CN1308971C - Method for preparing ferrite from waste zinc-manganese battery - Google Patents
Method for preparing ferrite from waste zinc-manganese battery Download PDFInfo
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Abstract
The method for preparing the ferrite from the waste zinc-manganese battery comprises the following steps: (1) Crushing a zinc-manganese battery, roughly separating iron, zinc and manganese, and respectively dissolving the iron, the zinc and the manganese by using sulfuric acid to obtain reaction precursor ferrous sulfate, zinc sulfate and manganese sulfate solutions; (2) Mixing the reaction precursors in proportion and then reacting the mixture with ammonium oxalate to prepare a ferrite precursor; and (3) roasting the precursor at high temperature to obtain a ferrite product. The method realizes the recycling of substances contained in the waste zinc-manganese battery while performing harmless treatment on the waste zinc-manganese battery, and has the characteristics of simple method, economy and practicability.
Description
(I) technical field
The invention relates to a method for preparing a soft magnetic ferrite product by using a waste zinc-manganese battery as a raw material, belonging to the technology of recycling harmful solid wastes.
(II) background of the invention
Batteries have been widely used in many areas of modern society, and china now has a total production of only zinc-manganese batteries (including zinc-manganese dry batteries and alkaline-manganese batteries) reaching over 200 billion annually. The waste batteries generated after the failure are recycled, so that the mercury, zinc, copper, manganese and other substances in the batteries can be recycled, and the problem of possible environmental pollution caused by the waste batteries can be solved.
At present, various waste zinc-manganese battery recycling methods based on pyrometallurgical or hydrometallurgical process flows have been developed. The pyrometallurgical process is sequentially separated according to volatility differences of different substances in the battery under high-temperature conditions, and the method has the advantages of short technological process, good mercury recovery rate and large energy consumption and equipment investment; the hydrometallurgy method is characterized in that the waste materials of the batteries are dissolved and then separated, so that the process flow is complex, and different species in the batteries can be easily recovered respectively. Different from the respective recovery of each component in the battery, the zinc-manganese battery is used as a raw material to directly produce a new product, such as ferrite which is widely applied in the industries of color TV, transformers and the like, and the resource recycling cost is greatly reduced because single metal is not recovered any more, so that the economic benefit of the process is improved, and the method has a great development prospect. The invention relates to a method for preparing soft magnetic zinc-manganese ferrite by taking waste zinc-manganese batteries as raw materials.
In the research of using waste zinc-manganese battery to prepare zinc-manganese ferrite, chinese patent (application number: 1357936A) reports a method for preparing ferrite by using zinc-shell dry battery, i.e. after vacuum roasting of broken battery to remove mercury, using nitric acid and hydrochloric acid mixed acid to dissolve MnO 2 Filtering out filter residue with Zn, and adding FeSO 4 ·7H 2 O, adjusting the pH to be 9.5-11.5 by using a strong alkali solution, heating at the constant temperature of 75-80 ℃ for 1.5h, blowing air to oxidize to generate ferrite crystal precipitate, and finally obtaining a spinel type zinc-manganese composite ferrite finished product with excellent magnetism through suction filtration, drying, sintering and molding. Japanese patent (JP 05198418) discloses a method of leaching a battery crushed material by hydrochloric acid, filtering filter residue, adding iron powder to reduce mercury and remove mercury,adjusting the proportion of Fe, zn and Mn in the solution, adjusting pH to 10.O with alkali, and adjusting pH with KClO 3 Oxidizing to obtain zinc-manganese ferrite which contains no mercury and has excellent magnetism. The method disclosed in us patent (UP 5707541) is to crush and screen the cells, wash the screen with water, then calcine at 700-950 ℃ to obtain zinc-manganese oxide, and then react with iron oxide to prepare ferrite. Xi (J.Power Sources, 2004) discloses dissolving the battery directly with sulfuric acid plus hydrogen peroxide solution, adding manganese sulfate and iron powder to adjust the ratio of each substance in the solution and removing mercury when the pH value is 3-5, then adding ammoniaWater and ammonium bicarbonate are precipitated, and finally ferrite is obtained through high-temperature sintering.
In addition to zinc-manganese batteries with zinc casings, a considerable number of waste zinc-manganese batteries produced in society are iron casings, and mercury in the waste zinc-manganese batteries needs to be recycled in the process of processing the battery preparation precursors, so that the preparation method for the zinc-casing batteries has limitations. Moreover, the composition of each element in different waste batteries is not fixed, and the final performance of the product is also affected by the different composition ratios of each element in the prepared ferrite, so if the ferrite is prepared by directly taking iron, zinc and manganese contained in the batteries as precursors and then adjusting the ratios of the elements by adding different precursors, the preparation of the ferrite with different compositions becomes difficult.
