phosphoric acid mass fraction and system pressure on the yield of a-AL were investigated. The optimal conditions were 140 ℃ ,3% phosphoric acid mass fraction and 9 kPa of system pressure. The selectivity and yield of α- AL can be obtained as 96% and 88% ,respectively.