新型固定床气体氟化法制备低氧氟化钆

Preparation of Hypoxia Gadolinium Fluoride with Fixed-bed Gas Fluorination Method

在固定床气体氟化反应器内,以氧化钆为原料,氟化氢为氟化剂,采用控制变量法研究了温度、时间、气体流量、氟化氢用量和料层厚度对氧化钆氟化过程的影响。结果表明,氧化钆与氟化氢在90℃开始反应,反应初期有中间产物Gd4O3F6生成;在氟化温度为540℃、氟化氢过理论量为50%、氟化时间为7 h、氟化氢平均流量为1.5 kg·h-1、料层厚度为30 mm的条件下,可获得氟化率大于99.95%、氟含量大于26.59%、氧含量小于0.05%的低氧氟化钆。

GdF3 was synthesized using Gd203 as raw material and HF as fluridizer in the fixed - bed gas fluorination reactor. Effects of temperature, time, gas flow rate, gas consumption and material thickness on fluorination process were investigated by the variable -controlling method. Gd2O3 starts to react with HF gas at 90℃, and the intermediate product of the reaction is Gd4O3 F6. The fluorination efficiency of more than 99.95%, fluorine content of more than 26.59% and the oxygen content of less than 0.02% can be reached when the excessive dosage of HF gas of 50%, the fluorination time of 7 h, the HF gas flow rate of 1.5 kg/h, the charging level is 30 ram, and at 540℃.