CN103757311A - Method for leaching positive-negative pole material mixture of waste nickel-metal hydride battery - Google Patents
Method for leaching positive-negative pole material mixture of waste nickel-metal hydride battery Download PDFInfo
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- 238000002386 leaching Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000002699 waste material Substances 0.000 title claims abstract description 10
- 229910052987 metal hydride Inorganic materials 0.000 title description 11
- 239000000203 mixture Substances 0.000 title description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 16
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 238000002347 injection Methods 0.000 claims abstract description 3
- 239000007924 injection Substances 0.000 claims abstract description 3
- 238000005086 pumping Methods 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 150000002739 metals Chemical class 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 abstract description 6
- 235000010265 sodium sulphite Nutrition 0.000 abstract description 6
- 239000010926 waste battery Substances 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 26
- 229910017052 cobalt Inorganic materials 0.000 description 12
- 239000010941 cobalt Substances 0.000 description 12
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 12
- 229910052759 nickel Inorganic materials 0.000 description 12
- 229910052761 rare earth metal Inorganic materials 0.000 description 8
- 150000002910 rare earth metals Chemical class 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018095 Ni-MH Inorganic materials 0.000 description 1
- 229910018477 Ni—MH Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
Classifications
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- 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
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- Manufacture And Refinement Of Metals (AREA)
Abstract
本发明介绍的镍氢废电池正负极混合材料的浸出方法是将从镍氢废电池中分离出分离出的并经焙烧预处理得到的正负极混合材料放入耐压和耐硫酸腐蚀的容器中，并将硫酸泵入该容器，然后密封容器，并用注入泵将Na2SO3溶液泵入容器，此后关闭Na2SO3溶液泵入阀门进行浸出。The method for leaching the positive and negative mixed materials of nickel-hydrogen waste batteries introduced in the present invention is to put the positive and negative mixed materials separated from the waste nickel-hydrogen batteries and obtained through roasting pretreatment into a pressure-resistant and sulfuric acid corrosion-resistant The container, and pump sulfuric acid into the container, then seal the container, and use the injection pump to pump the Na2SO3 solution into the container, and then close the Na2SO3 solution pumping valve for leaching.
Description
技术领域 technical field
本发明涉及镍氢废电池正负极混合材料的一种浸出方法。 The invention relates to a method for leaching mixed positive and negative electrodes of waste nickel-metal hydride batteries.
背景技术 Background technique
镍氢电池是一类广泛使用的电池，该电池使用报废后将产生大量废电池。由于这类电池含有大量重金属，若弃入环境，将对环境产生很大的直接和潜在危害。镍氢废电池正负极混合材料主要含镍、钴和稀土，三者的总含量高达75～97%，很具回收价值。目前从镍氢废电池正负极混合材料中回收镍、钴和稀土的工艺主要有火法工艺和湿法工艺。火法工艺得到的产品为合金材料，很难获得较纯的镍、钴和稀土。湿法工艺比较容易得到较纯的镍、钴和稀土。浸出是湿法工艺中必不可少的一个过程。目前镍氢废电池正负极混合材料的浸出方法主要有盐酸浸出法、硫酸浸出法、硝酸浸出法和混酸（硫酸加硝酸）浸出法。盐酸浸出法的设备腐蚀大，酸雾产生量大而污染环境。硫酸浸出法消耗较昂贵的还原剂（如双氧水等），而且浸出速度较慢，酸耗高。硝酸浸出法的硝酸消耗量大，而且会产生大量氮氧化物，污染环境。所有的湿法工艺都存在如何经济地提高浸出速度、提高金属浸出率、降低酸耗和其它辅料消耗的问题。虽然硝酸加工业纯氧浸出法和混酸加工业纯氧浸出法较好地解决了上述问题，但浸出设备较复杂，而且废电池浸出所需工业纯氧量不大，废电池处理企业就地生产工业纯氧自用不经济，工业纯氧的储存、运输和使用比较麻烦。开发设备腐蚀小、浸出速度快、浸出率高、酸耗和其它辅料消耗低、使用方便、基本无环境污染的镍氢废电池正负极混合材料的浸出方法具有较大实用价值。 Ni-MH batteries are a type of batteries widely used, and a large amount of waste batteries will be produced after the batteries are scrapped. Because this type of battery contains a large amount of heavy metals, if it is discarded into the environment, it will cause great direct and potential harm to the environment. The positive and negative mixed materials of nickel-metal hydride batteries mainly contain nickel, cobalt and rare earth, and the total content of the three is as high as 75-97%, which is very valuable for recycling. At present, the processes for recovering nickel, cobalt and rare earth from the positive and negative mixed materials of nickel-metal hydride batteries mainly include