【摘要】 以2,2-二(4-羟基苯基)六氟丙烷为原料,分别经硝化和还原反应合成出2,2-二(3-氨基-4-羟基苯基)六氟丙烷。并在实验室小试成功后,进行工厂中试研究,以确定中试的各个工艺参数。结果表明,对于第1步硝化反应,以乙醇做溶剂,用量为n(乙醇)/n〔2,2-二(4-羟基苯基)六氟丙烷〕=4,n(稀硝酸)/n〔2,2-二(4-羟基苯基)六氟丙烷〕=2.15,反应温度为60℃,反应时间为6 h的条件下,合成2,2-二(3-硝基-4-羟基苯基)六氟丙烷的产率达到最高值96%。对于第2步还原反应,采用自制FeCl3/活性炭为催化剂,乙醇做溶剂,n(水合肼)/n〔2,2-二(3-硝基-4-羟基苯基)六氟丙烷〕=0.2,m(FeCl3/活性炭)/m〔2,2-二(3-硝基4-羟基苯基)六氟丙烷〕=0.05,反应温度为85℃,反应时间为10 h的条件下,合成2,2-二(3-氨基-4-羟基苯基)六氟丙烷的产率达到最高值92%。该工艺条件在工厂已进行了中试研究,确定了工业实验的各个工艺参数和工艺条件。更多还原

【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.更多还原