李慧 胡远卓 徐琼

摘 要 以竹加工业副产物竹粉为原料，利用磷酸活化-微波炭化法制备新型炭基固体磺酸催化剂.设计正交试验考察竹粉与磷酸固液比、磷酸浓度、微波功率与微波时间对所制备的炭基固体磺酸样品中的磺酸量的影响.结果表明：新型炭基磺酸催化剂适宜的制备条件为：固液比为1∶6，磷酸质量分数为40%，浸渍时间12 h，微波功率为800 W，微波时间为20 min.催化剂在合成环己酮乙二醇缩酮的反应中表现出优良的催化活性和重复使用性.与传统的炭化方法相比，磷酸活化-微波炭化法具有加热快、效率高、能耗低、生产周期短等优点.

关键词 炭基磺酸；微波炭化法；生物质转化；缩酮

中图分类号 TQ352文献标识码 A文章编号 1000-2537（2017）06-0061-05

Abstract A novel char sulfonic solid acid catalyst was prepared by using phosphoric acid activated-microwave carbonization method using waste bamboo powder as the raw material.The impact of the ratio of solid to liquid， concentration of phosphoric acid， microwave power and time on the amount of sulfonic acid consumed in the carbon-based solid sulfonic acid samples were thoroughly investigated by the orthogonal design.Our results showed that the optimal preparation conditionis are as follows： the solid-liquid ratio was 1∶6， the volume fraction of phosphoric acid was 40%， dipping time 12 h， microwave power 800 W， and microwave time 20 mins. This catalyst showed excellent catalytic activities and reusability in the synthesis of cyclohexanone ethylene ketal. Compared with the conventional carbonization method， our phosphoric acid activated-microwave carbonization method has following advantages： fast heating， high efficiency， low energy consumption， and short production cycle.

Key words char sulfonic acid； microwave carbonization； biomass conversion； ketal

我國拥有十分丰富的农林废弃物，年产量达到亿吨以上[1]，农林废弃物一直是制备活性炭的廉价原料.微波加热通过被加热体内部偶极分子高频往复运动，产生“内摩擦热”而使被加热物料温度升高，不须任何热传导过程就能使物料内外部同时加热升温，加热速度快且均匀，热利用率高[2-8].因此近十年来利用微波加热的方式得到了广泛应用[9-10].以可再生生物质资源为原料，经炭化、磺化后制备的炭基磺酸催化剂具有高酸量高催化活性[11-18]，在酯化[16-17]、水解[18-19]等各类酸催化反应中都表现出优异的催化性能.文献报道的炭化方法多采用传统的热解炭化法或水热炭化法[20]，尚未见采用微波炭化方法制备此类催化剂的报道.

基于微波炭……