临氢烷基化“一锅法”制备二甲基异丙基胺

全文下载： 202101004.pdf

文章编号： 16726987（2021）01002806； DOI： 10.16351/j.16726987.2021.01.004

杨凯欣， 刘仕伟， 于世涛*(青岛科技大学 化工学院，山东 青岛 266042)

摘要： 以价廉易得的二甲胺和丙酮为原料，采用临氢烷基化“一锅法”制备二甲基异丙基胺，考察了物料配比、催化剂种类、氢气压力、反应温度和反应时间等因素对反应结果的影响，得到较佳反应条件，即：二甲胺(质量分数33%水溶液)981 g、n(二甲胺)∶n(丙酮)=10∶12、催化剂Pd/C(质量分数5%)003 g、p(H2) 40 MPa、反应温度110 ℃、反应时间10 h，在该条件下，二甲胺转化率可达984%，目标产物选择性达893%。反应混合物精馏分离制产品的研究结果表明：二甲基异丙基胺和丙酮存在最低共沸点(共沸温度53 ℃，共沸物组成依次为30%和70%)；精馏过程共有三组馏分采出，其中，塔顶物料温度65 ℃、回流比3∶1~5∶1条件下，得到产品二甲基异丙基胺的纯度和收率分别为998%和78%。

关键词： 丙酮； 二甲胺； 二甲基异丙基胺； 加氢； 催化

中图分类号： TQ 226.3文献标志码： A

引用格式： 杨凯欣， 刘仕伟， 于世涛. 临氢烷基化“一锅法”制备二甲基异丙基胺［J］. 青岛科技大学学报(自然科学版), 2021, 42(1): 2833.

YANG Kaixin, LIU Shiwei, YU Shitao. Onepot synthesis of dimethylisopropylamine via hydroalkylation reaction［J］. Journal of Qingdao University of Science and Technology（Natural Science Edition), 2021, 42(1): 2833.

Onepot Synthesis of Dimethylisopropylamine via Hydroalkylation ReactionYANG Kaixin, LIU Shiwei, YU Shitao

(College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China)

Abstract: In this paper, dimethylisopropylamine was synthesized by using "onepot" of hydroalkylation method. Dimethylamine and acetone, for its inexpensive and readily available quality, were used as raw materials. The influence of the factors including raw material ratio, the type of catalyst, hydrogen pressure, reaction temperature and reaction time were examined, and the optimal conditions for the synthesis of the target product were obtained. The optimum reaction conditions were as follows: dimethylamine (33% aqueous solution) 9.81 g, n(dimethylamine)∶n(acetone)= 1.0∶1.2, Pd/C (5%) catalyst 0.03 g, p(H2)=4.0 MPa, reaction temperature 110 ℃ and reaction time 1.0 h. Under these conditions, the conversion of dimethylamine was 98.4%, and the selectivity of the target product was 89.3%. The results of research on the separation and distillation of reaction mixtures showed that dimethylisopropylamine and acetone have the lowest azeotropic point (azeotropic temperature is 53 ℃, azeotrope composition is 30% and 70% respectively). A total of three groups of fractions were produced during the rectification process. Among them, under the conditions of a temperature of 65 ℃ at the top of the column and a reflux ratio of 3∶1—5∶1, the purity and yield of the product dimethylisopropylamine were 99.8% and 78%, respectively. The above research results can provide useful guidance for the industrial synthesis of dimethylisopropylamine.

Key words: acetone; dimethylamine; dimethylisopropylamine; hydrogenation; catalysis

收稿日期：  20200225

作者简介： 杨凯欣(1994—)，女，硕士研究生.*通信联系人.