摘要
以1,4-二氧六环为溶剂,NaOH为催化剂,对废弃的含4,4'-联苯二酚(BP)单元的芳香族聚酯型液晶高分子(LCP),在常压下通过水解反应回收制备4,4'-联苯二酚进行了研究。在反应混合物的质量比m(LCP)∶m(溶剂)∶m(H2O)∶m(NaOH)=1∶4∶1.5∶0.6的最优条件下,液晶高分子的水解率达97%以上。通过在水解液中加入HCl并控制其pH在8.5,沉淀得到4,4'-联苯二酚。4,4'-联苯二酚经水洗、干燥、甲醇重结晶后,液相色谱检测其纯度可达99.9%,从废弃液晶高分子中制备4,4'-联苯二酚的收率为70%。
In this paper, 4,4'-biphenol (BP) was prepared from LCP ( PHBA-BP-PTA terpolymer) waste by hydrolysis process under atmospheric pressure using NaOH as catalyst, 1,4-dioxane and water as solvent. The effects of catalyst and solvent on hydrolysis reaction were studied. Under the optimum conditions of reaction temperature 100 ~C ,reaction time 8 h and ratio of reaction mixture:m(LCP):m (solvent) : m ( H20 ) : rn ( NaOH ) = 1:4:1.5 : 0. 6, the hydrolysis efficiency of the LCP was over 97 %. With the addition of HC1 in the hydrolysate until pH = 8.5,4,4'-biphenol precipitation was formed. After 4,4'-biphenol was washed with water, dried and recrystallized in methanol, its purity could reach 99.9%. The yield of 4,4'-biphenol from the LCP waste was 70%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2013年第2期213-216,220,共5页
Fine Chemicals
关键词
LCP
联苯二酚
水解
回收
精细化工中间体
LCP
4,4'-biphenol
hydrolysis
recover
fine chemical intermediates