碘催化合成1,3-丙二醇缩环己酮

Catalytic Synthesis of Cyclohexanone 1,3 - Propanediol Ketal by Iodine

研究了单质碘催化环己酮与1,3-丙二醇的缩酮化反应,考察了反应时间、醇酮摩尔比、催化剂质量、带水剂体积等因素对1,3-丙二醇缩环己酮收率的影响。结果表明,单质碘有着较好的催化活性,在回流条件下,当环己酮的物质的量为0.1 mol,醇酮摩尔比为1.2,催化剂质量为0.052 g(约占反应体系总摩尔分数的7.0×10-5),带水剂环己烷体积为8 mL,反应30 min后,缩酮收率可达到81.6％,且所得产品无色透明,纯度大于99％。合成反应条件温和,催化剂用量小,操作简便,后处理过程简单,无三废产生。产品经折射率、红外光谱和气相色谱进行了表征。

The ketalization of cyclohexanone and 1,3 - propanediol ketal catalyzed by I2 was studied. The effects of reaction time, molar ratio of 1,3 - propanediol and cyclohexanone, catalyst amount and the volume of water- carrying agent on the yield of cyclohexanone 1,3 - propanediol ketal were investigated. The results show that I2 has a good catalytic activity. The most suitable condition for the reaction are as follows: when the amount of cyclohexanone is 0. 1 mol, molar ratio of 1,3 - propanediol and cyclohexanone is 1.2, molar ratio of catalyst to reactant is about 7.0×10-5, cyclohexane as the water - carrying agent is 8 mL, reaction time is 30 min. The yield is up to 81. 6% . The product is colorless and transparent, the purity is over 99% . Under the mild reaction condition, the three wastes could not be produced with easy manipulation, simple after- treatment and low catalyst amount. The product was characterized by refractive index, IR and GC.