Disclosure of the invention
The invention aims to provide a novel method for preparing a soft magnetic ferrite product by using a waste zinc-manganese battery as a raw material, aiming at solving the problems in the prior art.
In order to realize the purpose of the invention, the invention comprehensively uses a high-temperature heating method and a liquid leaching method to prepare the ferrite precursor from the waste battery, and finally realizes the harmless treatment of the waste zinc-manganese battery and the synthesis of a new zinc-manganese ferrite product. Specifically, the method comprises the following steps:
(1) Preparing a reaction precursor: the method comprises the following steps of opening shells of waste batteries by using a crusher, separating iron shells by using a magnetic separation method, washing and roasting magnetic separation residues to obtain roughly separated zinc and manganese monomers or compounds of the zinc and manganese monomers, and dissolving the separated substances by using sulfuric acid respectively to obtain ferrous sulfate, zinc sulfate and manganese sulfate solutions as precursors of subsequent reactions;
(2) Preparing a zinc-manganese ferrite precursor: the Fe content in the ferrous sulfate, zinc sulfate and manganese sulfate solutions obtained above was determined by flame atomic absorption photometry 2+ 、Zn 2+ 、Mn 2+ According to the proportion of iron, zinc and manganese ions in the prepared ferrite, extracting ferrous sulfate, zinc sulfate and manganese sulfate solution according to stoichiometric ratio, mixing them together, adding precipitant, and regulating reaction by using ammonia waterThe pH value of the reaction solution is 3-5, and the precipitate obtained by filtering after the reaction is finished is ferrite precursor;
(3) Preparing a ferrite product: the ferrite precursor is presintered in an inert atmosphere, and then is ground, tabletted and roasted at high temperature to obtain the required ferrite final product.
In the step (1) of the method, the crusher used for opening the shell can be a general cutter or a special crusher; the specific operation of separating the iron shell by a magnetic separation method is that the battery shell with ferromagnetism is adsorbed on the surface of the iron shell by a magnet and then removed to obtain separation; the temperature for roasting the washed magnetic separation residues is 800-950 ℃, and the time is not less than 0.5h; when sulfuric acid is used for dissolving various species, the concentration of the sulfuric acid solution is 0.5-4mol/L, and the mole number of the required sulfuric acid is not less than 1.1 times of the mole number of the dissolved species.
In the step (2), the adopted precipitator is one of ammonium oxalate and ammonia water, the addition amount of the precipitator is not less than 1.1 times of the total mole number of the three metal salt ions, the reaction temperature is not less than 40 ℃, the reaction time is not less than 0.5h, the generated yellow precipitate is filtered at room temperature, and the obtained precipitate is dried in vacuum to obtain the ferrite precursor.
In the step (3), the gas used for keeping the inert atmosphere is one of nitrogen and argon; the pre-sintering temperature is 700-850 ℃, and the pre-sintering time is not less than 1h; the high-temperature roasting temperature is not less than 850 ℃, and the roasting time is not less than 2h.
In the step (1) of the method, roasting the washed magnetic separation residue is carried out in a sealable roasting furnace with a tail gas treatment function, and in the step (3), pre-burning and high-temperature roasting processes of the ferrite precursor are carried out in a tubular electric furnace.
At present, one part of the waste zinc-manganese batteries is a zinc shell, the other part of the waste zinc-manganese batteries is an iron shell battery, and the collected waste zinc-manganese batteries are usually mixed together. Iron is an essential element for preparing ferrite, but because the iron content of batteries of different types is different, a nickel corrosion-resistant layer is arranged on the surface of an iron shell, and nickel is an impurity for preparing zinc-manganese ferrite, the shell of the iron shell battery is separated and specially treated in the treatment process. The battery is broken by a crusher, a magnetic iron shell is separated by a magnetic separation method, and after washing, the iron shell can be dissolved by sulfuric acid to obtain a ferrous sulfate solution, wherein the ferrous sulfate is used as one of the raw materials for preparing the ferrite precursor later. Because the nickel anti-corrosion coating on the iron shell cannot be dissolved under the reaction conditions used, the dissolving solution is mainly ferrous sulfate. By adopting the method, the condition that nickel enters filtrate to increase the impurity removal requirement in the subsequent step can be avoided, and the residue rich in nickel can also be used for recovering nickel; meanwhile, because the components of the waste batteries in the used raw materials have great uncertainty, the method is favorable for controlling the iron content in the preparation liquid in the subsequent steps.
