硫酸氢钠掺杂聚苯胺催化合成环己酮缩乙二醇

以聚苯胺PAn和硫酸氢钠为原料,制备了硫酸氢钠掺杂率为20%(质量分数)的催化剂PAn-NaHSO4,并用于催化合成环己酮缩乙二醇,探讨了PAn-NaHSO4的催化活性,系统考察了醇酮摩尔比、催化剂用量、反应时间和带水剂用量对环己酮缩乙二醇收率的影响,并且用正交试验对反应条件进行了优化。在环己酮用量为0.1 mol,n(乙二醇)∶n(环己酮)=1.6∶1,催化剂用量占反应物总质量的1.2%,带水剂环己烷用量为9 mL,反应时间为2.5 h的条件下,产品收率可达96.79%,产品经红外光谱、气-质联用定性分析确定为环己酮缩乙二醇,经气相色谱检测纯度大于99.0%,催化剂重复使用5次后,产品收率仍大于90.0%。

Catalytic synthesis of cyclohexanone ethylene ketal by polyaniline doped with sodium hydrogen sulfate

Cyclohexanone ethylene ketal was synthesized from cyclohexanone and ethylene glycol as starting materials using polyaniline(PAn) doped with 20%(mass fraction) of sodium hydrogen sulfate(PAn-NaHSO4) as catalyst.Catalytic activity of PAn-NaHSO4 was investigated.Effect of factors such as mole ratio of ethylene glycol to cyclohexanone,dosage of the catalyst,reaction time,dosage of water stripping agent on product yield were examined systematically and optimum reaction conditions were identified by orthogonal designed experiment.Under optimal conditions:based on amount of cyclohexanone 0.1 mol,mole ratio n(ethylene glycol)∶ n(cyclohexanone)=1.6∶ 1,mass fraction of PAn-NaHSO4 1.2% of the total reactants,water stripping agent cyclohexane 9 mL and reaction time 2.5 h,yield of the product achieves 96.79%.The product was identified as cyclohexanone ethylene ketal by IR and GC-MS.Purity of product achieves 99.0%.After reusing the catalyst for 5 times,yield of the product is still higher than 90.0%.