CN1039136C - 低品位及难处理贵金属物料的富集活化溶解方法 - Google Patents
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Abstract
低品位及难处理贵金属物料的富集活化溶解方法。方法步骤包括：(1)利用原料含有的硫化物或添加重金属硫化物熔炼金属锍，分离渣，(2)锍加铝熔炼铝合金化，(3)铝合金加稀酸溶解分离贱金属，(4)稀酸不溶渣酸氧化介质溶解贵金属。
Description
低品位及难处理贵金属物料的富集活化溶解方法，本发明是属于贵金属冶金。
贵金属Au、Ag、Pt、Pd、Rh、Ir、Os、Ru在原料中含量少而分散，其冶金过程有一系列富集、活化、分离精炼冗长的过程。近年来，溶剂萃取法从溶液中分离提取贵金属的新技术逐步发展应用。溶剂萃取法要求精矿中所有贵金属都转入溶液，而且性质、成分和浓度容易调整。英国阿克统精炼厂对品位大于50％的贵金属精矿采用过氧化钠熔融法(Ep0048103)，通过碱熔改变了贵金属的状态，使其易于溶解，但原料中的SiO2碱熔融时形成硅酸盐，浸出时形成硅胶，使过滤困难。美国专利US4451290“从废料及残渣中回收铂族金属”是将含贵金属残渣与含硫浸滤渣及熔剂高温熔融，以产生含贵金属的铜锍相及浮渣，氧化除去多余的铁、镍，再用铜或镍、铁中选择的熔化金属与铜锍相接触，以捕集贵金属。此法发明了从含贵金属废料或废渣中用锍熔融法及铜捕集法结合富集贵金属的方法，方法是火法冶金，未涉及高品位贵金属精矿的制备及贵金属的活化和溶解，而且贵金属回收率除铂较高外，其余不高，特别是银及钯均较低。
本发明的目的是针对低品位(＜10％)或难处理的含贵金属(Au、Ag、Pt、Pd、Rh、Ir、Os、Ru)的物料，研究发明一种使所有贵金属进一步富集并活化，获得高品位贵金属精矿，再高效简便溶解，制备高浓度、杂质含量少的贵金属溶液的方法，有利于下一步溶剂萃取或其它贵金属精炼技术的采用进行。
所发明的低品位及难处理贵金属物料的富集活化溶解方法，包括熔炼金属锍、铝合金化、酸浸出贱金属、酸氧化介质溶解贵金属几个步骤，其特征在于：(1)低品位及难处理的含贵金属物料利用其含有的贱金属硫化物，或者量不够时添加铁、镍、铜及其它重有色金属硫化物中一种或数种，其比例为贵金属：贱金属(重量比)＝1∶1-25，加入熔点为550-1000℃的钠硼玻璃渣或能形成钠硼玻璃的造渣物料覆盖，在粘土或石墨坩埚中熔炼，温度为900-1300℃，保温时间0.5-1.5小时，贵金属捕集于锍相或金属相，物料中的造渣物如硅、钙等与钠硼玻璃覆盖渣形成熔点为790-850℃的钠-硼-硅玻璃体渣，锍与渣分离，渣复用一至二次，渣中贵金属可降至30g/t左右，锍中贵金属直收率＞99.6％；(2)将(1)所得富集了贵金属的锍加添铝，锍：铝(重量比)＝1∶0.5-3，在粘土或石墨坩埚中，温度1000-1200℃，进行熔炼铝合金化，保温时间10-30分钟；(3)将(2)步骤所得铝合金块在1-4mol/l稀盐酸或稀硫酸中加热溶解贱金属，保持溶液中铝及贱金属离子总浓度＜150g/l，温度＞90℃，固液分离，滤液不含贵金属，可排弃或并入贱金属回收系统，滤渣为品位＞50％的贵金属活性精矿；(4)将(3)所得贵金属活性精矿用盐酸加氧化剂溶解全部贵金属，溶液酸度为4-8mol/l，氧化剂为氯气或过氧化氢水溶液中任选一种，温度为80-100℃，溶解时间2-5小时，贵金属溶解率分别为：Au99.9％，Pt99.9％，Pd99.9％，Rh99.8％，Ir99.9 ％，Os99.6％，Ru99.6％左右，不溶渣量很少，贵金属含量很少(-1％)，可并入下批熔炼用或者，在(1)、(2)、(3)步骤处理后，(4)将(3)步骤所得固体贵金属活性精矿用已知方法先氧化蒸馏分离饿，钌；(5)将(4)所剩余渣用盐酸加氧化剂溶解其它贵金属，溶液酸度为4-8mol/l，氧化剂为氯气或过氧化氢水溶液中任选一种，温度为80-100℃，溶解时间2-5小时。
