高校化学工程学报Issue(1)：92-97,6.DOI:10.3969/j.issn.1003-9015.2014.01.014
1,2-戊二醇的新合成方法及工艺优化研究
Study on the New Synthetic Method of 1,2-Pentanediol and Process Optimization Thereof
摘要
Abstract
A new feasible synthetic route for the synthesis of 1,2-pentanediol was designed and optimized in this paper with butyraldehyde and paraformaldehyde as the starting material. The effects of feed ratio, reaction temperature, catalyst dosage and reaction pressure on the yield of product were studied. The reaction was divided into two steps. The first step, using 3-ethyl benzothiazole bromide as catalyst, the intermediate product 1-hydroxy-2-pentanone was synthesized by cross-acyloin condensation between n-butyraldehyde and paraformaldehyde. The optimum condition is: n (butyraldehyde): n (paraformaldehyde) =1:1.5, n (butyl aldehyde):n (catalytic agent)=1:0.1, temperature 70℃, the average yield obtained by six repeated experiments is 56.6%. In the second step, the final product 1,2-pentanediol was synthesized with hydrogenation reduction of 1-hydroxy-2-pentanone by using Pd/C as catalyst. The optimum condition is: Pd/C catalyst dosage 3.5%( relative to the 1-hydroxy-2-pentanone quality ), hydrogen pressure 1.5 MPa, temperature 55℃, the average yield obtained by six repeated experiments is 91.6%. Total yield of two steps is 51.8%, the cost of material is only 40,000 yuan/ton. The structures of product were analyzed and characterized by IR, 1H-NMR, MS. This process has advantages of easy available raw material, simple technology with mild reaction conditions, high content of the product and suitable for industrialized production.关键词
1,2-戊二醇/1-羟基-2-戊酮/交叉偶姻缩合/催化加氢Key words
1,2-pentanediol/1-hydroxy-2-pentanone/cross-benzoin condensation/catalytic hydrogenation分类
化学化工引用本文复制引用
徐保明,唐强,罗岩,程乾,陈坤..1,2-戊二醇的新合成方法及工艺优化研究[J].高校化学工程学报,2014,(1):92-97,6.基金项目
湖北省自然科学基金重点项目(2010CDA020)；湖北省教育厅科研项目(D20111402)。 （2010CDA020）
