摘要
以甘蔗糖蜜为原料、硫酸为催化剂,催化水解制备了乙酰丙酸（levulinic acid,LA）,以LA得率（水解液中LA占甘蔗糖蜜中转化糖的质量百分数,下同）为指标,在单因素实验基础上,考察了反应时间、甘蔗糖蜜的质量分数（占反应原料质量,下同）、甘蔗糖蜜与硫酸的质量比、反应温度的影响。采用Box-Benhnken中心组合实验原理和响应面分析法（RSM）对乙酰丙酸制备条件进行了优化。结果表明：建立的二次多项式模型回归性显著而失拟项不显著,模型拟合性良好。各因素对LA得率均有显著性影响,按影响程度从大到小依次为：甘蔗糖蜜与硫酸的质量比〉反应温度〉反应时间〉甘蔗糖蜜的质量分数。实验最终确定乙酰丙酸最佳制备条件为：反应时间5 h、w（甘蔗糖蜜）=40%、m（甘蔗糖蜜）/m（硫酸）=23.40、反应温度151℃。在该条件下进行了3次重复实验,LA得率平均值为30.11%,与预测值30.96%相对偏差0.85%,模拟可靠。
In the process of production of levulinic acid （LA） by sulfuric acid catalytic hydrolysis of cane molasses, the effects of reaction time, mass ratio of molasses to raw material, mass ratio of molasses to catalyst and reaction temperature on the LA yield （ the mass ratio of target product LA to invert sugar in sugarcane molasses, the same below ） were investigated based on single-factor experiments. Box- Benhnken center combination experimental principle and response surface methodology （RSM） were adopted to optimize the preparation conditions of LA. A quadratic polynomial regression model was established to predict LA yield. The results showed that the regression of this model was significant while the lack of fit was not significant, which indicated the model fitted well with experimental data. All factors could significantly influence the LA yield, and the order of importance was mass ratio of molasses to catalyst 〉 reaction temperature 〉 reaction time 〉 mass ratio of molasses to raw materials. The optimal conditions for the preparation of LA were obtained as follows：mass fraction of molasses 40% ,mass ratio of molasses to sulfuric acid 23.40,reaction temperature 151 ℃ and reaction time 5 h. Under these conditions,three repeated experiments were carried out,and the average value of LA yield reached 30. 11%. Compared with the predicted value of 30.96%, the relative deviation was only 0. 85% ,which proved the model was reasonable and feasible.
作者
宋道君
陆小芳
徐勇军
涂伟萍
廖俊旭
SONG Dao-jun1, LU Xiao-fang1 ,XU Yong-jun2. , TU Wei-ping1, LIAO Jun-xu2(1. School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510641, Guangdong, China;2. School of Chemical Engineering and Energy Technology, Dongguan University of Technology, Dongguan 523808, Guangdong, China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2018年第4期612-619,共8页
Fine Chemicals
基金
国家自然科学基金(51476036)~~
关键词
甘蔗糖蜜
乙酰丙酸
催化水解
响应面分析
中心组合实验
cane molasses
levulinic acid
catalytic hydrolysis
response surface methodology
center
