CN115537569A - 一种湿法炼锌福美钠钴渣综合利用的方法 - Google Patents
一种湿法炼锌福美钠钴渣综合利用的方法 Download PDFInfo
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 150
- 239000010941 cobalt Substances 0.000 title claims abstract description 144
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 144
- 239000002893 slag Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 40
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 37
- 239000011701 zinc Substances 0.000 title claims abstract description 37
- GSFSVEDCYBDIGW-UHFFFAOYSA-N 2-(1,3-benzothiazol-2-yl)-6-chlorophenol Chemical compound OC1=C(Cl)C=CC=C1C1=NC2=CC=CC=C2S1 GSFSVEDCYBDIGW-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000009854 hydrometallurgy Methods 0.000 title claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 41
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 238000002386 leaching Methods 0.000 claims abstract description 35
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 31
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- 239000002904 solvent Substances 0.000 claims abstract description 18
- 238000007731 hot pressing Methods 0.000 claims abstract description 17
- 238000004090 dissolution Methods 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000000706 filtrate Substances 0.000 claims abstract description 13
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000001556 precipitation Methods 0.000 claims abstract description 9
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- IYPQZXRHDNGZEB-UHFFFAOYSA-N cobalt sodium Chemical compound [Na].[Co] IYPQZXRHDNGZEB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000004821 distillation Methods 0.000 claims description 2
- 238000004064 recycling Methods 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000779 smoke Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- 238000011084 recovery Methods 0.000 description 16
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 14
- 239000011734 sodium Substances 0.000 description 14
- 229910052708 sodium Inorganic materials 0.000 description 14
- NCTHNHPAQAVBEB-WGCWOXMQSA-M sodium ferulate Chemical compound [Na+].COC1=CC(\C=C\C([O-])=O)=CC=C1O NCTHNHPAQAVBEB-WGCWOXMQSA-M 0.000 description 10
- 239000002253 acid Substances 0.000 description 5
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- 238000005406 washing Methods 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- 239000005843 Thiram Substances 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 description 3
