第 49 卷第 2 期 | ![](image2/wentou.gif) | Vol. 49 No. 2 | 2019 年 4 月 | Apr 2019 |
|
所属栏目:香精香料
臭氧氧化法合成2,3-丁二酮 |
何 磊1,2,3,4,宋梦新1,2,潘 苗1,2
(1. 淮阴工学院 矿盐资源深度利用技术国家地方联合工程研究中心,江苏 淮安 223003;2. 淮阴工学院 江苏省特色资源开发与药用研究重点实验室,江苏 淮安,223003;3. 淮安万邦香料工业有限公司,江苏 淮安 223003;4. 南开大学 化学学院,天津 300071) |
摘 要:以乙醛为原料,经过缩合和氧化两步反应合成了2,3-丁二酮,在氧化反应时采用臭氧氧化工艺,优化工艺条件为:n(水)∶n(乙偶姻)∶n(乙酸)=1∶0.51∶0.007 5,臭氧氧化温度10℃,臭氧流速0.3 L·min-1,搅拌速度600 r·min-1,反应时间90 min;在上述条件下,2,3-丁二酮收率为96.2%,工业合成试验的分离收率仍可达95.0%。采用熔点检测、FTIR、1H NMR、13C NMR和质谱技术对产物结构进行了表征与确证。 |
关键词:2,3-丁二酮;乙醛;臭氧氧化 |
中图分类号:TQ224.24 文献标识码:A 文章编号:1009-9212(2019)02-0066-04 |
|
Synthesis of 2,3-Butanedione by Ozonization |
HE Lei1,2,3,4, SONG Meng-xin1,2, PAN Miao1,2
(1. National & Local Joint Engineering Research Center for Mineral Salt Deep Utilization, Huaiyin Institute of Technology, Huaian 223003, Jiangsu, China; 2. Jiangsu Key Laboratory of Regional Resource Exploitation and Medicinal Research, Huaiyin Institute of Technology, Huaian 223003, China; 3. Wanbang Perfume Industrial Limited Company, Huaian 223003,China; 4. College of Chemistry, Nankai University, Huaian 223003, China) |
Abstract:2,3-Butanedione was synthesized by condensation and ozonization using acetaldehyde as the raw material. The ascertained optimum conditions were as followings: mole ratio of water, acetoin and acetic acid was of 1∶0.51∶0.007 5; ozonization temperature was of 10℃;the ozone flow was of 0.3 L·min-1; mixing speed was of 600 r·min-1, ozonization time was of 90 min. Under the above conditions, a yield of 96.2% was achieved; the yield also reached up to 95.0% through the test by industrialized production. The structure of the obtained product was characterized by melting point test, FTIR, 1H NMR, 13C NMR and MS. |
Key words:2,3-butanedione; acetaldehyde; ozonization |
|
基金项目:江苏省自然科学基金(BK20130420),江苏省博士后科研资助计划(2018K152C)。
|
作者简介:何 磊(1980-),男,江苏淮安人,讲师,博士,主要从事精细化工研究(E-mail:heleihuaina@hyit.edu.cn)。
|
收稿日期:2019-04-09
|
|