CN111826177B - 一种废弃发光二极管封装材料热解处理协同荧光粉稀土回收方法 - Google Patents
一种废弃发光二极管封装材料热解处理协同荧光粉稀土回收方法 Download PDFInfo
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- CN111826177B CN111826177B CN202010662003.7A CN202010662003A CN111826177B CN 111826177 B CN111826177 B CN 111826177B CN 202010662003 A CN202010662003 A CN 202010662003A CN 111826177 B CN111826177 B CN 111826177B
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Abstract
本发明公开了一种废弃发光二极管封装材料热解处理协同荧光粉稀土回收方法。基于有机高分子化合物的热解特性，催化热解发光二极管中有机高分子物质，并将热解残渣中的碳转化为水煤气，实现发光二极管的高效拆解，解决了传统机械拆解方法存在发光二极管组分混杂、荧光粉中稀土元素回收困难等问题，生成的热解气和水煤气可为热解系统持续供能，并回收烟气中的热量，节约能源；同时，基于荧光粉的化学溶解反应机理，采用碱熔‑酸浸联合工艺高效回收废弃发光二极管荧光粉中稀土元素，可实现废弃发光二极管荧光粉中稀土元素的梯次浸出，沉淀回收稀土草酸盐，大大降低后期分离提纯的难度。
Description
技术领域
本发明涉及废弃发光二极管的处理方法，特别是涉及废弃发光二极管封装材料热解处理协同碱熔-酸浸回收废弃发光二极管荧光粉中稀土元素的方法。
背景技术
发光二极管(Light Emitting Diode，LED)是一种新型全固态光源，具有发光效率高、寿命长等诸多优点，已广泛应用于交通、显示、照明等领域。2018年，我国生产的发光二极管占全球产量70％，消费市场达3085.2亿元；预计到2020年，将达到4418.3亿元，年复合增速达12.7％。发光二极管在实际使用中受电流和放热的影响，平均寿命约为3年。随着发光二极管广泛普及，产生了大量的报废产品。发光二极管平均含有荧光粉约为2～5毫克/支，如按3毫克/支计，据初步估算，我国仅在2019年因废弃发光二极管导致的荧光粉浪费就达99.8吨，其中含有Eu、Y、Ce、Tb、Gd等稀土元素。倘若废弃发光二极管随生活垃圾一并填埋或焚烧，其树脂部分易因高温焚烧产生二噁英，而荧光粉将会对土壤、水体等产生危害，影响生态环境安全。与此同时，由于长期不合理的开采利用和贸易，我国稀土资源已从20世纪70年代占世界总量的74％下降至2013年的23％。开展发光二极管的无害化处理和资源化回收利用，不仅可以带来巨大的经济利益，同时也是节约稀土矿产开采、促进稀土可持续利用的重要途径。
