摘要
在2,6-萘二磺酸钠碱熔反应中加入助流剂X,合成2,6-二羟基萘。用甲醇、丙酸、水、碳酸钠的混合溶液对2,6-二羟基萘粗品进行精制,得到高纯度、高收率的2,6-二羟基萘。最佳工艺条件为:2,6-萘二磺酸钠、Na OH、KOH的质量比为1∶2.4∶2.0,混合碱与助流剂X质量比为10∶1,通入氮气,在340~350℃之间反应1 h,收率在90%左右。2,6-二羟基萘粗品与甲醇、丙酸、水按质量比1∶1.5∶1.5∶1.5混合,2,6-二羟基萘粗品与碳酸钠质量比为200∶3,经精制提纯产品纯度达到98%以上,收率在66%以上。
2,6-Dihydroxynaphthalene is synthesized by adding flow aiding agent X during the alkaline fusion of disodium 2,6-naphthalenedisulfonate. The mixed solvent of methanol,propionic acid,water and sodium carbonate is used to refine the crude product of 2,6-dihydroxynaphthalene. High purity and yield of the product can be obtained under the following alkaline fusion technical conditions： 1∶ 2. 4∶ 2. 0 mass ratio of 2,6-naphthalenedisulfonate,Na OH and KOH,10∶1 mass ratio of mixed alkaline and flow aiding agent X,340-350℃ of reaction temperature,1 hour of reaction time under N2. The yield of crude 2,6-dihydroxynaphthalene is about 90%. When the ratio of the crude 2,6-dihydroxynaphthalene,methanol,propionic acid and water is 1∶ 1. 5∶ 1. 5∶ 1. 5,the mass ratio of the crude 2,6-dihydroxynaphthalene and sodium carbonate is 200∶ 3,the purity of refined product is up to 98% and the yield is about 66%.
出处
《现代化工》
CAS
CSCD
北大核心
2017年第2期102-106,共5页
Modern Chemical Industry
基金
国家自然科学基金(21276187)
天津市自然科学基金(16JCYBJC20800)
天津市科技创新平台计划(14TXGCCX00017)
关键词
碱熔
2
6-二羟基萘
助流剂X
2
6-萘二磺酸钠
alkali fusion
2
6-dihydroxynaphthalene
flow aiding agent X
disodium 2
6-naphthalenedisulfonate