本发明的优点是：1、所能处理的物料适应范围宽，贵金属品位0.1-20％，贵金属∶贱金属＝1∶1-25，SiO2、Al2O3等造渣物含量较高的物料，难处理物料均可处理，2、在活化贵金属，使其转化为易溶解状态的同时，进一步分离了SiO2、Al2O3及贱金属。3、贵金属精矿品位高，活性好，贵金属溶解率及金属回收率高，4工艺过程简便，溶解过程迅速。
实施例
实例1，碱熔蒸馏锇、钌及HCl/Cl2溶解的不溶残渣贵金属富集物143.5g，成份为(％)：Au0.275 Pt5.57Pd0.925 Rh0.377 Ir1.35 OS0.075 Ru0.378，贱金属总和小于0.4％。
(1)加入Ni3S220g，FeS23g与残渣混合，用60gSiO2，75g B2O3，56gNa2CO3造渣物覆盖物料，在粘土坩埚中于1250℃熔炼，保温30分钟，冷却后渣与锍分离；(2)所获得的27.6g锍加45g铝在粘土坩埚中，在1150℃熔炼15分钟，得铝合金71.5g，铝渣4.67g；(3)将铝合金用3mol/lHcl；在温度＞90℃加热溶解，固液分离；(4)将(3)所得固体贵金属精矿用6mol/l HCl+过氧化氢溶解，温度为水沸腾温度，溶解10分钟，精矿全部溶完。
贵金属走向，溶解率如表1：表1名称 Au Pt Pd Rh Ir Os Ru炉渣成分g/t 49.2 390 200 35 23 25.9 41.6铝渣成分％ 0.125 2.37 0.409 0.17 0.32 0.128 0.2662盐酸浸出液成分g/l 痕 痕 痕 痕 痕 痕 痕贵金属溶液浓度g/l 0.92 18.98 3.07 1.28 4.67 0.231 1.269炉渣中分散率％ 3.1 1.2 3.7 1.6 0.30 5.98 1.89铝渣中分散率％ 1.5 1.4 1.4 1.47 0.77 5.6 2.3贵液中分配率％ 95.5 97.4 95.0 97.0 98.9 88.4 95.8金属平衡％ 100 100 100 100 100 100 100实例2
某厂贵金属富集物3780g，成份为(％)：Au0.113Pt0.094 Pd0.076 Rh0.0037 Ir0.0148Os0.00872 Ru0.0054 Cu4.76 Ni4.19Fe10.21 SiO211.1 Al2O3＜1S14.11CaO12.52 MgO1.39
其中ΣPt+Au＝0.3156％，贱金属19.166％，贵贱比1∶60，造渣物为26.01％。
(1)加入SiO2 1210g，硼砂1512g，Na2CO3 1134g造渣物料覆盖于物料上，在粘土坩埚中，于1250℃温度下熔炼0.5小时，冷却后渣锍分离，炉渣重2480g，锍重418.1g。
(2)按锍∶铝＝1∶1.5的比例，将锍和铝混合加入粘土坩埚中，中频电炉加热，于1150℃温度熔炼反应10分钟，得铝合金870g。
(3)铝合金经稀硫酸(浓度3mol/l)，温度＞90℃加热溶解后，过滤，洗涤，干燥，铝渣干重31.5g
(4)铝渣(贵金属精矿)先氧化蒸馏分离Os、Ru、再用8mol/1HCl通Cl2氧化，温度＞80℃，溶解1小时，过滤得贵金属溶液587.5ml，不溶渣干重1.51g，溶液中贵贱比为14∶1。
