丙烯醛水合加氢制1,3-丙二醇

PREPARATION OF 1,3-PROPANEDIOL BASED ON HYDRATION OF ACROLEIN WITH SUBSEQUENT HYDROGENATION

考察了丙烯醛水合及 3 羟基丙醛加氢制 1,3 丙二醇的工艺条件。在装有阳离子交换树脂催化剂的固定床层反应中 ,当水合温度 4 0～ 5 5℃、空速 3～ 5h-1、丙烯醛质量分数 13 %～ 17% ,并加入少量对苯二酚阻聚剂时 ,丙烯醛单程转化率可达到 85 % ,选择性大于 90 %。在高压釜内进行 3 羟基丙醛加氢时 ,催化剂投料量 1.5 %～ 2 .0 % ,一段加氢温度 3 0～ 5 0℃ ,二段加氢温度 110～13 0℃ ,氢气压力 6.0MPa ,搅拌速度 5 0 0r/min ,使用细颗粒Raney镍催化剂 ,可使 3 羟基丙醛加氢转化率达到 10 0 % ,1,3 丙二醇的选择性也在 99%以上 ,在产品中醛基含量小于 3 0 0 μg/g。

The studies on preparation of 1,3 propanediol by hydration of acrolein and hydrogenation of 3 hydroxypropionaldehyde (3 HPA) were carried out. The conversion of hydration of acrolein was higher than 85%, and the selectivity to 3 HPA was above 90% in the presence of acidic ion exchange resin at a reaction temperature of 40-55 ℃ , a weight space velocity of 3-5 h -1 , and an acrolein concentration of 13%-17% carried in a fixed bed reactor. With Raney nickel catalyst, the carbonyl content in the product was reduced to less than 300 μg/g with hydrogenation of 3 HPA in an autoclave at a stirred rate of 500rpm. The reaction temperatures for the overall hydrogenation in stage 1 and stage 2 were 30-50 ℃ and 110-130℃ respectively, the hydrogen pressure was 6.0MPa, and the catalyst concentration was 1.5%-2%. The conversion and 1,3 propanediol selectivity of hydrogenation were 100% and higher than 99% respectively.