CN108946826A - A method of handling copper in nickeliferous cobalt sulfate solution, manganese impurity - Google Patents
A method of handling copper in nickeliferous cobalt sulfate solution, manganese impurity Download PDFInfo
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- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 title claims abstract description 48
- 229940044175 cobalt sulfate Drugs 0.000 title claims abstract description 47
- 229910000361 cobalt sulfate Inorganic materials 0.000 title claims abstract description 47
- 239000010949 copper Substances 0.000 title claims abstract description 44
- 239000011572 manganese Substances 0.000 title claims abstract description 41
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 36
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 33
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000012535 impurity Substances 0.000 title claims abstract description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 89
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 62
- 239000010941 cobalt Substances 0.000 claims abstract description 62
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 41
- 239000012074 organic phase Substances 0.000 claims abstract description 33
- 239000000344 soap Substances 0.000 claims abstract description 32
- 238000000605 extraction Methods 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012071 phase Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000003085 diluting agent Substances 0.000 claims abstract description 6
- 239000003350 kerosene Substances 0.000 claims abstract description 6
- 230000000717 retained effect Effects 0.000 claims abstract description 6
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 4
- 150000003841 chloride salts Chemical class 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000008346 aqueous phase Substances 0.000 claims description 2
- 238000010979 pH adjustment Methods 0.000 claims description 2
- 238000004065 wastewater treatment Methods 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241000220317 Rosa Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- -1 cobalt metals Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 150000004965 peroxy acids Chemical group 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/10—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/01—Preparation or separation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
本发明公开了一种处理含镍硫酸钴溶液中铜、锰杂质的方法，包括步骤：1）调节含镍硫酸钴原料液pH；2）制备P204钴皂：将萃取剂P204和稀释剂磺化煤油混合，依次加入NaOH溶液和钴皂前液，有机相为P204钴皂；3）利用P204钴皂萃取除铜、锰：将P204钴皂加入到硫酸钴原料液中，萃取，硫酸钴原料液中的铜、锰转入有机相，钴、镍保留到水相中，水相为含钴、镍的P204萃余液；4）洗钴：使未完全反应的P204钴皂中的钴转到水相中；5）反萃取：产出含钴低于1.0g/L的氯化盐反萃液。本发明能够有效地将铜、锰杂质从含镍硫酸钴溶液中除去，且不会引入其他杂质，产出的产品质量达到生产精制硫酸钴或精制氯化钴需求。The invention discloses a method for treating copper and manganese impurities in nickel-containing cobalt sulfate solution, comprising the steps of: 1) adjusting pH of nickel-containing cobalt sulfate raw material solution; 2) preparing P204 cobalt soap: sulfonating extractant P204 and diluent Mix kerosene, add NaOH solution and cobalt soap pre-liquid in sequence, the organic phase is P204 cobalt soap; 3) Use P204 cobalt soap to extract copper and manganese: add P204 cobalt soap to cobalt sulfate raw material solution, extract, cobalt sulfate raw material solution Copper and manganese in the liquid are transferred to the organic phase, cobalt and nickel are retained in the water phase, and the water phase is the P204 raffinate containing cobalt and nickel; 4) cobalt washing: the cobalt in the incompletely reacted P204 cobalt soap is transferred to in the water phase; 5) Back extraction: produce a chloride salt back extraction solution containing less than 1.0 g/L of cobalt. The invention can effectively remove copper and manganese impurities from the nickel-containing cobalt sulfate solution without introducing other impurities, and the quality of the produced product meets the requirements for producing refined cobalt sulfate or refined cobalt chloride.
Description
技术领域technical field
本发明属于有色金属冶炼技术领域，具体涉及一种处理含镍硫酸钴溶液中铜、锰杂质的方法。The invention belongs to the technical field of nonferrous metal smelting, and in particular relates to a method for treating copper and manganese impurities in a nickel-containing cobalt sulfate solution.