pyrotechnics and wet processes. The products obtained by the fire process are alloy materials, and it is difficult to obtain relatively pure nickel, cobalt and rare earth. The wet process is relatively easy to obtain relatively pure nickel, cobalt and rare earth. Leaching is an essential process in the wet process. At present, the leaching methods of the mixed positive and negative electrodes of nickel-metal hydride batteries mainly include hydrochloric acid leaching method, sulfuric acid leaching method, nitric acid leaching method and mixed acid (sulfuric acid plus nitric acid) leaching method. The equipment of the hydrochloric acid leaching method is highly corroded, and the amount of acid mist generated is large and pollutes the environment. Sulfuric acid leaching consumes more expensive reducing agents (such as hydrogen peroxide, etc.), and the leaching speed is slow and the acid consumption is high. The consumption of nitric acid in the nitric acid leaching method is large, and a large amount of nitrogen oxides will be produced, which will pollute the environment. All wet processes have the problem of how to economically increase the leaching speed, increase the metal leaching rate, and reduce the consumption of acid and other auxiliary materials. Although the pure oxygen leaching method in the nitric acid processing industry and the pure oxygen leaching method in the mixed acid processing industry have solved the above problems, the leaching equipment is relatively complicated, and the amount of industrial pure oxygen required for the leaching of waste batteries is not large, and waste battery treatment enterprises produce on-site Industrial pure oxygen is not economical for personal use, and the storage, transportation and use of industrial pure oxygen are troublesome. It is of great practical value to develop a leaching method for the mixed positive and negative electrodes of nickel-metal hydride batteries with low equipment corrosion, fast leaching speed, high leaching rate, low acid consumption and other auxiliary material consumption, convenient use, and basically no environmental pollution.
the
发明内容 Contents of the invention
针对目前镍氢废电池正负极混合材料浸出的问题，本发明的目的是寻找一种金属浸出率高，使用方便，不用昂贵还原剂，基本无氮氧化物污染的镍氢废电池正负极混合材料的浸出方法，其特征在于将从镍氢废电池中分离出分离出的并经焙烧预处理得到的正负极混合材料放入耐压和耐硫酸腐蚀的容器中，并将硫酸泵入该容器，然后密封容器，并用注入泵将Na2SO3溶液泵入容器，此后关闭Na2SO3溶液泵入阀门进行浸出，浸出结束后 进行液固分离，得到所需浸出溶液。反应温度为40℃～80℃, 浸出的硫酸初始浓度为1mol/L～4mol/L, 浸出时间为1h～3h，浸出过程进行搅拌，搅拌速度为30r/min～120r/min。硫酸加入量为加入反应容器的正负极混合材料中全部金属浸出的硫酸理论消耗量的110%～150%。Na2SO3的加入量为将正负极混合材料中全部高价金属还原为低价金属的Na2SO3理论消耗量的105%～120%。 Aiming at the current problem of leaching the positive and negative mixed materials of waste nickel-hydrogen batteries, the purpose of this invention is to find a positive and negative electrode of spent nickel-hydrogen batteries that has a high metal leaching rate, is easy to use, does not require expensive reducing agents, and is basically free from nitrogen oxide pollution. The leaching method of the mixed material is characterized in that the positive and negative mixed materials separated from the waste nickel-metal hydride batteries and obtained through roasting pretreatment are put into a pressure-resistant and sulfuric acid corrosion-resistant container, and the sulfuric acid is pumped into the Then seal the container, and use the injection pump to pump the Na2SO3 solution into the container, then close the Na2SO3 solution pumping valve for leaching, and perform liquid-solid separation after leaching to obtain the required leaching solution. The reaction temperature is 40°C-80°C, the initial concentration of leached sulfuric acid is 1mol/L-4mol/L, the leaching time is 1h-3h, the leaching process is stirred, and the stirring speed is 30r/min-120r/min. The amount of sulfuric acid added is 110% to 150% of the theoretical consumption of sulfuric acid for leaching all the metals in the positive and negative mixed materials added to the reaction vessel. The amount of Na 2 SO 3 added is 105% to 120% of the theoretical consumption of Na 2 SO 3 for reducing all high-valent metals in the positive and negative electrode mixture materials to low-valent metals.