Washing the magnetic separation residue with water can remove part of dissolved mercury and most of electrolyte in the residue, thereby reducing acid consumption in the subsequent acid dissolving step and eliminating the influence of potassium ions in the electrolyte entering into the reaction solution on the performance of ferrite products. The water washing liquid is treated according to a general harmful waste liquid treatment method.
The magnetic separation residue after roasting and water washing also has the function of removing trace mercury in the battery, and can be treated by burning and decomposing organic matters such as a diaphragm in the battery. The filter equipment is added on the used roasting furnace, so that the environmental protection requirements on the recovery of mercury and emission can be met. In addition, because the battery contains a considerable amount of carbon materials, the high-valence manganese compounds in the magnetic separation residues can be reduced by controlling the roasting temperature and the reaction atmosphere, and the acid leaching reaction of the manganese elements in the subsequent process is facilitated. The reaction of this step takes place in Wherein with MnO 2 Compared with MnO is more soluble in the later used dissolving acid. In the roasting condition, according to the composition condition of roasted material selecting proper roasting time and temp. so as to separate mercury and organic matter in it and make most of MnO be separated 2 And reduction is obtained.
When the magnetic separation residue is calcined at a temperature of 800-950 c, which is already above or close to the boiling points of mercury and zinc, a small part of the zinc will be separated from the mercury by forming a vapor together with mercury during calcination, as will be the case with the small amount of cadmium and lead contained in the battery waste. Thus, during firing, the volatiles recovered will be a mixture of mercury, zinc, cadmium and lead. During the roasting, most of the metallic zinc and zinc oxide contained in the roasting residue will be distributed in the upper layer of the roasted mass, depending on the nature of zinc and its oxides. The zinc sulfate and manganese sulfate precursors required by the subsequent reaction can be obtained by roughly separating the metal zinc, the zinc oxide and the manganese oxide and then respectively dissolving the metal zinc, the zinc oxide and the manganese oxide by using sulfuric acid. It is to be noted that the zinc sulphate solution thus obtained will contain a small amount of manganese sulphate, which will also contain a certain amountZinc sulfate. The purpose of such separation is mainly to obtain each reactant with a certain composition in advance, so as to facilitate the subsequent preparation of ferrite precursors with a certain stoichiometric ratio according to needs. In addition, mnO which is not reduced in the process of dissolving a manganese compound with sulfuric acid to produce manganese sulfate 2 And the carbon material and metallic copper will both be separated as residue; when the zinc and the compounds thereof are dissolved by sulfuric acid, the residual trace cadmium and lead in the zinc and the compounds thereof are separated as residues by generating precipitates.
Zn in the above-obtained iron sulfate, zinc sulfate and manganese sulfate solutions was measured by flame atomic absorption photometry 2+ 、Mn 2+ 、Fe 2+ And the concentration of nickel and copper impurities. If the content of nickel and copper in each solution exceeds the standard, impurity removal treatment is carried out by using a solvent extraction method. According to the proportion of iron ions, zinc ions and manganese ions in the ferrite to be prepared, ferrous sulfate, zinc sulfate and manganese sulfate solutions are respectively taken according to the stoichiometric ratio and mixed together. Then adding a proper amount of ammonium oxalate precipitating agent and adjusting the pH value of the reaction solution to prepare the zinc-manganese ferrite precursor. Pre-sintering the obtained precursor at the temperature of 700-850 ℃ under the inert atmosphere condition, grinding and tabletting, and roasting at the temperature of not less than 850 ℃ to obtain the final product.
The invention has the following advantages or effects:
1. the waste zinc-manganese battery is used as a raw material to prepare the zinc-manganese ferrite, so that the problem of environmental pollution of the waste zinc-manganese battery is solved, the main substances contained in the waste battery are recycled, and the process has high economic value and social value.
2. Because the components of the used waste batteries are uncertain in the specific treatment process, the invention firstly carries out coarse separation on the needed species of iron, zinc and manganese when preparing the ferrite, and then carries out mixing according to the need to prepare the ferrite material with a certain stoichiometric ratio.
3. The method has simple process and easy implementation.
(IV) description of the drawings
FIG. 1 is a schematic process flow diagram of the method of the present invention
FIG. 2 is an X-ray diffraction diagram of ferrite prepared by the method of the present invention sintered at a temperature of 1150 deg.C
(V) specific embodiments
Example 1
An example of the invention will now be described in detail with reference to figures 1 and 2, using spent zinc-manganese batteries (approximately 35% of iron-clad batteries) commercially available and prepared ferrites of (MnO) composition 0.26 (ZnO) 0.23 (Fe 2 O 3 ) 0.51 。
The roasting furnace used for roasting the washed magnetic separation residues is self-made, the roasting temperature is 850 ℃, and the roasting time is 1h.