背景技术Background technique
工业硫酸钴，分子式为CoSO4·7H2O，玫瑰红色结晶，脱水后呈红色粉末，溶于水和甲醇，微溶于乙醇，用于陶瓷釉料、油漆催干剂，电镀、电池等领域，随着我国经济的快速发展，带动了新能源汽车行业对电池用硫酸钴产品的旺盛需求。Industrial cobalt sulfate, the molecular formula is CoSO4 7H2O, rose red crystal, red powder after dehydration, soluble in water and methanol, slightly soluble in ethanol, used in ceramic glaze, paint drier, electroplating, battery and other fields, with The rapid development of my country's economy has driven the strong demand for cobalt sulfate products for batteries in the new energy automobile industry.
关于含镍硫酸钴溶液中铜、锰杂质离子的去除，目前通用的方法有两种：方法一是粗制硫酸钴溶液→铜萃取剂预除铜→P204萃取除铜锰→含镍硫酸钴溶液；方法二是粗制硫酸钴溶液→P204萃取除铜锰→含镍硫酸钴溶液。Regarding the removal of copper and manganese impurity ions in nickel-containing cobalt sulfate solution, there are currently two common methods: method one is crude cobalt sulfate solution→copper extractant pre-removal of copper→P204 extraction to remove copper and manganese→nickel-containing cobalt sulfate solution The second method is crude cobalt sulfate solution → P204 extraction to remove copper and manganese → nickel-containing cobalt sulfate solution.
上述两种方法，作为硫酸盐体系下，处理粗制硫酸钴溶液的主要方法，主要存在以下缺点：1） 方法一通常用于处理含铜高于10g/L的低锰硫酸钴溶液，铜以含铜高酸的形式开路。2）方法二适用于铜、锰含量较低的低杂硫酸钴溶液。3）因为P204萃取剂对Cu/Co（或Mn/Co）的分离因子较低，总体来说，上述方法对杂质金属、钴金属浓度几乎相当的高锰硫酸钴溶液，往往需要多次P204萃取处理，才能实现杂质与钴的深度分离。The above two methods, as the main method for processing crude cobalt sulfate solution under the sulfate system, mainly have the following disadvantages: 1) Method one is usually used to process low-manganese cobalt sulfate solution containing copper higher than 10g/L. Copper-containing peracid forms an open circuit. 2) Method 2 is suitable for low-impurity cobalt sulfate solution with low copper and manganese content. 3) Because the separation factor of P204 extractant for Cu/Co (or Mn/Co) is low, in general, the above method often requires multiple P204 extractions for permanganese cobalt sulfate solutions with almost equal concentrations of impurity metals and cobalt metals Treatment can achieve deep separation of impurities and cobalt.
发明内容Contents of the invention
本发明为了克服上述两种处理方法的不足，解决高杂质硫酸钴溶液处理过程中铜、锰难以深度去除的难题，提供了一种去除含镍硫酸钴溶液中铜、锰等杂质的方法。In order to overcome the deficiencies of the above two treatment methods, the present invention solves the difficult problem of deep removal of copper and manganese during the treatment of high-impurity cobalt sulfate solution, and provides a method for removing impurities such as copper and manganese in nickel-containing cobalt sulfate solution.
