以稻草水解残渣为原料,经减压热解炭化和发烟硫酸磺化制备出了新型固体酸稻草炭磺酸.炭化是从室温以10℃/m in升温到150℃,恒温3 h;磺化按1∶10的炭酸质量比加入发烟硫酸(50%SO3),在80℃下恒温3h,制得的稻草炭磺酸的酸量达到2.0 mmol/g.稻草炭磺酸在甘油缩环己酮反应中表现出了良好的催化活性.在环己酮用量0.10 mol,丙三醇0.12 mol,催化剂用量10 mg,带水剂环己烷15 mL,反应2.5 h,环己酮转化率达99.3%,并以良好的稳定性而可重复使用.
As a novel solid acid,rice straw char sulfonic acid was prepared using the residues in sulfuric acid hydrolysis of rice straw as raw material,via decompression charring and sulfonating by oleum.Charring was operated by heating from room temperature to 150 ℃ at 10 ℃/min,then maintained for 3 h.Sulfonating was conducted at 80 ℃ for 3 h at mass ratio of char to oleum being 1∶10.The acid capacity of rice straw char sulfonic acid was 2.0 mmol/g.Rice straw char sulfonic acid showed excellent catalytic performance in condensation of glycerol with cyclohexanone.When the amount of cyclohexanone was 0.10 mol,glycerol was 0.12 mol,catalyst was 10 mg,15 mL cyclohexane was used as water-carrying agent in the process,the conversion percent of cyclohexanone came up to 99.3% after reacting for 2.5 h.The catalyst can be reused and have good stability.