本发明的目的是这样实现的：在密闭和Na2SO3存在的条件下，硫酸浸出经焙烧预处理后的镍氢废电池正负极混合材料（材料中的镍、钴和稀土呈氧化物形态）时，浸出过程发生如下主要化学反应： The object of the present invention is achieved like this: under airtight and Na2SO3Under the condition that exists, sulfuric acid leaches the mixed positive and negative electrodes of nickel-metal hydride batteries (nickel, cobalt and rare earth in the material are oxides after roasting pretreatment) form), the following main chemical reactions occur during the leaching process:
NiO + H2SO4 = NiSO4 + H2O NiO + H2SO4 = NiSO4 + H2O
Ni2O3 + 2H2SO4 + Na2SO3 = 2NiSO4 + Na2SO4 + 2H2O Ni 2 O 3 + 2H 2 SO 4 + Na 2 SO 3 = 2NiSO 4 + Na 2 SO 4 + 2H 2 O
CoO + H2SO4 = CoSO4 + H2O CoO + H2SO4 = CoSO4 + H2O
Co2O3 + 2H2SO4 + Na2SO3 = 2CoSO4 + Na2SO4 + 2H2O Co 2 O 3 + 2H 2 SO 4 + Na 2 SO 3 = 2CoSO 4 + Na 2 SO 4 + 2H 2 O
Re2O3 + 3H2SO4 = Re2(SO4)3 + 3H2O Re 2 O 3 + 3H 2 SO 4 = Re 2 (SO 4 ) 3 + 3H 2 O
由于Na2SO3的还原能力比现有浸出方法中普遍使用的双氧水的还原能力强得多，而且不需要在强酸性环境下才能还原，这样可以降低浸出过程的酸度，减少硫酸和还原剂的消耗，提高反应速度。Na2SO3可以彻底破坏正负极混合材料中高价氧化物的层状结构，提高有价金属的浸出率。Na2SO3与H2SO4反应生成H2SO3和SO2，这些生成物与Ni2O3和Co2O3反应被消耗掉，由于SO2在水溶液中有一定的溶解度，释放在反应器上部空间中的SO2较少，而且随着反应的进行，SO2将不断被消耗，所以整个反应在微正压下进行。 Since the reducing power of Na2SO3 is much stronger than that of hydrogen peroxide commonly used in existing leaching methods, and it does not need to be reduced in a strongly acidic environment, it can reduce the acidity of the leaching process and reduce the amount of sulfuric acid and reducing agents. Consumption, increase reaction speed. Na 2 SO 3 can completely destroy the layered structure of high-valent oxides in the positive and negative mixed materials, and improve the leaching rate of valuable metals. Na 2 SO 3 reacts with H 2 SO 4 to generate H 2 SO 3 and SO 2 , and these products react with Ni 2 O 3 and Co 2 O 3 to be consumed. Since SO 2 has a certain solubility in aqueous solution, it is released in There is less SO2 in the upper space of the reactor, and as the reaction proceeds, SO2 will be continuously consumed, so the whole reaction is carried out under slightly positive pressure.
相对于现有方法，本发明的突出优点是采用Na2SO3作还原剂浸出镍氢废电池正负极混合材料，反应速度快，反应酸度较低，硫酸和还原剂的消耗量小；正负极混合材料中高价氧化物的层状结构破坏彻底，可提高金属浸出率；浸出液后续处理中不需要中和大量的酸，成本较低；Na2SO3来源广泛，价格便宜。浸出液后续处理中产生的废弃物量少，较低了污染治理费用，具有明显的经济效益和环境效益。 Compared with the existing method, the outstanding advantage of the present invention is that Na2SO3 is used as the reducing agent to leach the positive and negative electrode mixed materials of nickel-metal hydride waste batteries, the reaction speed is fast, the reaction acidity is low, and the consumption of sulfuric acid and reducing agent is small; The layered structure of high-valent oxides in the negative electrode mixture material is completely destroyed, which can increase the metal leaching rate; the subsequent treatment of the leaching solution does not need to neutralize a large amount of acid, and the cost is low; Na 2 SO 3 comes from a wide range of sources and is cheap. The amount of waste generated in the subsequent treatment of the leachate is small, the cost of pollution control is lower, and it has obvious economic and environmental benefits.
