水合磷酸铁铵的低热固相合成及其对乙酸丁酯的催化作用

以Fe2(SO4)3与NH4H2PO4·12H2O为原料,PEG-400为表面活性剂,经低热固相反应合成得到水合磷酸铁铵,经XRD分析表征确定其分子式为Fe3(NH4)(PO3(OH)0.666O0.333)3(PO2(OH)2)3(H2O)6Fe3H23.998NO29.997P6后,用其作为催化剂进行乙酸丁酯的合成试验。试验应用均匀设计试验法及数据挖掘技术,在数据挖掘成果的指导下考察反应时间、醇酸物质的量比及催化剂用量等因素对收率的影响。获得催化反应的最佳工艺条件是反应时间6h,醇酸物质的量比1.56∶1,催化剂用量1.73g。在这个最优的工艺条件下,水合磷酸铁铵催化合成乙酸丁酯的收率可达到98.6%。水合磷酸氢铁铵不仅合成工艺简单,可行,而且作为乙酸丁酯的催化剂时,具有良好的催化活性,工业应用潜质大。

Synthesis of Ammonium Ferric Phosphate Hydrate by Solid State Reaction and Its Catalysis Effect to Butyl Acetate

Ammonium ferric phosphate hydrate was prepared with Fe₂ (SO₄)₃ and NH₄H₂PO₄·12H₂O as raw materials via solid state reaction at room temperature and PEG-400 as surfactant.The characteristics results of XRD indicated that the mol ecular formula of the product was Fe₃ (NH₄) (PO₃ (OH)_0.666O_0.333)₃ (PO₂ (OH)₂)₃ (H₂O)₆ Fe₃H_23.998NO_29.997P₆.Synthesis experiments of butyl acetate were done used ammonium ferric phosphate hydrate as catalyzer, and application of uniform experimental design as well as data mining technology were applied in the experiments to study effect of the test factors to yield and to obtain the optimal technical conditions of the experiments, which the test factors were reaction time, mol ar ratio of alcohol to acid and amount of catalyzer.The results of catalysis tests showed that ammonium ferric phosphate hydrate had good catalysis activity, the optimal technical conditions were:reaction time 6h, mol ar ratio of alcohol to acid 1.56:1, amount of catalyzer 1.73g, and the reaction yield was 98.6% at the optimal technical conditions.The work of this paper showed that ammonium ferric phosphate hydrate had potential for industry application because it was not only feasible and simple in synthesis technics, but also had good catalysis activity for synthesis of butyl acetate.