| 摘要: |
| 【目的】研究确定利用提取皂甙后的黄姜皂素废渣制备乙酰丙酸的最佳条件。【方法】在常压下，采用酸催化方法，首先利用单因素试验分别探讨了不同催化酸种类、催化酸体积分数、反应温度、反应时间、液固质量比和黄姜皂素废渣粒度对乙酰丙酸产率的影响。在单因素试验的基础上，采用Box-Behnken中心组合设计，选用硫酸体积分数、反应时间、液固质量比和废渣粒度进行4因素3水平试验，对黄姜皂素废渣制备乙酰丙酸的工艺条件进行了优化。【结果】单因素试验表明，在反应温度为100 ℃、硫酸体积分数为4%、液固质量比为12∶1、反应时间为10 h、黄姜皂素废渣粒度为0.84 mm的条件下，乙酰丙酸产率最高，可达18.31%。对多因素试验数据进行拟合后，得到生产乙酰丙酸的最佳工艺条件为：硫酸体积分数4.5%,反应时间12.5 h,液固质量比18∶1,黄姜皂素废渣粒度0.25 mm，在此条件下，乙酰丙酸的理论产率可达20.67%。【结论】硫酸体积分数、反应时间和液固质量比是影响黄姜皂素废渣水解的主要因素，黄姜皂素废渣粒度（0.15～0.84 mm）对乙酰丙酸产率的影响不大。 |
| 关键词: 黄姜皂素废渣 乙酰丙酸 酸催化水解 工艺条件优化 |
| DOI： |
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| 基金项目:国家环保示范项目（财建［2004］278号） |
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| Experimental studies for levulinic acid production from diosgenin solid waste |
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| Abstract: |
| 【Objective】The studies were carried out to explore the conditions of levulinic acid from diosgenin solid waste.【Method】By using single factor experiment method,the acid catalysis was used to detect the effects of catalytic acid,acid volume fraction,reaction temperature,reaction time,liquid-solid ratio and granularity on levulinic acid production from diosgenin solid waste at atmospheric pressure.Based on this,response surface experiments design by Box Behnken of four factors and three levels was conducted to obtain the optimized process conditions.The four factors were sulfuric acid volume fraction,reaction time,liquid solid ratio and granularity.【Result】Single factor experiment indicated that the maximum yield of 18.31% levulinic acid was achieved at 4% sulfuric acid volume fraction,12∶1 of liquid-solid ratio,10 h of reaction time and 0.84 mm of granularity in 100 ℃ water-bath temperature.Data fitting of multiple factor experiment indicated that theoretical yield of 20.67% was obtained at 4.5% sulfuric acid volume fraction,18∶1 of liquid solid ratio,12.5 h of reaction time and 0.25 mm of granularity in 100 ℃ water-bath temperature.【Conclusion】Sulfuric acid volume fraction,reactive time and liquid-solid ratio were main factors for hydrolysis of diosgenin solid waste,and the granularity in the range of 0.15-0.84 mm had little influence. |
| Key words: diosgenin solid waste levulinic acid acid catalysis process condition optimization |
