Refining and Utilization of Rare Earth Elements from Phosphors in Waste Fluorescent Lamp

废荧光灯荧光粉中稀土元素的提炼及利用

• 批准号: 11793009
• 负责人: HIRAJIMA Tsuyoshi
• 金额: $ 2.3万
• 依托单位: HOKKAIDO UNIVERSITY
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for University and Society Collaboration
• 财政年份: 1999
• 资助国家: 日本
• 起止时间: 1999 至 2001
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-11793009/
• 关键词: Fluorescent Lamp; Rare Earth Phosphor; Processing and Separation; Recycling; Sulfuric Acid Leaching; Coprecipitation; Rare Earth Elemnets; Synthesis; 廃蛍光管; 重液選別; 風力選別; Multi-Gravity Separator; 浮選; カイクロン; 高純度化; 再合成法; 希土類蛍光管; 溶媒抽出; 侵出; 等電

The separation and acidic leaching behaviors of phosphor sludge have been examined to establish the recycling system of rare earth components contained in fluorescent lamp waste. At first, separation characteristic of rare earth components and calcium phosphate in phosphor sludge was investigated by heavy media separation, hydro separation, pneumatic separation, gravity separation and flotation. Newly developed heavy media separation method showed highest separation efficiency, recovery and grade of rare earth phosphors and the pneumatic separation was the second result. After pneumatic separation of phosphor sludge, rare earth components were leached in various acidic solutions and sodium hydroxide solution. For recovery of soluble component in leaching solution, rare earth component was recovered by treatment processes such as hydroxide and oxalate precipitations. Yttrium and europium from phosphor sludge contained in fluorescent lamp waste were recovered effectively by three process … More es of pneumatic separation, sulfuric acid leaching and oxalate precipitation methods. Their recovery was finallv about 65%, and its purity was 98.2%. It was also found that separation and recovery of rare earth elements from the leaching solution by multistage countercurrent extraction were possible.Synthesis method and sintering conditions have been examined to establish the synthesizing Y_20_3 : Eu^<3+> from phosphor sludge in processing waste fluorescent lamp. Y_20_3 : Eu^<3+> were synthesized by 1.5 mol/l sulfuric acid leaching, subsequent treatment processes such as hydroxide and oxalate precipitations, freeze-dry, and sintering in optimum condltions ; sintering temperature is 1200℃, sintering time is 40 hours, with addition of 1% barium borate as the flux. Y_20_3 : Eu^<3+> powder synthesized from phosphor sludge, was obtained well crystal structure of above 0.2 μm crystal size, and with 50% particle size in the range of 5-6 μm. It was found that Y_20_3 : Eu^<3+> powder synthesized from phosphor sludge by this work could be used substantially as a red rare earth phosphor. Less

为建立荧光灯废料中稀土成分的回收利用体系，研究了荧光粉污泥的分离和酸浸行为。新开发的重介质分离方法显示出最高的稀土荧光粉分离效率、回收率和品位，气力分离是继气力分离之后的第二个结果。荧光粉污泥中的稀土成分在各种酸性溶液和氢氧化钠溶液中浸出。为了回收浸出液中的可溶性成分，通过处理工艺从荧光粉污泥中含有的氢氧化物和草酸盐沉淀物中回收稀土成分。通过气力分离法、硫酸浸出法和草酸盐沉淀法三种工艺对灯管废料进行了有效回收。最终纯度约为65%，纯度为98.2%，并发现通过多级逆流萃取从浸出液中分离回收稀土元素是可能的。对合成方法和烧结条件进行了研究，建立了Y_20_3:Eu的合成方法。 ^<3+>是从处理废荧光灯中的荧光粉污泥中Y_20_3:Eu^<3+>通过1.5合成的。 mol/l硫酸浸出，氢氧化物、草酸盐沉淀、冷冻干燥等后续处理工艺，在最佳条件下烧结；烧结温度1200℃，烧结时间40小时，添加1%硼酸钡作为助熔剂。 Y_20_3：由磷污泥合成的Eu^<3+>粉末，得到上述良好的晶体结构发现本工作以荧光粉污泥为原料合成的Y_20_3:Eu^3+粉体晶粒尺寸为0.2μm，50%粒径在5-6μm范围内，基本可以作为红色稀土荧光粉使用。 。较少的

项目成果

高橋 徹: "風力分級および硫酸浸出法による廃蛍光体スラッジからの希土類元素の分離回収"資源と素材. 117. 579-585 (2001)

高桥彻：“风力分级和硫酸浸出法从废磷污泥中分离回收稀土元素”资源与材料。

Tsuyoshi Hirajima: "Separation Performance of Zigzag Air Classifier"Proceedings of 6th Int.Symp.East Asian Recycling Technology. 759-764 (2001)

Tsuyoshi Hirajima：“锯齿形空气分级机的分离性能”第六届国际东亚回收技术会议论文集。

Touru Takahashi: "Synthesis of Rare Earth Phosphor from Phosphor Sludge in Processing Plant of Waste Fluorescent Lamp"Reports of Hokkaido Industrial Research Institute. No. 300. 1-8 (2001)

高桥彻：《从废荧光灯处理厂的荧光粉污泥中合成稀土荧光粉》北海道工业研究所的报告。

Tsuyoshi Hirajima: "Separation Performance of Zigzag Air Classifier"Proceedings of 6th Int. Symp. East Asian Recycling Technology. 759-764 (2001)

Tsuyoshi Hirajima：“之字形空气分级机的分离性能”第六届国际会议论文集

平島剛: "ジグザグ風力選別機によるPET樹脂フレーク回収のオンラインモニタリング"第11回廃棄物学会研究発表会講演論文集. I. 445-447 (2000)

Tsuyoshi Hirashima：“使用锯齿形风力分选机在线监测 PET 树脂薄片回收”第 11 届日本废物管理学会研究会议记录 I. 445-447 (2000)。