贵金属走向及溶解率如表2表2名称 Au Pt Pd Rh Ir Os Ru炉渣中含量g/t 7.5 17.7 7.7 4.3 6.62 2.15 2.14铝渣中含量g/t 180 168 137 4.4 15.0 390 380铝渣溶解液中含量g/l 痕 痕 痕 痕 痕 痕 痕最终不溶渣中含量g/t 798.95 1990 1010 224 752.7 914.5 562.6贵液中浓度g/l 7.22 6.06 4.84 0.23 0.946 0.0052 0.0216Os、Ru吸收液 / / / / / 0.34 0.123中浓度g/l炉渣中分散率 0.44 1.2 0.67 0.76 0.29 1.6 2.1铝渣中分散率 0.13 0.15 0.15 0.1 0.0 80.37 5.8最终不溶渣中 0.028 0.00 0.05 0.2 0.2 0.42 0.39残留率％贵金属溶液中 99.4 98.5 99.12 96.4 99.14 0.93 1.2分配率％Os、Ru吸 / / / / / 94.7 83.2中分配率％贵金属溶解率 99.97 99.92 99.95 99.8 99.8 99.58* 99.61*(蒸出率)*％金属平衡％ 100 100 100 100 100 100 100
实例3 某厂贵金属物料3605g，成分为(％)：Au1.46Pt3.58 Pd1.92 Rh0.16 Ir0.149 Os0.159 Ru0.32 Cu9.64 Ni7.98 Fe1.48 S33.04 SiO28.81 CaO1.78 Al2O30.66，其中Au+ΣPt＝7.748％，贱金属＝19.1％，贵贱比＝1∶2.5，造渣物＝11.25％，(1)加入361g SiO2，361g硼砂，2.89g Na2CO3造渣物混合后覆盖在物料上，在粘土坩埚中于1250℃温度下熔炼1.5小时，分层熔体倾倒放渣或冷却后渣锍分离，炉渣重1250g，锍重1455.7g。
(2)按锍∶铝＝1∶1.5比例，加入粘土坩埚中于1150℃温度下熔炼反应10分钟，得铝合金重3091.5g。
(3)铝合金用3mol/l盐酸溶解贱金属，温度＞90℃，不含贵金属的溶液废弃，得铝渣干重17.2g。
(4)铝渣(贵金属精矿)先氧化蒸馏Os、Ru后再用8molHcl通cl2加热溶解贵金属1.5小时，温度＞80℃，过滤贵金属溶液体积为2500ml，滤渣干重为13.1g，溶液中贵贱比为12.6∶1。
金属走向及溶解率如表3表3名称 Au Pt Pd Rh Ir Os Ru炉渣中含量g/t 5.3 6.3 3.8 4.0 2.93 1.35 1.86铝渣中含量g/t 1870 4102 5333 213 173 30 80盐酸溶解液中含量g/l 痕 痕 痕 痕 痕 痕 痕最终不溶渣中含量g/l 651 1965 1058 5000 415.7 376.1 784.9贵液中浓度g/l 21.06 51.67 27.65 2.27 2.12 0.95 2.63Os、Ru吸收液 / / / / / 1.24 1.81中浓度g/l炉渣中分散率％ 0.013 0.006 0.007 0.087 0.068 0.030 0.020铝渣中分散率％ 0.061 0.055 0.13 0.064 0.056 0.009 0.012最终不溶渣中 0.016 0.02 0.02 1.1 0.1 0.086 0.09残留率％贵金属溶液中 99.89 99.92 99.8 98.7 99.77 41.42 57.35分配率％Os、Ru吸收液 / / / / / 58.46 42.55中分配率％贵金属溶解率 99.98 99.98 99.98 98.9 99.9 99.9* 9.9*(蒸出率)*％金属平衡％ 100 100 100 100 100 100 100
Claims (2)
1、低品位及难处理贵金属物料的富集活化溶解方法，其特征在于：
1.1低品位及难处理贵金属物料利用其含有的贱金属硫化物，或添加铁、镍、铜及其它重有色金属硫化物中一种或数种，在钠硼玻璃渣或能形成钠硼玻璃渣的造渣物料的覆盖下熔炼，贵金属富集于金属锍中，物料中的造渣物与钠硼玻璃形成钠硼硅玻璃渣，锍与渣分离，具体条件为：贵金属∶贱金属(重量比)＝1∶1-25，钠硼玻璃渣熔化温度为550℃-1000℃，在粘土或石墨坩埚中熔炼，熔炼温度为900℃-1300℃，保温时间0.5-1.5小时，渣复用一至二次；
