CN100557045C - 从高炉瓦斯灰中提取金属铟、锌、铋的方法 - Google Patents
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Abstract
本发明是一种高炉从瓦斯灰中提取金属铟、锌、铋的方法，步骤是：瓦斯灰加焦粉和添加剂用回转窑进行还原挥发，使铟、锌、铅、铋呈气态氧化物富集于烟气，铁进入炉渣；对烟气进行收尘得锌氧粉；对锌氧粉进行湿法脱氯，加入适当NaOH液，95℃的温度下反复洗涤；对脱氯后的产物进行中性酸浸，将较易溶于酸的锌等金属溶浸进入中性液中，铟、铅、铋则留于渣中；对中性液进行净化以除去残留的铁和镉，然后电解得锌产品；对中性渣加入浓硫酸进行二次高温强酸浸出，浸渣回收铋和铅。浸出液为含铟料液，用P204萃取，用盐酸进行反萃取，经置换、熔铸得粗铟，再经真空蒸馏脱杂和电解处理得4N-5N高纯铟。本发明对含铟浸出液采用变价化合物还原-P204萃取—置换工艺，经济高效地提铟，工艺顺畅，取得重大突破。
Description
技术领域
本发明属于一种从高炉瓦斯灰(泥)中提取金属铟、锌、铋的方法。
背景技术
在高炉炼铁的生产过程中，对高炉产出的荒煤气进行除尘过程而产生的固体废弃物，用干法布袋除尘器捕收的俗称瓦斯灰，用湿法收尘器捕收的俗称瓦斯泥。瓦斯灰(泥)为微粒物料，化学成分比较复杂，除铁之外，尚含有未燃烧完全的炭和锌、铅、铟等少量有色金属。如某钢铁公司所产炼铁烟尘的物质组成为：Fe28％，C18％，Zn9％，Pb1％，InO.012％，S0.6％，SiO29％，CaO6％，C11～2％，水份5-50％。
人们一向认为瓦斯灰较难利用或者利用价值不大，将之丢弃堆存于周围山地，长期风吹雨淋，任意飘扬流失，对周围环境造成较大污染。中国钢产量约为每年4亿吨，居世界首位，一年产出的高炉炼铁烟尘约280万吨(干基)，全世界的烟尘产出量更大。随着世界各国对环保要求的提高，对高炉炼铁烟尘的无害化、资源化处理日益迫切。
特别应当指出的是，铟为现代电子工业、通讯工业等行业中一种十分重要的金属材料，价值是锌、铅等常见有色金属的几十甚至几百倍，如能开发出从高炉瓦斯灰中提取高纯铟的技术，意义重大。
然而，现有技术中，从瓦斯灰(泥)中提取高纯铟的技术，至今未见报道。为便于叙述起见，以下瓦斯灰均包含瓦斯泥。
发明内容
本发明的目的就是要提出一种从高炉炼铁的瓦斯灰中提取金属铟、锌、铋的方法，变废为宝，实现这种固体废弃物的无害化和资源化处理，并能产生较高的经济和社会效益，以弥补现有技术的不足。
本发明提出的这种从高炉瓦斯灰中提取金属铟、锌、铋的方法，其特征在于它含如下步骤：
(1)将瓦斯灰用回转窑加入焦粉和添加剂进行还原挥发，使铟、锌、铅、铋呈气态氧化物形态富集，转移于烟气，铁金属则进入炉渣再回收；
回转窑中加入的添加剂为石英或灰石，添加量按渣碱度予以控制。
(2)对烟气进行收尘处理捕集锌氧粉，达标废气排放；
(3)对锌氧粉进行湿法脱氯，具体做法是：加入适当NaOH液，95℃的温度下反复洗涤。
(4)对脱氯后的产物进行中性酸浸，控制pH值为5.2-5.4，将较易溶于酸的锌等金属熔浸进入中性液中，铟、铅、铋则留于中性渣中；
(5)对中性液进行净化以除去残留的铁和镉等，然后电解得锌片，进而熔铸得锌锭产品；
(6)对中性渣加入浓硫酸进行二次高温强酸浸出，浸渣回收铋和铅。浸出液为含铟料液，用P204萃取，用盐酸进行反萃取，经置换、熔铸得粗铟，再经真空蒸馏脱杂和电解处理得4N-5N高纯铟产品。
萃取作业中的萃取余液返回上道中性浸出作业。
二次酸浸作业的条件为起始H2SO43-4N，95℃。
(7)提铟后的浸渣再用盐酸浸出、铁屑置换回收金属铋，浸出残渣为常规炼铅原料。
本发明将有色冶炼工艺中成熟的回转窑还原挥发技术移植于处理黑色冶炼的固废物，使用巧妙的工艺配方和合理的设备改造，保证了高效、连续和大规模地生产，产出富集比达五倍以上的含铟氧化锌粉，为下步的湿法提取奠定了基础。回转窑还原挥发处理炼铁烟尘所得氧化锌粉是一种淡绿色粉末，除含有色金属锌、铅、铟外，还含有5-9％的有害杂质——氯和氟。现有炼锌厂皆不能直接使用此类原料来生产电锌，而只能用之生产硫酸锌，二种产品价值相差巨大。本发明则能从氧化锌粉直接生产出电锌的，实现了现有技术的重大突破。本发明对含铟浸出液采用变价化合物还原-P204萃取-置换工艺，可以经济有效地提取铟，使工艺顺畅，得到含In＞99％的粗铟。现有技术对粗铟的提炼采用化学精炼-多次电解的工艺，费时费钱，而且难以得到5N级的高纯铟，本发明采用直空蒸馏-电解工艺做到了较低成本获得质量稳定的4N-5N高纯铟。
本发明亦可应用于处理炼钢电炉烟尘、其它氧化锌物料等而回收锌、铟等金属。
