酸性阳离子交换树脂催化制备6,6'-二羟基-3,3,3',3'-四甲基-1,1'-螺二氢茚的工艺研究  

Preparation technology of 6,6'-dihydroxy-3,3,3',3'-tetramethyl-1,1'spirobiindane with acid cation exchange resin as catalyst

作　　者：许平[1] 陈群[1] 何明阳[1] 孙富安[1] 张益峰[1] 

机构地区：[1]常州大学石油化工学院,江苏常州213164

出　　处：《化工进展》2012年第8期1741-1744,1827,共5页Chemical Industry and Engineering Progress

摘　　要：利用双酚A结晶残液为原料,以磺化聚氯代苯乙烯-二乙烯基苯强酸性阳离子交换树脂为催化剂,通过固定床连续催化制备6,6'-二羟基-3,3,3',3'-四甲基-1,1'-螺二氢茚。反应器中装填50mL(22 g,E=1.8 mmol H+/mL)干树脂,在T=150℃、WHVS=0.48 h-1条件下,连续反应1000 h,反应液中6,6'-二羟基-3,3,3',3'-四甲基-1,1'-螺二氢茚质量浓度可达43.5%,催化剂交换量保持为3.8 mmol/g。产物经重结晶纯化后熔点215～217℃,纯度≥99.98%(HPLC)。通过HPLC、IR、NMR等方法分析产物含量及结构,用STATISTIC统计软件对反应条件进行了优化。研究结果对于改进双酚A生产工艺中的残液处理方式,填补国内在新型双酚类单体生产空白具有重要的意义。In this paper,a new preparation method of a continuous fixed-bed catalytic system for 6,6’-dihydroxy-3,3,3’,3’-tetramethyl-1,1’-spirobiindane was reported with bisphenol A crystalline residue solution as raw material,and sulfonated polyvinyl generation of styrene-divinylbenzene strong acid cation exchange resin as catalyst.Stainless steel reactor with ？30 mm was filled by 50 mL（22g,E = 1.8 mmol H＋/mL） dry resin.In the condition of T =150 ℃,WHVS = 0.48h-1,it had reacted continuously for 1000 h,the concentration of 6,6 ’-dihydroxy-3,3,3’,3’-tetramethyl-1,1’-spirobiindane in reaction solution was stabilized at 43.5%,and the exchange capacity of catalyst remained 3.8 mmol/g.Product was purified by recrystallization,and the melting point was 215—217 ℃,purity was≥ 99.98%（HPLC）.By HPLC,IR,NMR and other methods for the analysis of product content and structure,reaction conditions were optimized with a statistical software STATISTIC.The results for the improvement on the production process of bisphenol A residue treatment suggest a brand new method for bisphenol monomer production.

关 键 词：6 6’-二羟基-3 3 3’ 3’-四甲基-1 1’-螺二氢茚 双酚A 固定床连续催化 

分 类 号：TQ322.4[化学工程—合成树脂塑料工业]