CN104603858A - 从含锰材料的氧化物中回收金属有价值物 - Google Patents
从含锰材料的氧化物中回收金属有价值物 Download PDFInfo
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Abstract
一种改良的用于处理含锰材料如通过海底采矿回收的结核矿的方法,所述方法包括使所述材料与氨反应,以及用无机酸浸提,并且涉及用于从这样的结核矿中回收有价值成分尤其是锰、钴、镍、铁、铜、钛、钒、铈和钼的方法。还公开了一种用于硝酸盐产品的生产的方法。
Description
发明领域
本发明涉及用于通过使用氨气处理含锰材料如氧化物、碳酸盐和矿石的方法。本发明非常适合处理通过海底采矿回收的多金属含锰结核矿(nodule),并且具体涉及用于从这样的结核矿中回收有价值成分尤其是锰、钴、镍、铜和铁的方法。
发明背景
多金属结核矿或锰结核矿是由在核心周围的铁和锰氢氧化物的同心层形成的岩石凝结物。
在大洋底部上的海底结核矿包括在其组成中包含锰(Mn),并且通常包含Ni、Co、Cu、Zn和Fe,以及少量的钛、钒、钼和铈。此外经常存在以下金属中的一种或多种:镁、铝、钙、镉、钾、钠、锆、钛、铅、磷和钡。深海结核矿通常含有约28%Mn、约10%FeO、约1%Cu和约1.2%Ni。
锰结核矿中大多数所需的有价值金属与不溶性的氧化的锰如MnO2结合。少于10%的含于结核矿中的锰是酸溶性的。因此,为了回收金属成分,作为第一步,必须用适合的还原剂还原MnO2。在过去,SO2已经用于此目的,并且一氧化碳(CO)已经用于铜回收过程。然而这种现有技术工艺通常并不能回收适合的锰产物,并且能够回收仅约80至约92%的主要金属有价值物(metal values),并且通常产生大量的废料,其可能包含未被完全移除的金属组分。
发明概述
通过本发明处理的含锰材料不仅可以包括矿石或深海结核矿,而且还可以包括携带氧化锰的电池如锌-碳、碱性和锂(LMO或LiMn2O4)电池,或者其他任何形式的含锰矿物或物质。
本发明是用于通过在水溶液中用氨处理含锰材料而从包括深海锰结核矿在内的海底含锰材料中回收锰和其他金属有价值物(“有利可图的金属(pay metal)”)(如果存在的话)的方法。气态NH3与矿石反应
7MnO2(s)+2NH3(g)->7MnO(s)+3H2O(1)+2NO2(g)
释放了捕获的所需有价值金属。一吨的NH3比8吨的SO2更有效。
在用氨气将MnO2还原后,可以使用任何无机酸从起始含锰材料中浸提并回收锰和其他金属。硝酸是优选的浸提材料,因为在氨反应中由H2O和NO2形成一些硝酸。
本发明尤其可用于制造硝酸盐产品,如***、肥料或其他硝酸盐。
发明目的
本发明的主要目的是提供改良的从携带锰的材料中,包括从海底锰结核矿中回收锰的方法。
本发明的另一个目的是提供有效的用于从携带锰的材料中回收金属有价值物的方法,所述金属有价值物(如果存在的话)包括任何镍、钴、铜、镁、铝、铁、钙、镉、钾、钠、锆、钛、锌、铅、铈、钼、磷、钡和钒。
本发明的另一个目的是提供有效的从包括深海锰结核矿在内的海底含锰材料中回收其他金属有价值物的方法。
本发明的另一个目的是生产硝酸盐产品。
附图简述
通过参照下文的详细描述和附图,前述和其他目的将变得更加显而易见,其中:
唯一的图是本发明的方法的优选实施方案的图解的流程图。
详细描述
现在参照附图,该方法以可以从大洋、海或其他水体得到的含锰材料10如深海锰结核矿开始。有时在大型湖泊中发现此类结核矿。深海结核矿含有超过20%的锰,通常约28%。
除了锰之外,此类深海结核矿可以含有以下金属中的至少一种:镍、钴、铜、镁、铝、铁、钙、镉、钾、钠、锆、钛、锌、铈、钼、磷、钡、铅和钒。本发明的方法包括这些金属有价值物中的许多种的有效浸提和回收。
任选地,将结核矿或其他含锰材料粉碎或研磨以增加用于稍后的反应的表面积。有利地,通过任何方便的方法,如洗涤,优选用水洗涤,移除结核矿中的任何氯化物。可以在任何粉碎之前、期间或之后完成此步骤,但是优选在粉碎之后。
