磷酸三丁酯制备工艺研究

Study on preparation technology of tributyl phosphate

通过引入不同缚酸剂作为路易斯碱,开展了活性溶剂法,来抑制传统磷酸三丁酯合成工艺中发生的副反应,提高磷酸三丁酯产品收率。进一步开展活性溶剂筛选试验,活性溶剂工艺条件优化试验,活性溶剂工艺验证放大试验,结果表明,乙酸丁酯作为路易斯碱,当三氯氧磷、丁醇和乙酸丁酯的投料物质的量比为1∶4∶3时,不仅磷酸三丁酯合成收率达90.2%,氯化氢脱除率达77.6%,又可以最大程度降低投料量,减轻回收压力。通过2L的放大实验,验证了该制备工艺可获得73%~75%的氯化氢脱除率,92%~95%的磷酸三丁酯收率,纯度达98.8%,具有较好应用前景。

By introducing different acid binding agents as Lewis bases,An active solvent method was developed to inhibit the side reactions in the traditional synthesis process of tributyl phosphate,to improve the yield of tributyl phosphate.Further carry out the active solvent screening test,the active solvent process conditions optimization test,the active solvent process verification and amplification test,The results showed that butyl acetate was used as Lewis base,When the molar ratio of phosphorus trichlorooxychloride,butanol and butyl acetate was 1∶4∶3,not only was the yield of tributyl phosphate reached 90.2%,but the removal rate of hydrogen chloride reached 77.6%,It can also reduce the feeding amount and the recovery pressure to the greatest extent.Through the amplification experiment of 2 L,it is verified that the preparation process can obtain 73-75%removal rate of hydrochloric acid,92-95%yield of tributyl phosphate,and the purity can reach 98.8%,This preparation process has a good application prospect.