W. Xiao-xia
2014
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Journal
Fine chemicals
Abstract
Using 2,2-bis( 4-hydroxyphenyl) hexafluoropropane as raw material,2,2-bis( 3-amino-4-hydroxyphenyl) hexafluoropropane was synthesized by nitrification reaction and reduction reaction. The pilot-scale study was carried out to determine the technological data after the success of laboratory experiment. The results indicate that,for the nitrification reaction,the conditions of n( ethanol) /n〔2,2-bis( 4-hydroxyphenyl) hexafluoropropane 〕 = 4,n( the dilute nitric acid) /n 〔2,2-bis( 4-hydroxyphenyl) hexafluoropropane〕= 2. 15,60 ℃ and the reaction time( 6 h) can give the highest yield of 2,2-bis( 3-nitro-4-hydroxyphenyl) hexafluoropropane( 96%). As for the reduction reaction,using FeCl3/ activated carbon as catalyst and ethanol as solvent,the conditions of n( hydrazine hydrate) /n〔2,2-bis( 3-nitro-4-hydroxyphenyl) hexafluoropropane 〕 = 0. 2,m( FeCl3/ activated carbon) /m〔2,2-bis( 3-nitro-4-hydroxyphenyl) hexafluoropropane〕= 0. 05,85 ℃ and the reaction time( 10 h) can give the highest yield of 2,2-bis( 3-amino-4-hydroxyphenyl) hexafluoropropane( 92%).The above process conditions have been studied in the factory and the technological data and the technological conditions have been determined.