磺化椰壳炭固体酸催化剂的制备及催化酯化反应研究

Preparation of sulfonated coconut shell activated carbon solid acid catalyst and applied in esterification

以海南椰壳纤维为原料,采用浸渍法活化、管式炉炭化等过程制备椰壳活性炭,然后以浓硫酸为磺化剂,磺化制备了具有多孔特征的椰壳炭固体酸。并对制得的椰壳炭固体酸进行了结构表征。通过乙酸和正丁醇的酯化反应,对催化剂的性能进行了测试,考察了催化剂制备过程中物料比、灼烧温度、炭化时间、磺化剂用量等因素对催化反应的影响。结果表明:在椰壳纤维原料与活化剂氢氧化钾的质量配合比为1∶1,炭化温度为450℃,炭化时间为2h,椰壳活性炭与磺化剂投量配合比为1g∶20mL,磺化时间为2h条件下,制得的磺化椰壳固体酸的催化性能最好,并在催化乙酸与正丁醇的酯化反应中2h转化率达到96.6%。

Carbon-based solid acid catalysts were prepared by sulfonation of porous coconut shell carbon which was prepared from coconut shell fiber by impregnation-activation and calcination in tube furnace.The structures of the solid acids were characterized by IR,XRD,SEM and so on.The performance of catalysts were verified by esterification of acetic acid and n-butanol,and the effects of the procedure such as material ratio,calcination temperature,calcination time,amount of sulfonating agent and sulfonation time on the esterification were investigated.It's shown when the ratio of coconut shell fiber material and activator KOH was 1∶1,the carbonization temperature of 450℃,the calcination time was 2h,the coconut shell activated carbon with a sulfonating agent dosage was 1g∶20mL,sulfonation time was 2h,the conversion rate in the catalytic esterification of acetic acid and butanol reached 96.6%.