有色金属科学与工程
有色金屬科學與工程
유색금속과학여공정
JIANGXI NONFERROUS METALS
2015年
1期
106-110
,共5页
杨明%吴迪%叶信宇%焦芸芬%吴龙%黄昕%李琴
楊明%吳迪%葉信宇%焦蕓芬%吳龍%黃昕%李琴
양명%오적%협신우%초예분%오룡%황흔%리금
大粒度%氧化钕%P507-N235-磺化煤油-环己烷%草酸%反萃余液
大粒度%氧化釹%P507-N235-磺化煤油-環己烷%草痠%反萃餘液
대립도%양화녀%P507-N235-광화매유-배기완%초산%반췌여액
large particle%neodymium oxide%P507-N235-kerosene-cyclohexane%oxalic acid%stripping solution
以草酸为沉淀剂,P507-N235-磺化煤油-环己烷体系分离稀土过程中的氯化钕反萃余液为原料,制备了大粒度氧化钕.采用激光粒度仪结合扫描电镜对样品进行粒度、形貌分析;使用X 射线衍射对前驱体煅烧样品进行物相分析,结合差热分析研究前驱体的热分解过程.沉淀过程中草酸钕前驱体粒度的主要影响因素为反应温度、搅拌速度、沉淀剂滴加速度及陈化时间,其最佳制备条件为反应温度50℃,搅拌速度300 r/min,沉淀剂滴加速度9 mL/min,陈化时间24 h.对比实验表明,氯化钕反萃余液中残余的有机相可以有效地增大前驱体的粒度.草酸钕前驱体在煅烧温度800℃下保温2 h可完全转化为Nd2O3,氧化钕粒径达到50μm以上.
以草痠為沉澱劑,P507-N235-磺化煤油-環己烷體繫分離稀土過程中的氯化釹反萃餘液為原料,製備瞭大粒度氧化釹.採用激光粒度儀結閤掃描電鏡對樣品進行粒度、形貌分析;使用X 射線衍射對前驅體煅燒樣品進行物相分析,結閤差熱分析研究前驅體的熱分解過程.沉澱過程中草痠釹前驅體粒度的主要影響因素為反應溫度、攪拌速度、沉澱劑滴加速度及陳化時間,其最佳製備條件為反應溫度50℃,攪拌速度300 r/min,沉澱劑滴加速度9 mL/min,陳化時間24 h.對比實驗錶明,氯化釹反萃餘液中殘餘的有機相可以有效地增大前驅體的粒度.草痠釹前驅體在煅燒溫度800℃下保溫2 h可完全轉化為Nd2O3,氧化釹粒徑達到50μm以上.
이초산위침정제,P507-N235-광화매유-배기완체계분리희토과정중적록화녀반췌여액위원료,제비료대립도양화녀.채용격광립도의결합소묘전경대양품진행립도、형모분석;사용X 사선연사대전구체단소양품진행물상분석,결합차열분석연구전구체적열분해과정.침정과정중초산녀전구체립도적주요영향인소위반응온도、교반속도、침정제적가속도급진화시간,기최가제비조건위반응온도50℃,교반속도300 r/min,침정제적가속도9 mL/min,진화시간24 h.대비실험표명,록화녀반췌여액중잔여적유궤상가이유효지증대전구체적립도.초산녀전구체재단소온도800℃하보온2 h가완전전화위Nd2O3,양화녀립경체도50μm이상.
The large particle neodymium oxide is prepared with oxalic acid as precipitator, and stripping solution by P507-N235-kerosene-cyclohexane system as mother solution. The particle size, morphology ,phase composition and thermal stability of samples are characterized by laser particle size analyzers, including SEM , XRD and TG-DTG. The main parameters affecting the particle size of precursor in precipitation are reaction temperature, stirring velocity, feeding speed and aging time. The optimum parameters are as follows: reaction temperature, 50 ℃; stirring velocity, 300 r/min; feeding speed, 9 mL/min; aging time, 24 h. A comparative experiment indicates that the residual organic phase in stripping solution can effectively increase the particle size of precursor. Comparative experiments show that the residual organic phase stripping solution of neodymium oxide effectively increases the particle size of precursor. The precursor decomposes completely to neodymium oxide calcined at 800 ℃ for 2 h. The median particle size of final neodymium oxide is larger than 50μm.