摘要
研究了以乙酰丙酸(LA)和苯酚为原料,盐酸为催化剂,巯基乙酸为助催化剂合成4,4’-双(4’-羟苯基)戊酸的工艺。考察了助催化剂种类及用量、反应物料配比、反应温度、反应时间和催化剂用量等因素的影响。通过正交试验,优化了合成工艺。试验表明:n(苯酚)∶n(LA)(摩尔比)=4∶1,反应温度60℃,反应时间为45 h,n(HCl)∶n(LA)=4∶1时,最高产率为97.1%。产物结构经红光外光谱、氢核磁谱进行了表征确定为4,4’-双(4’-羟苯基)戊酸。
4,4'-Bis(4'-hydroxyphenyl)-pentanoic acid was synthesized using levulinie acid and phenol as raw materials. Hydrochloric acid and mercaptoacetic acid were used as catalyst and assistant catalyst respectively. The effects of assistant catalyst, molar ratio of the raw materials, reaction temperature, reaction time and catalyst on the reaction were studied and the conditions were optimized by orthogonal experiments. When the molar ratio of phenol to levulinic acid was 4 : 1, reaction temperature was 60 ℃, reaction time was 45 h and molar ratio of HCl to levulinic acid was 4 ; 1, The yield of the product was 97.1%. From IR and ^1H NMR results, the product was validated as 4,4'-bis(4'-hydroxyphenyl)-pentanoic acid.
出处
《化学世界》
CAS
CSCD
北大核心
2006年第5期293-295,共3页
Chemical World
基金
河南省教育厅自然科学研究计划项目资助(200510459056)
关键词
乙酰丙酸
双酚酸
合成
高分子材料
levulinic acid
diphenolic acid
synthesis
polymer material