磷石膏催化合成缩醛(酮)

Synthesis of acetals(ketals) catalyzed by phosphogypsum

以磷石膏(PG)为催化剂催化合成缩醛(酮)。考察了醇酮摩尔比、催化剂用量、反应时间、带水剂种类及用量、催化剂重复使用次数等因素对合成环己酮乙二醇缩酮的影响,研究了PG催化合成12种缩醛(酮)的催化活性。实验结果表明,在PG用量为环己酮的7.5%(w)、醇酮摩尔比为1.5、环己烷16 m L、反应时间2.5 h的条件下,PG催化合成环己酮乙二醇缩酮的产率可达99.9%以上;PG重复使用8次后,环己酮乙二醇缩酮产率仍达98.5%以上;在12种缩醛(酮)的制备反应中PG均表现出优良的催化性能,PG具有环境友好型固体酸催化剂的潜质,有望实现磷酸工业副产的回收利用和资源化处理。

The synthesis of acetals（ketones） catalyzed by phosphogypsum（PG） was explored. The effects of the mole ratio of ethylene glycol to cyclohexanone,catalyst dosage,reaction time,watercarrying agents,cyclohexane dosage and catalyst reuse times on the yields of cyclohexanone glycol ketal were investigated. The results showed that the yield of cyclohexanone glycol ketal reached 99.9%under the conditions of catalyst dosage 7.5%（w）, mole ratio of ethylene glycol to cyclohexanone 1.5,cyclohexane 16 m L and reaction time 2.5 h. After PG was reused 8 times,the yield of cyclohexanone glycol ketal still reached 98.5%. The catalytic activities of PG in the syntheses of 12 acetals（ketones） were studied. PG indicated excellent catalytic performances for the synthesis of the 12 acetals（ketones） and was a environmentally friendly solid acid catalyst for the utilization of the byproduct PG from phosphate industry.