目前我国废弃发光二极管回收利用尚处于起步阶段，相关研究工作也才刚刚开始，现有回收研究主要以发光二极管拆解和半导体回收为主，针对废弃发光二极管中的稀土回收还不多见。废弃发光二极管机械拆解采用机械切割、拆解、破碎的方法分离发光二极管机构，并采用风选、电选的方式分选(专利CN201210368117.6、CN201710884418.7、CN201811260077.7)。该方法机械机构较为简单、可实现废弃发光二极管的大规模快速分离，但该方法会造成金属和非金属部分混杂，增加后续处理的工艺难度并增加环境风险。同时，废弃发光二极管荧光粉难以用常规酸浸法回收，如氮化物体系的SiAlON:Eu2+属于六方晶体，具有较高的化学稳定性，通过常规酸浸方法难以破坏其结构；石榴石体系的(Y,Gd)3(Al,Ga)5O12:Ce也难溶于常规酸类，致使废弃发光二极管中稀土元素回收困难。
因此，为了高效处理废弃理发光二极管并回收其中的树脂和稀土元素，同时避免工艺流程复杂、资源浪费率高、回收过程二次污染严重等问题，基于树脂的热解特性和荧光粉中稀土组份的矿相特性，需要开发一种新型的废弃发光二极管回收处理方法。
发明内容
本专利发明了一种废弃发光二极管封装材料热解处理协同荧光粉稀土回收方法，解决了传统机械拆解方法中存在废弃发光二极管成分混杂、所含稀土元素回收困难等问题。基于有机高分子化合物的热解特性，催化热解废弃发光二极管中的有机高分子物质，实现废弃发光二极管的拆解并转化生成热解气、热解油和热解渣，热解渣通入高温水蒸气将其中的碳转化为水煤气。热解气和水煤气可为整套系统补充供能，热解油可作为燃料，银粉、金线、支架镀层金属和荧光粉留存于热解渣中。采用涡电流分选将热解渣中的荧光粉与银粉、金线、支架镀层金属分离。基于荧光粉中稀土组份的矿相特性，采用“碱熔-酸浸”联合工艺梯级高效提取稀土元素。首先，通过常规酸浸提取荧光粉中易溶组份，而难溶的石榴石体系荧光粉和氮氧化物体系荧光粉留在滤渣1中；然后，通过碱熔和酸浸实现氮氧化物体系荧光粉和石榴石体系荧光粉中稀土元素的高效提取；最后，通过草酸沉淀法回收稀土草酸盐。通过上述回收工艺设计，可实现废弃发光二极管中稀土元素的梯级高效提取，大大降低后期分离提纯的难度。
原料：
热解催化剂——Al2O3、ZnO、Fe2O3、CaO或Ca(OH)2等；
碱熔剂——Na2O2、NaOH或Na2CO3等；
酸浸溶剂——盐酸，质量分数38％；
酸浸助溶剂——双氧水，质量分数30％；
淋洗剂——NaOH；
分散剂——PEG 20000或PEI等；
沉淀剂——草酸溶液，质量浓度30g/L。
步骤：
实现本发明所叙述一种废弃发光二极管封装材料热解处理协同荧光粉稀土回收方法，包括如下步骤：
(1)废弃发光二极管热解：采用钢带连续式热解炉热解废弃发光二极管，以天然气和热解气作为能源，炉内通入N2作为保护气，燃烧烟气送入烟气锅炉冷却降温并回收热量，得到油气混合物和残渣。热解初始温度为300～400℃、结束温度为500～650℃，采用3段分区温控加热，1区温度300～400℃、2区温度400～500℃、3区温度500～650℃，热解时间为90～150min。
(2)制取水煤气：在N2气氛保护下将存在余热的残渣送入煤气发生炉，通入高温水蒸气，将残渣中的碳转化成水煤气，得到热解渣。水蒸气温度为750～900℃，反应压力2.3～3.2MPa，反应时间3～5min。
(3)淋洗分离油气混合物：将油气混合物送入喷淋冷凝塔，采用碱液喷淋的方式去除HBr并使油气分离，利用烟气锅炉的热量蒸干淋洗液中的水分制取NaBr，得到热解油、热解气和NaBr。NaOH溶液质量百分比浓度为5～10％。
(4)热解渣分选酸浸：采用涡电流分选将热解渣中的荧光粉与银粉、金线、支架镀层金属分离，在荧光粉中加入酸浸溶剂和酸浸助溶剂进行酸浸处理，过滤获得滤液1和滤渣1。酸浸反应温度为30～50℃、反应时间40～80min，酸浸溶剂加入量为每公斤碱熔产物加入酸浸溶剂3～8L，酸浸助溶剂加入量为每公斤碱熔产物加入酸浸助溶剂2～4L/kg。
