CN115094484A - 硫酸溶液中旋转阴极四排阳极连续固相、离子电解、氧化、机械分离处理废铅蓄电池工艺 - Google Patents
硫酸溶液中旋转阴极四排阳极连续固相、离子电解、氧化、机械分离处理废铅蓄电池工艺 Download PDFInfo
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Abstract
本发明提供一个在H2SO4电解液中旋转阴极四排阳极连续固相电解、离子电解、阳极氧化、机械分离处理废铅蓄电池工艺。电解是在不锈钢板制的电解槽中进行，H2SO4为电解液。旋转阴极由两层不锈钢板卷制而成。内层钻有孔洞，并布有螺旋带。人工拆解的极板，在旋转阴极内，铅膏与板栅机械分离。铅膏成分：Pb 0、PbO、PbO2、PbSO4作为分散固相均匀游离悬浮在电解液中，铅化合物中的铅经固相电解还原成电铅，沉积在旋转阴极表面；一部分Pb 0经离子电解还原成电铅，沉积在旋转阴极表面。另一部分Pb 0被阳极析出的氧原子氧化成PbO2沉积在阳极上。经脱膏后的板栅从旋转阴极内排出槽外。增加阳极板多产PbO2，少产电铅。电铅生产PbO2工艺复杂，污染环境。电铅、铅合金和PbO2、H2SO4做蓄电池。资源循环利用、绿色环保、无碳排放，生产连续进行。
Description
技术领域
本发明属于含铅废料固相电解、离子电解、阳极氧化、机械分离冶金领域。以湿法冶金方式处理废铅蓄电池回收铅、铅合金、PbO2、H2SO4.
背景技术
从废铅蓄电池中回收铅，传统的方法是火法熔炼。该方法高温操作，冶炼时放出大量的二氧化硫和铅蒸汽，严重污染环境，操作人员铅中毒。金属回收率底，能耗大。
为了解决火法熔炼存在的问题，广泛开展了湿法冶炼提取铅金属的工艺研究。研究的方法流程长，生产成本高于火法。
美国矿务局罗拉研究中心，把废铅蓄电池经M·A破碎分离，使极板板栅与铅膏分离，铅膏经脱硫转化酸溶电解得到电铅。板栅熔化铸成阳极板，进行电解精炼得到电铅。进行了工业实验。
意大利Engitec公司，半工业实验。废铅蓄电池经CX破碎分离，铅膏用Na2CO3脱硫转化，用HBF4浸出，生成Pb(BF4)2溶液。电解得到电铅。
在我国中科院化冶所含铅物料固相电解处理废铅蓄电池工艺。废铅蓄电池经M·A破碎分离得到铅膏和板栅，板栅熔化得到铅合金，出渣率20％，作为返料。铅膏经脱硫转化，制成阴极板，碱性溶液、固相电解，得到电铅。实现了工业化生产，电解周期20小时，间歇生产。
以上三个工艺过程都采用了CX或M·A破碎分离系统。铅膏经脱硫转化酸溶或固相电解得到电铅。工艺过程复杂。一套小型CX破碎分离装置每小时处理50吨废铅蓄电池，设备重50吨。
马光甲旋转阴极连续固相电解处理废铅蓄电池工艺。发明专利号为：201110173817.5，经脱硫转化的极板，不经CX或M·A破碎分离，加入到旋转阴极内，在碱性溶液中进行固相电解。在旋转阴极表面得到电铅，其内得到板栅，自动排出槽外。铅、板栅两者完全分离开，实现了工业化生产，生产连续进行。该发明没有公开铅膏中Pb°的去处、阳极上生成PbO的反应机理。
马光甲、郭西元、马龙、盛梅在NaOH电解液中旋转阴极四排阳极连续固相电解、离子电解、阳极氧化、机械分离处理废铅蓄电池工艺。发明专利号： 202110331238.2.公开了Pb°的去处，阳极生成PbO的反应机理。增加阳极多产PbO，少产电铅，电铅生成PbO工艺复杂，污染环境。实质审查中。
发明内容：
本发明提供一个在H2SO4电解液中旋转阴极四排阳极连续固相电解、离子电解、阳极氧化、机械分离处理废铅蓄电池工艺。电解是在不锈钢电解槽中进行 H2SO4电解液。旋转阴极由二层不锈钢板卷制而成、内层钻有孔洞，并布有螺旋带。
电解装置如图所示：图中1加料口、2极板、3电解槽、4电解溶液、5阳极、 6旋转阴极、7电铅、8导电棒、9螺旋带、10板栅集料斗、11出料口、12旋转轴、导电环、14板栅、15Pb°、16PbO2、17H2SO4
工艺过程详细过程如下：
人工拆解的极板(2)加入旋转阴极(6)中进行电解，(6)在螺旋带 (9)，的作用下使极板(2)从加料口(1)移向出料口(11)。在输送过程中极板(2)板栅(14)与铅膏分离。铅膏成分：Pb 0、PbO、PbO2、PbSO4作为分散固相均匀游离悬浮在电解液中(4)中，铅化合物中的铅经固相电解还原成电铅(7)沉积在旋转阴极(6)表面，一部分Pb°(15)经离子电解还原成电铅(7)沉积在旋转阴极(6)表面。另一部分Pb°(15)被阳极析出的氧原子氧化生成PbO2(16) 沉积在阳极(5)上，脱膏后的板栅(14)从旋转阴极(6)内排出槽外。得到电铅(7)板栅(14)和PbO2(16)、H2SO4(17)四个产品。
