催化加氢制备三(4-氨基苯基)硫代磷酸酯工艺条件的改进

以对硝基苯酚和三氯硫磷合成反应制得的三(4-硝基苯基)硫代磷酸酯为原料,催化加氢还原制备三(4-氨基苯基)硫代磷酸酯。通过对溶剂种类、催化剂型号及用量、反应温度、反应压力等工艺条件的研究,得出如下较佳的工艺条件:以甲醇为溶剂,Raney-N i为催化剂,反应温度70℃、反应压力2.0~3.0M Pa。所得成品纯度大于94%。通过补加少量新鲜催化剂,催化剂能够重复使用并且性能稳定。

Improving of Processing Conditions for Preparation of Tris(4 -Amino Phenyl)Thiophosphate by Catalytic Hydrogenation

Tris(4-amino phenyl)thiophosphate(TABSPE)was prepared by catalytic hydrogenation of tris((4-)nitro phenyl)thiophosphate(TNBSPE),which was synthesized from p-nitrophenol and PSCl_3.Effects of solvent,type and dosage of catalyst,reaction temperature and pressure on reaction were investigated.Under optimal technological conditions:methanol as solvent,Raney-Ni as catalyst,reaction temperature 70℃,and pressure 2.0-3.0MPa,purity of tris(4-amino phenyl)thiophosphate would be more than 94%.Hydrogenation catalyst could be reused and kept good activity by adding small amount of additional catalyst to reaction system.