在12中,结核矿在提高的温度下与氨反应。气态NH3与氧化锰矿石根据以下方程式反应:
7MnO2+2NH3->7MnO+3H2O+2NO2
在步骤14中,NH3与MnO2反应形成MnO、水和NO2,并且从结核矿中释放其他金属。NO2可以作为气体被移除或者反应形成硝酸。
在用氨将MnO2还原后,可以在浸提步骤16中使用任何无机酸从起始含锰材料中浸提并回收锰和其他金属盐18。硝酸是优选的浸提材料,因为在氨反应中形成一些硝酸。
在20中,使有利可图的金属从浸提步骤中形成的金属盐中沉淀并回收。在浸提后,然后将溶液的pH改变至约2.2-2.3以使水合氧化铁(FeOOH·H2O)沉淀。通过溶液的过滤移除沉淀的铁有价值物。可以通过多种方式获得这种pH变化,包括向溶液中加入氨或碱土金属氢氧化物如Mg(OH)2或Ca(OH)2,碱土金属氧化物如MgO或CaO,或碱土金属碳酸盐如Mg(CO3)2或Ca(CO3)2。
溶液中存在的任何铜、铅、镉和锌也从其中移除。一旦在溶液中,金属有价值物就可以作为氧化物或硫化物沉淀。优选地,将溶液调节至低pH,将硫化氢(H2S)或NaHS引入至溶液中,以使溶液中存在的任何铜、铅、镉和锌作为硫化物沉淀,并且通过过滤移除沉淀的金属有价值物。
然后提高溶液的pH,再次将硫化氢或NaHS加入至溶液中,以使钴和镍作为硫化物沉淀。在此步骤中还可以将铝和一些剩余的锌作为硫化物沉淀。
优选地,之后在22中将溶液的pH提高至约9以沉淀并回收锰氧化物和氢氧化物。在过滤残留物后,剩余的溶液是硝酸盐产品26,其可以被用作肥料,或用作硝酸盐的来源以在该方法中再次使用。
备选实施方案
备选地,含锰材料可以来源于工业废物或化学加工,或者是来自陆地采矿操作的含有锰的矿石,或者是从加工此类矿石中得到的含锰材料。含锰材料可以是通过从任何水体获得的多金属结核矿的现有化学或冶金处理得到的。
可以加热NH3或含锰材料或二者以增强反应。此外,可以在该方法中使用液氨,但是气态氨是优选的。
发明目的的达成的概述
根据前述,显而易见的是我们已经发明了改良的用于处理含锰材料的方法,其包括处理通过海底采矿回收的海底锰结核矿,以有效地使材料与氨反应,从而制备氧化锰产物并释放任何有价值金属,并且所述方法还用于有效地回收结核矿中包含的金属有价值物。我们也已经发明了改良的从含锰材料中回收锰的方法,其包括从携带锰的材料中回收其他金属有价值物,此类金属有价值物(如果存在的话)包括镍、钴、铜、镁、铝、铁、钙、镉、钾、钠、锆、钛、锌、铅、铈、钼、磷、钡和钒;以及有效的从包括深海锰结核矿在内的海底含锰材料中回收金属有价值物并且用于制造硝酸盐产品的方法。
应该理解的是,前述描述和具体的实施方案仅是说明本发明的最佳方式及其原理,并且本领域技术人员可以在不背离本发明的精神和范围的情况下对装置做出各种修改和补充。
Claims (18)
1.一种从含锰材料中回收金属有价值物的方法,所述方法包括以下步骤:
a.获得还含有其他金属的含锰材料;
b.使所述含锰材料与NH3反应以形成MnO并且释放所述其他金属;
c.用无机酸浸提反应后的材料以形成金属盐;
d.从所述金属盐中沉淀并回收有利可图的金属;以及
e.沉淀并回收锰氧化物和氢氧化物。
2.根据权利要求1所述的方法,其中所述含锰材料是从任何水体获得的多金属结核矿。
3.根据权利要求2所述的方法,其中所述含锰材料是深海锰结核矿。
4.根据权利要求1所述的方法,其中所述含锰材料是通过海底采矿回收的含锰结核矿。
5.根据权利要求1所述的方法,其中所述含锰材料是通过从任何水体获得的多金属结核矿的化学或冶金处理得到的。
6.根据权利要求5所述的方法,所述方法还包括粉碎或研磨所述结核矿。
7.根据权利要求1所述的方法,所述方法还包括通过洗涤所述含锰材料从所述材料中移除氯化物。
8.根据权利要求1所述的方法,其中步骤b在提高的温度下进行。
9.根据权利要求1所述的方法,其中所述含锰材料还含有由以下各项组成的组的金属中的至少一种:镍、钴、铁、铜、镁、铝、钙、镉、钾、钠、锆、钛、锌、铅、铈、钼、磷、钡和钒,所述方法还包括:
a.将碱土金属氧化物、氢氧化物或碳酸盐加入至所述溶液以使任何铁作为氢氧化铁沉淀;
