催化加氢制备三(4-氨基苯基)硫代磷酸酯工艺条件的改进

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

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-Ni为催化剂,反应温度70℃、反应压力2.0～3.0MPa.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.

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 PSCl3. 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.