本发明一种处理含镍硫酸钴溶液中铜、锰杂质的方法，包括以下步骤：A kind of method of the present invention handles copper, manganese impurity in nickel-containing cobalt sulfate solution, comprises the following steps:
a).调节含镍硫酸钴原料液pH：将硫酸钴溶液调节pH至2.5~4.0 ；a). Adjust the pH of the nickel-containing cobalt sulfate raw material solution: adjust the pH of the cobalt sulfate solution to 2.5 ~ 4.0;
b).制备P204钴皂：将萃取剂P204和稀释剂磺化煤油混合，依次加入30%的NaOH溶液和钴皂前液，形成的有机相为P204钴皂，并产出不含钴、镍的钴皂余液，钴皂余液排入废水处理系统，所述钴皂前液为Co2+浓度为60~80g/L的含镍硫酸钴溶液或含镍氯化钴溶液；b). Preparation of P204 cobalt soap: Mix extractant P204 and diluent sulfonated kerosene, add 30% NaOH solution and cobalt soap pre-liquid in sequence, the organic phase formed is P204 cobalt soap, and the output does not contain cobalt and nickel The cobalt soap residue, the cobalt soap residue is discharged into the waste water treatment system, and the liquid before the cobalt soap is Co Concentration is 60 ~ 80g/L nickel-containing cobalt sulfate solution or nickel-containing cobalt chloride solution;
c). 利用P204钴皂萃取除铜、锰：将步骤b制备的P204钴皂加入到步骤a 调节pH后的硫酸钴原料液中，控制有机相与水相流比为O/A=6:1～8:1，在常温下逆流萃取，使硫酸钴原料液中的铜、锰转入有机相，而钴、镍保留到水相中，进行有机相与水相分离，水相即为含钴、镍的P204萃余液；c). Use P204 cobalt soap to extract copper and manganese: add the P204 cobalt soap prepared in step b to the cobalt sulfate raw material solution after pH adjustment in step a, and control the flow ratio of the organic phase to the aqueous phase to be O/A=6: 1～8:1, countercurrent extraction at normal temperature, so that the copper and manganese in the cobalt sulfate raw material solution are transferred to the organic phase, while the cobalt and nickel are retained in the water phase, and the organic phase is separated from the water phase, and the water phase is cobalt-containing , P204 raffinate of nickel;
d). 洗钴：对步骤c中分离后的有机相用浓度为1.5～2.5mol/L的稀盐酸进行逆流洗涤，使未完全反应的P204钴皂中的钴转到水相中，钴的洗涤液并入步骤c之萃取过程重复利用；d). Cobalt washing: the organic phase separated in step c is countercurrently washed with dilute hydrochloric acid with a concentration of 1.5 to 2.5 mol/L, so that the cobalt in the incompletely reacted P204 cobalt soap is transferred to the water phase, and the cobalt The washing liquid is incorporated into the extraction process of step c for reuse;
e).反萃取：对步骤d中分离后的有机相用浓度为4.0~6.0mol/L的稀盐酸进行反萃取，产出含钴低于1.0g/L的氯化盐反萃液。e). Back-extraction: back-extract the organic phase separated in step d with dilute hydrochloric acid with a concentration of 4.0-6.0 mol/L to produce a chloride-salt back-extraction solution containing cobalt less than 1.0 g/L.
所述萃取剂的浓度为0.8～1.0mol/L；The concentration of the extractant is 0.8～1.0mol/L;
所述步骤b中钴皂前液与有机相进行至少5级逆流萃取；In the step b, the cobalt soap pre-liquid and the organic phase are subjected to at least 5 stages of countercurrent extraction;
所述步骤c中产出的P204萃余液充作步骤b的钴皂前液；The P204 raffinate produced in the step c is used as the cobalt soap pre-liquid of the step b;
所述步骤c中硫酸钴原料液与有机相进行至少8级逆流萃取；In the step c, the cobalt sulfate raw material liquid and the organic phase are subjected to at least 8 stages of countercurrent extraction;
所述步骤d中用稀盐酸对有机相进行至少5级逆流洗涤；In the step d, the organic phase is washed with dilute hydrochloric acid at least 5 stages of countercurrent;
所述步骤e中洗涤后的有机相进行至少5级逆流反萃取。The organic phase washed in step e is subjected to at least 5 stages of countercurrent back extraction.
本发明的有益技术效果：Beneficial technical effect of the present invention:
本发明能够有效地将铜、锰杂质从含镍硫酸钴溶液中除去，产出的含镍硫酸钴溶液中钴含量60-80g/L，铜含量低于0.001g/L，锰含量低于0.005g/L，产品质量达到精制硫酸钴或精制氯化钴需求；本发明工艺简单、可靠、可操作性强，铜、锰杂质与钴的分离深度高，且不会引入其他杂质，有着较好的经济价值。The invention can effectively remove copper and manganese impurities from the nickel-containing cobalt sulfate solution, and the cobalt content in the produced nickel-containing cobalt sulfate solution is 60-80g/L, the copper content is lower than 0.001g/L, and the manganese content is lower than 0.005 g/L, the product quality meets the requirements of refined cobalt sulfate or refined cobalt chloride; the process of the invention is simple, reliable, and operable, and the separation depth of copper, manganese impurities and cobalt is high, and other impurities will not be introduced, so it has better economic value.