以下是在H2SO4电解液中旋转阴极四排阳极连续固相电解、离子电解、阳极氧化、机械分离处理废铅蓄电池工艺。工艺条件是：H2SO4浓度40g/L，电解液温度室温、槽电压2.5～3V、阴极电流密度200A/m2，极间距60mm。
本发明工艺过程简单与火法相比消除了对环境的污染，无碳排放、金属回收率高，是个绿色环保的好工艺。
特别值得提及的是：本发明的关键设备旋转阴极，它代替了CX或M·A 破碎分离系统，代替了火法治炼的工艺和设备得到电铅、铅合金两个产品，阳极得到PbO2、H2SO4两个产品，无污染、无碳排放、绿色环保。
附图说明：
图1是旋转阴极四排阳极连续固相电解、离子电解、阳极氧化、机械分离处理废铅蓄电池装置、加料、产品俯视示意图。
具体实施方式
在H2SO4电解液中转阴极四排阳极连续固相电解、离子电解、阳极氧化、机械分离处理废铅蓄电池装置如图1所示：1加料、2极板、3电解槽、4电解液、 5阳极、6旋转阴极、7电铅、8导电棒、9螺旋带、10板栅集料斗、11出料口、 12旋转轴、13导电环、14板栅、15Pb°、16PbO2、17H2SO4。极板2在旋转阴极6 内机械分离成铅膏15Pb°和14板栅。一部分15Pb°经固相电解、离子电解，在旋转阴极6表面上得到7电铅，另一部分15Pb°被阳极析出的氧原子氧化成16PbO2，在阳极5上得到16PbO2。脱膏后的14板栅从旋转阴极6内排出槽外，得到板栅14。电铅、板栅、PbO2、H2SO4四个产品用来作铅蓄电池。实现了资源的循环利用。无污染、绿色环保、无碳排放。生产连续进行。
Claims (3)
1.在H2SO4电解液中旋转阴极四排阳极连续固相电解、离子电解、阳极氧化、机械分离处理废铅蓄电池工艺包括电解槽、H2SO4电解液、旋转阴极、四排阳极其特征是：旋转阴极由二层不锈钢板卷制而成、内层钻有孔洞，并布有螺旋带。
2.按权利要求1所述的，在H2SO4电解液中旋转阴极四排阳极连续固相电解、离子电解、阳极氧化、机械分离处理废铅蓄电池工艺其特征是：螺旋带外径φ1200mm、内径φ800mm.带长82m，并焊有导电棒。
3.按权利要求1所述的，在H2SO4电解液中旋转阴极四排阳极连续固相电解、离子电解、阳极氧化、机械分离处理废铅蓄电池工艺其特征是：四排阳极置于旋转阴极两侧，每侧二排，阳极为不锈钢板。
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| US20180355494A1 (en) * | 2015-05-13 | 2018-12-13 | Aqua Metals Inc. | Closed Loop Systems and Methods for Recycling Lead Acid Batteries |
| CN106065485A (zh) * | 2016-07-19 | 2016-11-02 | 云南祥云飞龙再生科技股份有限公司 | 一种硫酸铵氨电还原制取铅工艺 |
| US20190242022A1 (en) * | 2016-07-19 | 2019-08-08 | Xiangyun Tenglong Investment Co., Ltd. | Process for Preparing Lead by Electroreduction with Ammonium Sulfate and Ammonia |
| CN113046787A (zh) * | 2021-03-12 | 2021-06-29 | 赵坤 | 用于废铅蓄电池铅膏三元体系湿法铅回收电解液、系统及方法 |
| CN113151864A (zh) * | 2021-03-26 | 2021-07-23 | 马光甲 | 旋转阴极四排阳极连续固相电解、离子电解、阳极氧化、机械分离处理废铅蓄电池工艺 |
| CN113862479A (zh) * | 2021-09-26 | 2021-12-31 | 东北大学 | 一种废铅蓄电池中铅膏的资源化回收处理方法 |
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