- 229960002447 thiram Drugs 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910001429 cobalt ion Inorganic materials 0.000 description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 239000005870 Ziram Substances 0.000 description 1
- 150000001462 antimony Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical class [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
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- 235000019633 pungent taste Nutrition 0.000 description 1
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- 238000011069 regeneration method Methods 0.000 description 1
- -1 sodium cobalt fumarate Chemical compound 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- DUBNHZYBDBBJHD-UHFFFAOYSA-L ziram Chemical compound [Zn+2].CN(C)C([S-])=S.CN(C)C([S-])=S DUBNHZYBDBBJHD-UHFFFAOYSA-L 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
本发明涉及一种湿法炼锌福美钠钴渣综合利用的方法,属于冶金工程技术领域。本发明以二甲苯为溶剂对福美钠钴渣进行热压溶解浸出得到有机浸出液;将固体烧碱加入到有机浸出液中进行钴沉淀反应,固液分离得到富钴渣和混合有机溶液;混合有机溶液蒸馏,挥发回收二甲苯溶剂,残留有机除钴剂钠盐;有机除钴剂钠盐进行热过滤,得到有机钠盐滤液和有机含钴滤渣,有机含钴滤渣返回进行热压溶解浸出;有机钠盐滤液冷却至室温得到福美钠除钴剂,福美钠除钴剂返回湿法炼锌净化除钴系统进行除钴。本发明采用全湿法工艺实现湿法炼锌福美钠钴渣分离钴及福美钠除钴剂回收利用,无焙烧烟气,具有较好的经济、社会和环保效益。
Description
技术领域
本发明涉及一种湿法炼锌福美钠钴渣综合利用的方法,属于冶金工程技术领域。
背景技术
湿法炼锌是当前最主要的炼锌方法,含锌矿物浸出后的溶液除含锌外,通常含有一定浓度的Cu、Cd、Co、Ni、As、Sb、Ge等杂质元素,在电积锌之前需要进行净化处理。目前硫酸锌浸出液的净化除钴工艺,主要有两种,一种是应用较为广泛的加砷盐或锑盐的锌粉置换法,另一种是近些年发展起来的特殊化学品净化法,主要是有机试剂沉淀除钴。随着锌精矿中钴镍等杂质的含量越来越高,锌粉置换除钴无法达到较高要求,特殊化学品除钴,因其除钴效率高,受到普遍关注,发展越来越快,应用较多的是福美锌或福美钠等。该方法产出的净化渣含有10~20%的锌、4~6%的钴,经酸洗脱锌后钴含量可达到10%左右,经济价值较大,钴渣综合回收可为企业带来可观的经济效益。
目前,湿法炼锌企业有机除钴剂净化钴渣,普遍采用酸洗+焙烧+还原浸出的工艺回收钴,酸洗实现锌、钴的有效分离,高温焙烧使有机除钴剂与钴离子结合形成的稳定钴螯合物分解,有机物被燃烧,钴金属形成可溶化合物富集,焙烧后采用还原浸出回收钴,其效率可达95%以上。但由于有机除钴剂净化钴渣具有刺激性味道,且硫与氮含量较高,有机物焙烧释放含硫、含氮气体造成一定环境污染,且未能实现有机除钴剂的循环再利用,不适应国家产业政策和发展循环经济的要求。
如何综合开发利用湿法炼锌行业的有机除钴剂净化钴渣,有效解决锌冶炼除钴渣对环境的污染,研究开发独具特色的工艺技术,综合回收其中有价金属,同时实现有机除钴剂回收利用,是发展循环经济、建设资源节约型和环境友好型社会的重要途径和紧迫任务。
发明内容
本发明针对湿法炼锌福美钠净化除钴技术中酸洗除锌后产生的福美钠钴渣渣的处理问题,提出了一种湿法炼锌福美钠钴渣综合利用的方法,本发明采用全湿法工艺实现湿法炼锌福美钠钴渣分离钴及福美钠除钴剂回收利用,无焙烧烟气。
一种湿法炼锌福美钠钴渣综合利用的方法,具体步骤如下:
(1)以二甲苯为溶剂对福美钠钴渣进行热压溶解浸出得到有机浸出液;
(2)将固体烧碱加入到有机浸出液中进行钴沉淀反应,固液分离得到富钴渣和混合有机溶液;
(3)混合有机溶液蒸馏,挥发回收二甲苯溶剂,残留有机除钴剂钠盐;
(4)有机除钴剂钠盐进行热过滤,得到有机钠盐滤液和有机含钴滤渣,有机含钴滤渣返回步骤(1)进行热压溶解浸出;
(5)有机钠盐滤液冷却至室温得到福美钠除钴剂,福美钠除钴剂返回湿法炼锌净化除钴系统进行除钴;回收福美钠除钴剂的过程仅需自然冷却降温,无需能耗。
所述步骤(1)福美钠钴渣与二甲苯的固液比g:L为50~100:1。
所述步骤(1)热压溶解浸出的温度为125~130℃,时间为60~120min。
所述步骤(2)固体烧碱与有机浸出液的固液比g:L为10~20:1。
所述步骤(2)钴沉淀反应温度为80~90℃,时间为30~40min。
所述步骤(3)蒸馏温度为145~150℃。
所述步骤(4)热过滤温度为80~90℃。
本发明的有益效果是:
(1)本发明全流程非水溶液体系,避免福美钠钴渣与水共热时生成二甲胺和二硫化碳;热压溶解过程采用有机试剂作为溶剂,控制溶解过程温度低于溶剂的沸点,避免溶剂挥发;控制溶解过程温度略高于于福美钠的熔点,避免福美钠热解挥发,进行福美钠钴渣的热压溶解,使钴离子溶解进入有机浸出液,过程清洁高效,无有机物污染;