具体实施方式Detailed ways
下面通过具体实施例对本发明的处理方法做进一步说明：The processing method of the present invention will be further described below by specific examples:
含镍硫酸钴原料液的组成为Ni：3.93g/L,Co：30.52g/L,Cu：2.17g/L,Mn：39.57g/L。The composition of the nickel-containing cobalt sulfate raw material solution is Ni: 3.93g/L, Co: 30.52g/L, Cu: 2.17g/L, Mn: 39.57g/L.
本发明萃取剂P204与被萃金属离子发生如下反应：The extraction agent P204 of the present invention reacts with the extracted metal ion as follows:
钴皂制备：HX+NaOH→Na2X+H2O （式中HX表示P204，下同）Cobalt soap preparation: HX+NaOH→Na 2 X+H 2 O (where HX represents P204, the same below)
Na2X +Co2+→CoX+Na+ Na 2 X +Co 2+ →CoX+Na +
钴皂萃取除铜、锰：CoX+M2+→MX+Co2+ （式中M表示Cu、Mn）Cobalt soap extraction to remove copper and manganese: CoX+M 2+ →MX+Co 2+ (where M represents Cu and Mn)
洗钴：CoX+H2+→HX+Co2+ Cobalt washing: CoX+H 2+ →HX+Co 2+
反萃：MX+H+-→HX+M2+ Stripping: MX+H +- →HX+M 2+
实施例1Example 1
将含镍硫酸钴溶液调节pH值至2.5，有机相由萃取剂P204和稀释剂磺化煤油组成，其中萃取剂P204的浓度为0.8mol/L，钴皂有机镍负载量为11.03g/L，萃取相比O/A=8/1，8级逆流萃取，使铜、锰转入有机相而镍、钴保留于水相中，然后用稀盐酸对有机相进行5级洗涤，洗涤相比O/A=15/1，将有机相中的钴分离出来并入萃取进料级，产出萃余液的组成为Ni：4.77g/L,Co：71.09g/L, Cu：0.00045g/L,Mn：0.0028g/L,pH3.0。洗涤后有机再使用稀盐酸进行5级反萃，产出的反萃液的组成为Ni：0.0077g/L,Co：0.75g/L, Cu：7.35g/L,Mn：147.3g/L。The pH value of nickel-containing cobalt sulfate solution is adjusted to 2.5, and the organic phase is composed of extractant P204 and diluent sulfonated kerosene, wherein the concentration of extractant P204 is 0.8mol/L, and the organic nickel loading of cobalt soap is 11.03g/L, Extraction ratio O/A=8/1, 8-stage countercurrent extraction, copper and manganese are transferred to the organic phase while nickel and cobalt are retained in the water phase, and then the organic phase is washed with dilute hydrochloric acid for 5 stages, and the washing ratio is O /A=15/1, the cobalt in the organic phase is separated and fed into the extraction feed stage, and the composition of the output raffinate is Ni: 4.77g/L, Co: 71.09g/L, Cu: 0.00045g/L , Mn: 0.0028g/L, pH3.0. After washing, organically use dilute hydrochloric acid for 5-stage stripping, and the composition of the produced stripping solution is Ni: 0.0077g/L, Co: 0.75g/L, Cu: 7.35g/L, Mn: 147.3g/L.