1.2将1.1所得金属锍添加铝熔炼进行铝合金化，锍∶铝(重量比)＝1∶0.5-3，温度1000-1200℃，保温时间10-30分钟，在粘土或石墨坩埚中进行；
1.3将1.2所得铝合金块，用稀盐酸或稀硫酸浸出贱金属，溶液酸度为1-4mol/l，溶液中铝及贱金属离子总浓度＜150g/l，温度＞90℃，固液分离；
1.4将1.3所得固体(贵金属富集物)用盐酸加氧化剂溶解全部贵金属，溶液酸度为4-8mol/l，氧化剂为氯气或过氧化氢水溶液中任选一种，温度为80-100℃，溶解时间2-5小时。
2、如权利要求1所述的低品位及难处理贵金属物料的富集活化溶解方法，其特征在于：
2.1低品位及难处理贵金属物料经熔炼金属锍、锍加铝熔炼铝合金化、铝合金加稀酸溶解分离贱金属后，将所得固体(贵金属富集物)用已知方法先氧化蒸馏锇、钌，
2.2将2.1所剩余渣用盐酸加氧化剂溶解其它贵金属，溶液酸度为4-8mol/l，氧化剂为氯气或过氧化氢水溶液中任选一种，温度为80-100℃，溶解时间2-5小时。
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| CN102962446B (zh) * | 2012-11-13 | 2014-06-18 | 中国科学院长春应用化学研究所 | 一种液相溶解活化贵金属纳米粒子的方法 |
| CN103526040B (zh) * | 2013-10-11 | 2015-08-12 | 金川集团股份有限公司 | 一种从含铂族金属物料中去除贱金属的工艺 |
| CN105296759A (zh) * | 2015-11-18 | 2016-02-03 | 金川集团股份有限公司 | 一种从铂族金属料液中选择性分离铜、镍的方法 |
| CN109321753B (zh) * | 2018-11-27 | 2020-01-31 | 贵研资源（易门）有限公司 | 失效钯催化剂绿色回收方法 |
| CN110846505A (zh) * | 2019-11-21 | 2020-02-28 | 云龙县铂翠贵金属科技有限公司 | 一种从VOCs废催化剂中回收铂族金属的方法 |
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| JPS58151434A (ja) * | 1982-03-02 | 1983-09-08 | Shoei Kagaku Kogyo Kk | パラジウムの採取方法 |
| US4451290A (en) * | 1981-09-16 | 1984-05-29 | Matthey Rustenburg Refiners (Proprietary) Limited | Recovery of platinum group metals from scrap and residues |
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| US4451290A (en) * | 1981-09-16 | 1984-05-29 | Matthey Rustenburg Refiners (Proprietary) Limited | Recovery of platinum group metals from scrap and residues |
| JPS58151434A (ja) * | 1982-03-02 | 1983-09-08 | Shoei Kagaku Kogyo Kk | パラジウムの採取方法 |
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