生物质碳磺酸催化合成双酚酸

Synthesis of diphenolic acid catalyzed by biomass carbon sulfonic acid

双酚酸用于制备可降解双酚酸型高分子材料,但双酚酸合成所使用的催化剂有不足之处。采用一步水热炭化磺化法,将核桃壳和对甲苯磺酸等质量混合制备生物质碳磺酸。采用扫描电镜(SEM)、红外光谱(FTIR)、氨气吸附脱附(NH 3-TPD)和热重(TGA)对其结构分别进行分析。以生物质碳磺酸为催化剂,催化乙酰丙酸和苯酚缩合成双酚酸。考察了反应条件(催化剂用量、物料摩尔比、反应温度、反应时间)的变化对双酚酸产率的影响。试验表明在催化剂用量10%、n(苯酚):n(乙酰丙酸)4∶1、反应温度120℃、反应时间24 h的最佳条件下,双酚酸的产率可以达到92.4%。结构表明其在催化循环5次后,双酚酸的产率仍保持在80%以上,说明该催化剂的催化活性和稳定性较高。

Diphenolic acid is used to synthesize the degradable bisphenol acid-type polymer.However,the used catalysts for the synthesis of diphenolic acid were some defects.The biomass carbon sulfonated acid was prepared by mixing the nutshell and p-toluene sulfonic acid with the same mass using one-step hydrothermal charring and sulfonation.Its structure was characterized by scanning electron microscope(SEM),infrared analysis(FT-IR),ammonia adsorption desorption(NH 3-TPD)and thermogravimetric analysis(TGA).Then it was applied for the preparation of diphenolic acid with levulinic acid and phenol condensation.And the effects of reaction conditions on yield of diphenolic acid were investigated,such as catalyst dosage,molar ratio of raw materials,reaction temperature and reaction time.The results show that the optimal condition is 10%of catalyst dosage,4∶1 of molar ratio of phenol to levulinic acid,120℃of reaction temperature and 24 h of reaction time.The yeild of diphenolic acid comes up to 92%under the optimal reaction condition.The result show that the yield of diphenolic acid keeps at beyond 80%after 5 cycles.The biomass carbon sulfonated acid has high catalytic activity and stability.