实施例2Example 2
将含镍硫酸钴溶液调节pH值至4.0，有机相由萃取剂P204和稀释剂磺化煤油组成，其中萃取剂P204的浓度为1.0mol/L，钴皂有机镍负载量为14.03g/L，萃取相比O/A=6/1，8级逆流萃取，使铜、锰转入有机相而镍、钴保留于水相中，然后用稀盐酸对有机相进行5级洗涤，洗涤相比O/A=30/1，将有机相中的钴分离出来并入萃取进料级，产出萃余液的组成为Ni：5.29g/L,Co：68.63g/L, Cu：0.00072g/L,Mn：0.0031g/L,pH3.0。洗涤后有机再使用稀盐酸进行5级反萃，产出的反萃液的组成为Ni：0.0059g/L,Co：0.87g/L, Cu：7.10g/L,Mn：172.37g/L。The pH value of nickel-containing cobalt sulfate solution is adjusted to 4.0, and the organic phase is composed of extractant P204 and diluent sulfonated kerosene, wherein the concentration of extractant P204 is 1.0mol/L, and the organic nickel loading of cobalt soap is 14.03g/L, Extraction ratio O/A=6/1, 8-stage countercurrent extraction, copper and manganese are transferred to the organic phase while nickel and cobalt are retained in the water phase, and then the organic phase is washed with dilute hydrochloric acid in 5 stages, and the washing ratio is O /A=30/1, the cobalt in the organic phase is separated and fed into the extraction feed stage, and the composition of the output raffinate is Ni: 5.29g/L, Co: 68.63g/L, Cu: 0.00072g/L , Mn: 0.0031g/L, pH3.0. After washing, dilute hydrochloric acid is used for 5-stage stripping, and the composition of the produced stripping liquid is Ni: 0.0059g/L, Co: 0.87g/L, Cu: 7.10g/L, Mn: 172.37g/L.
实施例3Example 3
将含镍硫酸钴溶液调节pH值至3.5，有机相由萃取剂P204和稀释剂磺化煤油组成，其中萃取剂P204的浓度为0.91mol/L，钴皂有机镍负载量为11.47g/L，萃取相比O/A=7/1，8级逆流萃取，使铜、锰转入有机相而镍、钴保留于水相中，然后用稀盐酸对有机相进行5级洗涤，洗涤相比O/A=22/1，将有机相中的钴分离出来并入萃取进料级，产出萃余液的组成为Ni：5.82g/L,Co：77.57g/L, Cu：0.00061g/L,Mn：0.0036g/L,pH3.0。洗涤后有机再使用稀盐酸进行5级反萃，产出的反萃液的组成为Ni：0.0045g/L,Co：0.92g/L, Cu：7.93g/L,Mn：169.53g/L。The pH value of nickel-containing cobalt sulfate solution is adjusted to 3.5, and the organic phase is composed of extractant P204 and diluent sulfonated kerosene, wherein the concentration of extractant P204 is 0.91mol/L, and the organic nickel loading of cobalt soap is 11.47g/L, Extraction ratio O/A=7/1, 8-stage countercurrent extraction, copper and manganese are transferred to the organic phase while nickel and cobalt are retained in the water phase, and then the organic phase is washed with dilute hydrochloric acid in 5 stages, and the washing ratio is O /A=22/1, the cobalt in the organic phase is separated and fed into the extraction feed stage, and the composition of the output raffinate is Ni: 5.82g/L, Co: 77.57g/L, Cu: 0.00061g/L , Mn: 0.0036g/L, pH3.0. After washing, organically use dilute hydrochloric acid for 5-stage stripping, and the composition of the produced stripping liquid is Ni: 0.0045g/L, Co: 0.92g/L, Cu: 7.93g/L, Mn: 169.53g/L.
以上所述的仅是本发明的较佳实施例，并不局限发明。应当指出对于本领域的普通技术人员来说，在本发明所提供的技术启示下，还可以做出其它等同改进，均可以实现本发明的目的，都应视为本发明的保护范围。The above descriptions are only preferred embodiments of the present invention, and do not limit the invention. It should be pointed out that for those skilled in the art, under the technical inspiration provided by the present invention, other equivalent improvements can also be made, all of which can achieve the purpose of the present invention, and should be regarded as the protection scope of the present invention.
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