附图说明
附图为本发明的工艺流程图。
具体实施方式
实例一以上文提到的某钢铁公司所产炼铁烟尘(瓦斯泥)为例，其物质组成为：Fe28％，C18％，Zn9％，Pb1％，In0.012％，S0.6％，SiO29％，CaO6％，Cl1％，水份30％。
将这样的瓦斯泥与焦粉按100∶35的比例混匀，同时加入灰石粉作为添加剂，用φ2.1×32M回转窑在1200℃温度下进行还原挥发处理，加料量为混合物料～100t/d，焦粉～35t/d，产出锌氧粉～10t/d，其成分为Zn～55％±，Pb～9％±，Bi～0.6％，In～0.07％±，CL6-9％，窑渣含Zn＜0.5％，Pb＜0.2％，In＜0.002％，窑渣用弱磁选机进行磁选，得到含Fe＞55％铁精矿出售，非磁选产物外售水泥厂配料，含金属的挥发回收率为Zn～85％，Pb～80％，In～70％，Bi～70％。
对高氯锌氧进行碱洗脱氯，工艺控制条件为加入适当NaOH，控制洗液PH＞10，温度95℃，反复洗涤多次至CL＜0.05％。
用锌电解溶液(Zn50g/L，H2SO4150g/L)对脱氯后锌氧粉进行中性浸出，控制浸出终点pH5.2-5.4，使＞95％的锌被溶浸进入溶液，而让In、Pb残留于中性渣中。
含锌浸出液用常规的氧化除Fe、加锌粉置换除Cd、Ni、Co等而得净液，再用常规的锌电积方法产出锌片，熔铸得锌锭，同时产出废电解液返供中性浸出。
对中性浸出渣进行高温、高酸二次溶浸、控制工艺条件为始酸H2SO43-4N，温度95℃，时间6h，让中性浸出渣中的In和Zn尽可能溶浸进入溶液，Pb则残留于酸性残渣中。
对含In～500mg/L，Zn～80g/L，H2SO4～2N的溶浸液进行Fe3+→Fe2+的还原，在水平箱式混合澄清槽中加入30％P204+煤油进行多级萃取，用8NHCL多级反萃取，并控制萃取和反萃取的相比，得到含In25～50g/L的高铟液。
用碱调整高铟反萃液的pH至2.5，加入铝片进行置换反应而产出粗铟。
对粗铟压团-熔铸而产出含In＞99.5％之粗铟。
将粗铟通过真空蒸馏去除杂质后，按常规工艺进行电解精炼，产出含In99.993-99.999％之高纯铟。
提铟后的酸性残渣采常温HCl浸出，让Bi溶浸进入溶液，通过铁板置换而回收得海绵铋，熔铸成粗铋，经用常规火精炼产出精铋。HCl溶浸后的残渣之主成分为PbSO4，含Pb＞35％，可作铅原料外售给炼铅厂。
实例二另一钢铁厂瓦斯灰，成分为，％：Fe36，C20，Zn6.5，Pb1，CaO8，SiO23，In0.01，C11，水份15％。将其按瓦斯灰∶焦粉＝100∶30的比例(并配入少量高硅氧化锌矿)而加入φ2.5×38M回转窑进行还原挥发。日处理瓦斯灰150吨，所得锌氧粉成分约为％：Zn～50，Pb～10，In～0.06，CL6。对该锌氧粉及窑渣的处理与实例一相同，并据此产出铁精矿、锌、铟金属锭和铅渣。
Claims (6)
1、一种从高炉瓦斯灰中提取金属铟、锌、铋的方法，其特征在于它含如下步骤：
(1)将瓦斯灰用回转窑加入焦粉和添加剂石英或灰石进行还原挥发，使铟、锌、铅、铋呈气态氧化物形态富集，转移于烟气，铁金属则进入炉渣再回收；
(2)对烟气进行收尘处理捕集锌氧粉，达标废气排放；
(3)对锌氧粉进行湿法脱氯；
(4)对脱氯后的产物进行中性酸浸，控制pH值为5.2-5.4，将较易溶于酸的锌金属熔浸进入中性液中，铟、铅、铋则留于中性渣中；
(5)对中性液进行净化以除去残留的铁和镉，然后电解得锌片，进而熔铸得锌锭产品；
(6)对中性渣加入浓硫酸进行二次高温强酸浸出，浸渣回收铋和铅，浸出液为含铟料液，用P204萃取，用盐酸进行反萃取，经置换、熔铸得粗铟，再经真空蒸馏脱杂和电解处理得4N-5N高纯铟产品。
2、根据权利要求1所述的从高炉瓦斯灰中提取金属铟、锌、铋的方法，其特征在于提铟后的浸渣再用盐酸浸出、铁屑置换回收金属铋，浸出残渣为常规炼铅原料。
3、根据权利要求1所述的从高炉瓦斯灰中提取金属铟、锌、铋的方法，其特征在于回转窑中加入的添加剂为石英或灰石，添加量按渣碱度予以控制。
4、根据权利要求1所述的从高炉瓦斯灰中提取金属铟、锌、铋的方法，其特征在于萃取作业中的萃取余液返回上道中性浸出作业。
5、根据权利要求1所述的从高炉瓦斯灰中提取金属铟、锌、铋的方法，其特征在于二次酸浸作业的条件为起始H2SO43-4N，95℃。
6、根据权利要求1所述的从高炉瓦斯灰中提取金属铟、锌、铋的方法，其特征在于对锌氧粉进行湿法脱氯做法是加入NaOH液，控制pH＞10，95℃的温度下反每洗涤。
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