(5)碱熔酸浸：向滤渣1中加入碱熔剂，以天然气和水煤气作为能源，进行高温碱熔并获得碱熔产物；然后向碱熔产物中加入酸浸溶剂和酸浸助溶剂进行酸浸处理，实现氮氧化物体系荧光粉和石榴石体系荧光粉的浸出，过滤获得含Eu3+、Tb3+和Ce3+的滤液2。高温碱熔渣碱质量比为1:2～1:6，煅烧温度为600～1000℃、煅烧时间30～60min；酸浸反应温度为70～90℃、反应时间20～25min，酸浸溶剂加入量为每公斤碱熔产物加入酸浸溶剂3～8L，酸浸助溶剂加入量为每公斤碱熔产物加入酸浸助溶剂2～4L/kg。
(6)制取稀土草酸盐：将滤液1与滤液2混合，向混合溶液中加入分散剂，搅拌混均。加入草酸溶液后中用氨水调节溶液pH至1.8～2.0，23～28℃下沉降4～6小时。沉淀完全后，将沉淀过滤、洗涤，利用烟气锅炉的热量干燥后获得稀土草酸盐。分散剂为PEG 20000或PEI等，加入量为混合溶液质量的3～5％，草酸溶液加入量为混合溶液质量的20～33％。
基于有机高分子化合物的热解特性，将废弃发光二极管中的环氧树脂封装材料、银胶树脂和支架高分子基材等有机高分子物质热解，实现废弃发光二极管中各组分的分离，并基于荧光粉中稀土组份的矿相特性，采用“碱熔-酸浸”联合工艺梯级高效提取稀土元素。与传统工艺相比，该方法通过热解实现废旧发光二极管中树脂封装材料等有机高分子化合物的回收并可获得更高纯度的稀土草酸盐沉淀，避免稀土回收过程中其他杂质的影响，热解获得的热解气和水煤气可为系统供能，同时回收烟气中的热量，在工业应用上节约大量能源。同时采用封装材料热解处理协同“碱熔-酸浸”联合工艺回收荧光粉中的稀土元素可避免传统工艺过程中污染物的大量排放。
附图说明
图1表示废弃发光二极管封装材料热解处理协同荧光粉回收方法的工艺流程图
具体实施方式
实例中：
酸浸溶剂——盐酸，质量分数38％；
酸浸助溶剂——双氧水，质量分数30％；
沉淀剂——草酸溶液，浓度30g/L；
实例1
将废弃发光二极管送入钢带连续式热解炉热解90min，炉内通入N2作为保护气，设定热解初始温度为320℃、结束温度为520℃，采用3段分区温控加热，1区温度320℃、2区温度450℃、3区温度520℃，得到油气混合物和残渣；在N2气氛保护下将存在余热的残渣送入煤气发生炉，通入800℃的水蒸气，3.0MPa下反应4min，得到热解渣和水煤气；将油气混合物送入喷淋冷凝塔，喷淋质量百分比浓度6％的NaOH碱液，得到热解油、热解气和NaBr；采用涡电流分选热解渣，分离得到荧光粉，在每公斤荧光粉中加入6L质量分数38％的盐酸和2L质量分数30％的双氧水进行酸浸处理，设定反应温度为40℃、反应时间60min，过滤获得滤液1和滤渣1，Y3+浸出效率为99.95％；按照1:2的渣碱质量比在滤渣1中加入Na2O2碱熔剂高温碱熔，设定煅烧温度为700℃、煅烧时间60min，在每公斤滤渣1中加入4L质量分数38％的盐酸和2L质量分数30％的双氧水进行酸浸处理，设定反应温度为75℃、反应时间25min，过滤获得滤液2，Eu3+、Tb3+和Ce3+浸出效率为99.50％；将滤液1与滤液2混合，加入混合溶液2％质量的PEG 20000分散剂搅拌混均，加入混合溶液25％质量的30g/L草酸溶液，用氨水调节溶液pH至2.0，25℃下沉降4小时，过滤、洗涤、干燥后获得稀土草酸盐，稀土总回收率为99.12％。
