氰乙酸乙酯脱酸精制固体碱吸附剂的工业放大试验研究

Industrial application of solid base adsorption agent to deacidification refinement of ethyl cyanocaetate

采用混捏法制备出MgO／γ-Al2O3，固体碱吸附剂，测定了固体碱的脱酸效率、酸容量、吸附热及抗流失性能。通过固定床考察了固体碱吸附剂对氰乙酸乙酯样品的吸附脱酸效果，并对固体碱吸附剂的工业放大性能进行了考察。试验结果表明，当原料氰乙酸乙酯酸值为58×10^-6、控制吸附脱酸后的酸值小于10×10^-6时，实验室制备样品的脱酸能力达到240：1（体积比）；工业放大制备的MgO／γ-Al2O3固体碱，当进料酸值为60×10^-6-80×10^-6，精制后酸值不超过20×10^-6时，固体碱吸附剂脱酸能力为173：1（质量比）。氰乙酸乙酯润湿固体碱过程平均热效应为61．91J·g^-1（催化剂）；所制备固体碱吸附剂活性组分具有良好的抗冲刷性能，吸附精制后残留在氰乙酸乙酯样品中的金属镁质量分数低于2．0×10^-6。

MgO//γ-Al2O3 adsorption agents were prepared by wet-mixing-kneading method. The performances of deacidification efficiency, adsorption capacity, adsorption heat and anti-loss of metal were measured in deacidication refinement of ethyl cyanocaetate. The deacidification efficiency of MgO//γ-Al2O3 adsorption agent was evaluated using a fixed bed micro-reactor. Furthermore, the adsorption agent was prepared in commercial scale and applied in industry. The results show that the deacidification capacity of MgO/γ-Al2O3 prepared in laboratory could achieve 240：1 （volume ratio） when the acid value of the stock is 58 × 10^-6 and that of effluent is not more than 10 × 10^-6. The treating capacity of commercial MgO/γ-AlO3 could arrive 173：1 （ mass ratio） when the acid value of the stock is 60 × 10^-6- 80 × 10^-6 and that of effluent is not more than 20 × 10^-6. The average heat effect is 61.91 J · g ^- 1 for sample prepared in laboratory. Moreover, the performance of anti-loss of metal of this solid base adsorption agent is satisfactory, and the mass content of Mg in the effluent is less than 2.0 ×10^-6.