2,2-二(3-氨基-4-羟基苯基)六氟丙烷的合成

The synthesis of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane

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10h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。

Abstract:

Using 2,2-bis(4-hydroxyphenyl)hexafluoropropane as raw materials, 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane was synthesized by nitrification reaction and reduction reaction. The factory pilot-scale study was carried out to determine the technological date after the laboratory experiment succeed. The results indicated that as for the nitrification reaction, 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), which can get the highest 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane yield (96%). As for the reduction reaction, using FeCl3/ activated carbon as catalyst and ethanol was the solvent, 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), which can reach the highest 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane yield (92%). The above process conditions have been studied in the factory and determined the technological date and the technological conditions.