实例2
将废弃发光二极管送入钢带连续式热解炉热解90min，炉内通入N2作为保护气，设定热解初始温度为330℃、结束温度为560℃，采用3段分区温控加热，1区温度330℃、2区温度480℃、3区温度560℃，得到油气混合物和残渣；在N2气氛保护下将存在余热的残渣送入煤气发生炉，通入800℃的水蒸气，3.0MPa下反应4min，得到热解渣和水煤气；将油气混合物送入喷淋冷凝塔，喷淋质量百分比浓度6％的NaOH碱液，得到热解油、热解气和NaBr；采用涡电流分选热解渣，分离得到荧光粉，在每公斤荧光粉中加入6L质量分数38％的盐酸和2L质量分数30％的双氧水进行酸浸处理，设定反应温度为40℃、反应时间60min，过滤获得滤液1和滤渣1，Y3+浸出效率为99.96％；按照1:6的渣碱质量比在滤渣1中加入Na2O2碱熔剂高温碱熔，设定煅烧温度为750℃、煅烧时间65min，在每公斤滤渣1中加入4L质量分数38％的盐酸和2L质量分数30％的双氧水进行酸浸处理，设定反应温度为75℃、反应时间25min，过滤获得滤液2，Eu3+、Tb3+和Ce3+浸出效率为99.58％；将滤液1与滤液2混合，加入混合溶液2％质量的PEG 20000分散剂搅拌混均，加入混合溶液25％质量的30g/L草酸溶液，用氨水调节溶液pH至2.0，25℃下沉降4小时，过滤、洗涤、干燥后获得稀土草酸盐，稀土总回收率为99.75％。
实例3
将废弃发光二极管送入钢带连续式热解炉热解95min，炉内通入N2作为保护气，设定热解初始温度为340℃、结束温度为520℃，采用3段分区温控加热，1区温度340℃、2区温度470℃、3区温度520℃，得到油气混合物和残渣；在N2气氛保护下将存在余热的残渣送入煤气发生炉，通入800℃的水蒸气，3.0MPa下反应4min，得到热解渣和水煤气；将油气混合物送入喷淋冷凝塔，喷淋质量百分比浓度6％的NaOH碱液，得到热解油、热解气和NaBr；采用涡电流分选热解渣，分离得到荧光粉，在每公斤荧光粉中加入6L质量分数38％的盐酸和2L质量分数30％的双氧水进行酸浸处理，设定反应温度为40℃、反应时间60min，过滤获得滤液1和滤渣1，Y3+浸出效率为99.95％；按照1:4的渣碱质量比在滤渣1中加入Na2O2碱熔剂高温碱熔，设定煅烧温度为800℃、煅烧时间65min，在每公斤滤渣1中加入4L质量分数38％的盐酸和2L质量分数30％的双氧水进行酸浸处理，设定反应温度为75℃、反应时间25min，过滤获得滤液2，Eu3+、Tb3+和Ce3+浸出效率为99.53％；将滤液1与滤液2混合，加入混合溶液2％质量的PEG 20000分散剂搅拌混均，加入混合溶液25％质量的30g/L草酸溶液，用氨水调节溶液pH至2.0，25℃下沉降4小时，过滤、洗涤、干燥后获得稀土草酸盐，稀土总回收率为99.59％。
实例4
