摘要
利用中心组合设计试验选取炭化温度、磺化温度和磺化时间3个因素对龙竹碳基固体酸催化剂的催化性能影响,运用响应面法对其工艺参数进行优化,并利用SEM和FT-IR对催化剂进行表征。研究结果表明,根据试验数据建立的二次多项式数学模型具有高度显著性(P<0.0001),相关系数R2=0.9807,说明预测值和试验值之间具有很好的拟合度。通过对二次回归数学模型解逆矩阵得到制备竹炭基固体酸催化剂的最优化条件为:炭化温度为228.57℃,磺化温度为80℃,磺化时间为6.64h。在此条件下获得的碳基固体酸催化剂催化混合脂肪酸和甲醇酯化反应转化率的预测值为89.46%,试验值为89.98%,二者的相对偏差为0.58%,说明用此模型来分析和预测炭基固体酸催化剂的催化性能是可行可靠的。竹炭基固体酸催化剂的SEM和FT-IR分析表明,催化剂表面具有多孔型框架结构,空隙中含有呈片状或层状结构的无定型碳颗粒,催化剂分子结构上含有催化活性基团-SO3H基团。
The effect of carbonation temperature, sulfonation temperature and sulfonation time on the catalytic prop- erties of arbon-based solid catalyst were investigated by Box-Behnken design experiment. The technologic parameters were optimized with response surface methodology（RSM）. And the catalyst was characterized by SEM and FT-IR. The results showed that it was highly significant（P〈0. 0001）that the quadratic regression mathematics model established according to experimental data,which the coefficient of correlation was R2 =0. 9807. This illustrated that degree of fitting was provided with between the predicted value and the experimental value. The optimum technologic parameters were obtained through inverse matrix of quadratic regression mathematics model,which was by following： the carbonation temperature was 228. 57℃, the sulfonation temperature was 80℃ and the sulfonation time was 6.64h. Under these conditions, the predicted value that the convert ratio of esterification with mixed fatty acid and methyl catalyzed by the catalyst was 89.46%o while the ex- perimental value was 89.98% ,which the relative deviation between them was 0. 58%. Therefore, it was feasible and reliable that RSM was used to optimize the technologic parameters of catalytic properties of the catalyst. The SEM and FT-IR indi cated that the catalyst had many pass frame structure on surface, the amorphous carbon particles of sheet or layered struc- ture in interspaees and the -SO3 H of catalytic active group in molecular structure of the catalyst.
出处
《化工新型材料》
CAS
CSCD
北大核心
2013年第12期152-155,共4页
New Chemical Materials
基金
云南省教育厅基金重点项目(2001Z023)
国家科技支撑计划项目(2007BAD32B03)
关键词
碳基固体酸
响应面法
表征
酯化反应
carbon-based solid catalyst,response surface methodology, characterization, esterification
