化学工程2017,Vol.45Issue(9):52-57,6.DOI:10.3969/j.issn.1005-9954.2017.09.010
磺化碱熔法制备2,5-二甲基苯酚
Preparation of 2,5-xylenol by sulfonation and alkali fusion
摘要
Abstract
2,5-Xylenol was synthesized by sulfonation and alkali fusion using p-xylene as the starting material.Some factors influencing the yield and purity of the product in the sulfonation and alkali fusion were studied.By recycling and reusing the acidic filtrate in sulfonation the acid wastewater and the cost were reduced.The optimal sulfonation conditions:sulfuric acid was added to p-xylene slowly,the molar ratio of sulfuric acid and p-xylene 1.6 ∶ 1,reaction temperature 125 ℃,reaction time 2.0 h.The molar yield of sodium 2,5-xylenesulfonate is 96.87%,and the purity is 99.30%.In the alkali fusion,water vapor,sodium stearate and antioxidant were added in order to avoid overoxidation and increase the flow of materials,and improve the yield and purity.The optimal alkali fusion conditions:KOH,NaOH,wet sodium salt,antioxidant 1035 and sodium stearate are mixed into a reaction vessel,the mass ratio of NaOH and KOH 3 ∶ 2,antioxidant 1035 4 g,sodium stearate 9 g,reaction temperature 330-340 ℃,reaction time 2.0 h.The molar yield of 2,5-xylenol in the alkali fusion is 92.70%,and the purity is 99.45 %.关键词
2,5-二甲基苯磺酸钠/2,5-二甲基苯酚/磺化/碱熔/抗氧剂/硬脂酸钠Key words
sodium 2,5-xylenesulfonate/2,5-xylenol/sulfonation/alkali fusion/antioxidant/sodium stearate分类
化学化工引用本文复制引用
李彬,杨冬,张天永,宋良,袁仲飞..磺化碱熔法制备2,5-二甲基苯酚[J].化学工程,2017,45(9):52-57,6.基金项目
国家自然科学基金资助项目(21276187) (21276187)
天津市自然科学基金(16JCYBJC20800) (16JCYBJC20800)
天津市科技创新平台计划(14TXGCCX00017) (14TXGCCX00017)