将废弃发光二极管送入钢带连续式热解炉热解100min，炉内通入N2作为保护气，设定热解初始温度为320℃、结束温度为540℃，采用3段分区温控加热，1区温度320℃、2区温度480℃、3区温度540℃，得到油气混合物和残渣；在N2气氛保护下将存在余热的残渣送入煤气发生炉，通入800℃的水蒸气，3.0MPa下反应4min，得到热解渣和水煤气；将油气混合物送入喷淋冷凝塔，喷淋质量百分比浓度6％的NaOH碱液，得到热解油、热解气和NaBr；采用涡电流分选热解渣，分离得到荧光粉，在每公斤荧光粉中加入6L质量分数38％的盐酸和2L质量分数30％的双氧水进行酸浸处理，设定反应温度为40℃、反应时间60min，过滤获得滤液1和滤渣1，Y3+浸出效率为99.96％；按照1:4的渣碱质量比在滤渣1中加入Na2O2碱熔剂高温碱熔，设定煅烧温度为700℃、煅烧时间60min，在每公斤滤渣1中加入4L质量分数38％的盐酸和2L质量分数30％的双氧水进行酸浸处理，设定反应温度为85℃、反应时间20min，过滤获得滤液2，Eu3+、Tb3+和Ce3+浸出效率为99.56％；将滤液1与滤液2混合，加入混合溶液2％质量的PEG 20000分散剂搅拌混均，加入混合溶液25％质量的30g/L草酸溶液，用氨水调节溶液pH至2.0，25℃下沉降4小时，过滤、洗涤、干燥后获得稀土草酸盐，稀土总回收率为99.64％。
Claims (2)
1.一种废弃发光二极管封装材料热解处理协同荧光粉稀土回收方法，其特征在于以下步骤：
步骤1：采用钢带连续式热解炉热解废弃发光二极管，炉内通入N2作为保护气，加热升温热解得到油气混合物和残渣；热解初始温度为300~400℃、结束温度为500~650℃，采用3段分区温控加热，1区温度300~400℃、2区温度400~500℃、3区温度500~650℃，热解时间90~150min；
步骤2：在N2气氛保护下将存在余热的残渣送入煤气发生炉，通入高温水蒸气，将残渣中的碳转化成水煤气，得到热解渣；水蒸气的温度为750~900℃，反应压力2.3~3.2MPa，反应时间3~5min；
步骤3：将油气混合物送入喷淋冷凝塔，采用碱液喷淋的方式去除HBr并使油气分离，得到热解油、热解气和NaBr；
步骤4：采用涡电流分选热解渣，将荧光粉与银粉、金线、支架镀层金属分离，在荧光粉中加入酸浸溶剂和酸浸助溶剂进行酸浸处理，过滤获得滤液1和滤渣1；
步骤5：向滤渣1中加入碱熔剂，进行高温碱熔并获得碱熔产物；然后向碱熔产物中加入酸浸溶剂和酸浸助溶剂进行酸浸处理，实现氮氧化物体系荧光粉和石榴石体系荧光粉的浸出，过滤获得含Eu3+、Tb3+和Ce3+的滤液2；高温碱熔中滤渣1与碱熔剂质量比为1:2~1:6，煅烧温度为600~1000℃、煅烧时间30~60min；
步骤6：将滤液1与滤液2混合，加入分散剂搅拌混均，加入草酸溶液后用氨水调节溶液pH至1.8~2.0，23~28℃下沉降4~6小时，沉淀完全后将沉淀过滤、洗涤、干燥后获得稀土草酸盐；
步骤3中碱液为NaOH溶液，NaOH溶液质量百分比浓度为5~10%；
步骤4中酸浸反应温度为30~50℃、反应时间40~80min，酸浸溶剂加入量为每公斤碱熔产物加入酸浸溶剂3~8L，酸浸助溶剂加入量为每公斤碱熔产物加入酸浸助溶剂2~4L/kg；
步骤5中酸浸反应温度为70~90℃、反应时间20~25min，酸浸溶剂加入量为每公斤碱熔产物加入酸浸溶剂3~8L，酸浸助溶剂加入量为每公斤碱熔产物加入酸浸助溶剂2~4L/kg。
2.如权利要求1所述的一种废弃发光二极管封装材料热解处理协同荧光粉稀土回收方法，其特征在于：步骤6中分散剂为PEG 20000，加入量为混合溶液质量的3~5%，草酸溶液质量浓度为30g/L，加入量为混合溶液质量的20~33%。
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