具体实施方法Specific implementation method
实施例1：将100g经焙烧预处理的镍氢废电池正负极混合材料(含镍55.3%、钴6.2%、稀土12.5%)加入容积为2L的不锈钢压力反应釜中，加入2.0mol/L的硫酸750ml，加入Na2SO369g(300ml溶液),在40℃～50℃下密闭搅拌（搅拌速度80r/min）浸出2.5h，，浸出结束后进行液固分离，得到1000ml浸出溶液（不含浸出渣洗涤水）。镍、钴和稀土的浸出率分别为99.1%、98.2%和9.3 %（按进入浸出溶液和浸出渣洗涤液中的镍、钴和稀土计算）。 Example 1: Add 100 g of the positive and negative mixed materials of waste nickel-metal hydride batteries (containing 55.3% nickel, 6.2% cobalt, and 12.5% rare earth) through roasting pretreatment into a stainless steel pressure reactor with a volume of 2 L, and add 2.0 mol/L 750ml of sulfuric acid, add Na 2 SO 3 69g (300ml solution), leaching at 40℃～50℃ with airtight stirring (stirring speed 80r/min) for 2.5h, after leaching, liquid-solid separation is carried out to obtain 1000ml leaching solution (not containing leaching slag washing water). The leaching rates of nickel, cobalt and rare earths are 99.1%, 98.2% and 9.3% respectively (calculated based on nickel, cobalt and rare earths entering the leaching solution and leaching slag washing solution).
实施例2：将经焙烧预处理的500g镍氢废电池正负极混合材料(含镍55.3%、钴6.2%、稀土12.5%)加入容积为5L的不锈钢压力反应釜中，加入3.0mol/L的硫酸3000ml，加入Na2SO3390g(1600ml溶液),在70℃～80℃下密闭搅拌（搅拌速度70r/min）浸出1.0h，浸出结束后进行液固分离，得到4300ml浸出溶液（不含浸出渣洗涤水）。镍、钴和稀土的浸出率分别为99.6%、99.2%和7.6 %（按进入浸出溶液和浸出渣洗涤液中的镍、钴和稀土计算）。 Example 2: Add 500 g of mixed positive and negative electrode materials (containing 55.3% nickel, 6.2% cobalt, and 12.5% rare earth) of waste nickel-metal hydride batteries (containing 55.3% nickel, 6.2% cobalt, and 12.5% rare earth) that have been pretreated by roasting into a stainless steel pressure reactor with a volume of 5 L, and add 3.0 mol/L 3000ml of sulfuric acid, add 390g of Na 2 SO 3 (1600ml solution), leaching at 70℃～80℃ with airtight stirring (stirring speed 70r/min) for 1.0h. slag washing water). The leaching rates of nickel, cobalt and rare earths are 99.6%, 99.2% and 7.6% respectively (calculated based on nickel, cobalt and rare earths entering the leaching solution and leaching slag washing solution).
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629243A (en) * | 2009-06-23 | 2010-01-20 | 四川师范大学 | Infusion method of Ni-MH used battery anode and cathode mixed material |
| CN103088215A (en) * | 2012-10-16 | 2013-05-08 | 赣州市豪鹏科技有限公司 | Method for separating nickel-cobalt and manganese in nickel-cobalt-manganese material with high manganese-cobalt ratio |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629243A (en) * | 2009-06-23 | 2010-01-20 | 四川师范大学 | Infusion method of Ni-MH used battery anode and cathode mixed material |
| CN103088215A (en) * | 2012-10-16 | 2013-05-08 | 赣州市豪鹏科技有限公司 | Method for separating nickel-cobalt and manganese in nickel-cobalt-manganese material with high manganese-cobalt ratio |
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Application publication date: 20140430 |