(2)本发明过程仅需消耗烧碱,且具有双重作用。采用固体烧碱沉淀钴,同时将钠离子引入混合有机溶液形成有机除钴剂钠盐体系,以便获得有机钠盐滤液,实现福美钠再生;
(3)本发明福美钠除钴剂可循环利用。福美钠钴渣在分离富集钴的同时,实现了福美钠除钴剂回收利用,且回收福美钠过程仅需自然冷却降温,无需能耗;
附图说明
图1为本发明工艺流程图。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。
本发明实施例中采用的酸洗脱锌后的福美钠钴渣的主要成分为(质量百分数):Co8.12%,Zn 2.03%,Fe 1.36%,S 46.88%,C 20.71%,N 18.35%。
实施例1:一种湿法炼锌福美钠钴渣综合利用的方法(见图1),具体步骤如下:
(1)以二甲苯为溶剂对福美钠钴渣进行热压溶解浸出90min得到有机浸出液;其中福美钠钴渣与二甲苯的固液比g:L为50:1,热压溶解浸出温度为125℃;
(2)将固体烧碱加入到有机浸出液中,在温度90℃下进行钴沉淀反应30min,固液分离得到含钴47.52wt.%的富钴渣和混合有机溶液,钴回收率92.05%,富钴渣可用于钴回收精制;其中固体烧碱与有机浸出液福美钠钴渣的固液比g:L为10:1;
(3)混合有机溶液在温度150℃下蒸馏,挥发回收二甲苯溶剂,二甲苯溶剂回收率为95.31%,残留有机除钴剂钠盐;
(4)有机除钴剂钠盐在温度90℃下进行热过滤,得到有机钠盐滤液和含钴4.12%的有机含钴滤渣,有机含钴滤渣量为福美钠钴渣质量的16.03%,有机含钴滤渣返回步骤(1)进行热压溶解浸出;
(5)有机钠盐滤液自然冷却至室温(25℃)得到福美钠除钴剂,实现福美钠除钴剂的回收,回收率95.08%,福美钠除钴剂返回湿法炼锌净化除钴系统进行除钴;回收福美钠除钴剂的过程仅需自然冷却降温,无需能耗。
实施例2:一种湿法炼锌福美钠钴渣综合利用的方法(见图1),具体步骤如下:
(1)以二甲苯为溶剂对福美钠钴渣进行热压溶解浸出60min得到有机浸出液;其中福美钠钴渣与二甲苯的固液比g:L为80:1,热压溶解浸出温度为130℃;
(2)将固体烧碱加入到有机浸出液中,在温度90℃下进行钴沉淀反应40min,固液分离得到含钴49.35wt.%的富钴渣和混合有机溶液,钴回收率92.17%,富钴渣可用于钴回收精制;其中固体烧碱与有机浸出液福美钠钴渣的固液比g:L为15:1;
(3)混合有机溶液在温度145℃下蒸馏,挥发回收二甲苯溶剂,二甲苯溶剂回收率为94.78%,残留有机除钴剂钠盐;
(4)有机除钴剂钠盐在温度80℃下进行热过滤,得到有机钠盐滤液和含钴3.42%的有机含钴滤渣,有机含钴滤渣量为福美钠钴渣质量的15.26%,有机含钴滤渣返回步骤(1)进行热压溶解浸出;
(5)有机钠盐滤液自然冷却至室温(20℃)得到福美钠除钴剂,实现福美钠除钴剂的回收,回收率96.58%,福美钠除钴剂返回湿法炼锌净化除钴系统进行除钴;回收福美钠除钴剂的过程仅需自然冷却降温,无需能耗。
实施例3:一种湿法炼锌福美钠钴渣综合利用的方法(见图1),具体步骤如下:
(1)以二甲苯为溶剂对福美钠钴渣进行热压溶解浸出120min得到有机浸出液;其中福美钠钴渣与二甲苯的固液比g:L为100:1,热压溶解浸出温度为130℃;
(2)将固体烧碱加入到有机浸出液中,在温度80℃下进行钴沉淀反应35min,固液分离得到含钴48.29wt.%的富钴渣和混合有机溶液,钴回收率91.86%,富钴渣可用于钴回收精制;其中固体烧碱与有机浸出液福美钠钴渣的固液比g:L为20:1;
(3)混合有机溶液在温度145℃下蒸馏,挥发回收二甲苯溶剂,二甲苯溶剂回收率为95.06%,残留有机除钴剂钠盐;
(4)有机除钴剂钠盐在温度80℃下进行热过滤,得到有机钠盐滤液和含钴3.61%的有机含钴滤渣,有机含钴滤渣量为福美钠钴渣质量的16.71%,有机含钴滤渣返回步骤(1)进行热压溶解浸出;
(5)有机钠盐滤液自然冷却至室温(15℃)得到福美钠除钴剂,实现福美钠除钴剂的回收,回收率97.32%,福美钠除钴剂返回湿法炼锌净化除钴系统进行除钴;回收福美钠除钴剂的过程仅需自然冷却降温,无需能耗。
以上对本发明的具体实施方式作了详细说明,但是本发明并不限于上述实施方式,在本领域普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下作出各种变化。
Claims (7)
1.一种湿法炼锌福美钠钴渣综合利用的方法,其特征在于,具体步骤如下:
(1)以二甲苯为溶剂对福美钠钴渣进行热压溶解浸出得到有机浸出液;
(2)将固体烧碱加入到有机浸出液中进行钴沉淀反应,固液分离得到富钴渣和混合有机溶液;
(3)混合有机溶液蒸馏,挥发回收二甲苯溶剂,残留有机除钴剂钠盐;
(4)有机除钴剂钠盐进行热过滤,得到有机钠盐滤液和有机含钴滤渣,有机含钴滤渣返回步骤(1)进行热压溶解浸出;
(5)有机钠盐滤液冷却至室温得到福美钠除钴剂,福美钠除钴剂返回湿法炼锌净化除钴系统进行除钴。
2.根据权利要求1所述湿法炼锌福美钠钴渣综合利用的方法,其特征在于:步骤(1)福美钠钴渣与二甲苯的固液比g:L为50~100:1。
3.根据权利要求1所述湿法炼锌福美钠钴渣综合利用的方法,其特征在于:步骤(1)热压溶解浸出的温度为125~130℃,时间为60~120min。
4.根据权利要求1所述湿法炼锌福美钠钴渣综合利用的方法,其特征在于:步骤(2)固体烧碱与有机浸出液的固液比g:L为10~20:1。
5.根据权利要求1所述湿法炼锌福美钠钴渣综合利用的方法,其特征在于:步骤(2)钴沉淀反应温度为80~90℃,时间为30~40min。
6.根据权利要求1所述湿法炼锌福美钠钴渣综合利用的方法,其特征在于:步骤(3)蒸馏温度为145~150℃。
7.根据权利要求1所述湿法炼锌福美钠钴渣综合利用的方法,其特征在于:步骤(4)热过滤温度为80~90℃。
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