b.从所述溶液中过滤残留物;
c.使在所述溶液中存在的任何铜、铅和镉作为硫化物沉淀;以及
d.使任何钴和镍的硫化物沉淀,留下碱土金属硝酸盐。
10.根据权利要求1所述的方法,其中通过将所述溶液调节至低pH并将H2S或NaHS引入至所述溶液并且形成硫化物,来完成任何铜、铅或镉从所述溶液中的沉淀。
11.根据权利要求1所述的方法,其中通过提高所述溶液的pH并且将附加的H2S或NaHS引入至其中而进行钴和镍的硫化物的沉淀。
12.根据权利要求1所述的方法,其中通过将所述溶液pH提高至约9进行锰氧化物和氢氧化物的沉淀。
13.一种通过权利要求1所述的方法制备的硝酸盐产品。
14.一种通过权利要求1所述的方法制备的可再循环硝酸盐。
15.一种通过权利要求1所述的方法制备的硝酸盐肥料产品。
16.根据权利要求1所述的方法,其中所述含锰材料还含有铁,所述方法还包括:
a.将碱土金属氧化物、氢氧化物或碳酸盐加入至所述溶液以使氢氧化铁沉淀;以及
b.从所述溶液中过滤残留物。
17.根据权利要求1所述的方法,其中所述含锰材料还含有铜、铅和镉,所述方法还包括使在所述溶液中存在的铜、铅和镉作为硫化物沉淀。
18.根据权利要求1所述的方法,其中所述含锰材料还含有钴和镍,所述方法还包括使钴和镍的硫化物沉淀,从而留下碱土硝酸盐的步骤。
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CN111286605A (zh) * | 2018-12-06 | 2020-06-16 | 深圳市金航深海矿产开发集团有限公司 | 一种海底多金属结核有价金属回收以及联产ncm前驱体的方法 |
CN111455171A (zh) * | 2019-01-22 | 2020-07-28 | 深圳市金航深海矿产开发集团有限公司 | 一种海底多金属结核提取有价金属并联产锂电正极材料前驱体及掺钛正极材料的方法 |
WO2024108773A1 (zh) * | 2022-11-22 | 2024-05-30 | 广东邦普循环科技有限公司 | 一种废锂电池的回收处理方法 |
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EP2912649A4 (en) | 2016-06-01 |
US9284627B2 (en) | 2016-03-15 |
CA2878528C (en) | 2016-10-11 |
MX353785B (es) | 2018-01-29 |
KR20150040364A (ko) | 2015-04-14 |
FR3009828A1 (fr) | 2015-02-27 |
WO2014066169A1 (en) | 2014-05-01 |
TWI494439B (zh) | 2015-08-01 |
US20150218672A1 (en) | 2015-08-06 |
TW201435091A (zh) | 2014-09-16 |
AU2013335006B2 (en) | 2015-07-16 |
CN104603858B (zh) | 2017-04-05 |
CA2878528A1 (en) | 2014-05-01 |
AU2013335006A1 (en) | 2014-11-20 |
MX2014014398A (es) | 2015-05-11 |
PH12015500037A1 (en) | 2015-03-02 |
JP6182216B2 (ja) | 2017-08-16 |
RU2015108064A (ru) | 2016-12-20 |
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FR3009828B1 (fr) | 2016-01-08 |
RU2610103C2 (ru) | 2017-02-07 |
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