When iron shell separated by magnetic separation is used for preparing ferric sulfate, the reaction temperature condition is selected from room temperature, and H is used 2 SO 4 The concentration is 4mol/L, the iron and the sulfuric acid are dissolved according to the mol ratio of 1: 1.5, and the leaching rate of the iron can reach more than 93 percent finally. The obtained FeSO 4 Ni in solution 2- Is only Fe 2+ 2.5 parts per million, the content of nickel impurities meets the requirement, and further impurity removal treatment is not needed.
3mol/L of sulfuric acid is used at room temperature, and the zinc and manganese are dissolved according to the molar ratio of the dissolved species to the sulfuric acid of 1: 1.7 respectively. Testing solutions consisting mainly of zinc sulphate and manganese sulphate showed that the concentrations of copper and nickel impurity ions in both solutions were very low and negligible.
According to (MnO) 0.26 (ZnO) 0.23 (Fe 2 O 3 ) 0.51 In the proportion of (A) to (B), zn is contained 2+ ，Mn 2+ And Fe 2+ The reaction solutions of (1) were mixed (with pure substances to fine-tune the stoichiometry), and the total concentration of feed solution ions was 0.7mol/L. Under the reaction condition of 60 ℃, 0.35mol/L ammonium oxalate solution is added as a precipitator, and the adding amount of the ammonium oxalate is 1.3 times of the mole number of the three metal salt ions. Adding ammonia water to regulate reaction under the condition of stirringThe pH value of the solution is 3.6, the reaction is carried out for 1h, then the generated yellow precipitate is filtered at the room temperature, and the obtained precipitate is dried in vacuum at 90 ℃ to finally obtain the ferrite precursor.
Presintering the precursor at 800 ℃ for 2h, grinding and tabletting, and then sintering at 1150 ℃ under the condition of filling argon as protective gas to obtain the final product. The structure of the sample obtained by testing with an X-ray diffractometer shows that the prepared product is spinel type zinc manganese ferrite, the impurity phases are few, and the established process flow for preparing the zinc manganese ferrite by the waste alkaline zinc manganese battery is feasible.
Figure 2 shows the XRD test results for the product obtained after sintering at 1150 deg.c for 3 h. The magnetic property test showed that the specific saturation magnetization of the obtained sample was 79emu/g at the employed calcination temperature.
Example 2
The other points are the same as example 1 except that in the step (1), the temperature for roasting the magnetic separation residue after water washing is 800 ℃, the time is 5 hours, the concentration of the sulfuric acid for dissolving each species is 0.5mol/L, and the mole number of the required sulfuric acid is 2 times of the mole number of the dissolved species. In the step (2), the precipitator is ammonia water, and the addition amount of the precipitator is 2 times of the total mole number of the three metal salt ions. The gas used for keeping the inert atmosphere in the step (3) is nitrogen, the presintering temperature is 700 ℃, and the presintering time is 3 hours; the high-temperature roasting temperature is 1050 ℃, and the roasting time is 2 hours. The specific saturation magnetization of the obtained sample was 67emu/g.
Example 3
The procedure of example 1 was otherwise the same except that in step (1), the magnetic separation residue subjected to the water washing was calcined at 950 ℃ for 0.5 hour at a concentration of 4mol/L of sulfuric acid for dissolving each species, and the number of moles of sulfuric acid required was 1.1 times that of the dissolved species. The precipitator in the step (2) is ammonium oxalate, the adding amount of the precipitator is 1.1 times of the total mole number of the three metal salt ions, the temperature of the reaction solution is 40 ℃, and the reaction time is 0.5h. And (3) keeping the inert atmosphere in the step (3), wherein the used gas is argon, the presintering temperature is 850 ℃, the presintering time is 1h, the sintering is carried out for 3h at the sintering temperature of 950 ℃, and the specific saturation magnetization of the obtained sample is 58emu/g.
Example 4
Otherwise, the same as example 1, except that in step (3), sintering was carried out at a baking temperature of 850 ℃ for 2 hours, and the specific saturation magnetization of the obtained sample was 35emu/g.
Claims (5)
1. A method for preparing ferrite from waste zinc-manganese batteries is characterized by comprising the following steps:
(1) Preparing a reaction precursor: the method comprises the following steps of opening shells of waste batteries by using a crusher, separating iron shells by using a magnetic separation method, washing and roasting magnetic separation residues to obtain roughly separated zinc and manganese monomers or compounds of the zinc and manganese monomers, and dissolving the separated substances by using sulfuric acid respectively to obtain ferrous sulfate, zinc sulfate and manganese sulfate solutions as precursors of subsequent reactions;
(2) System for makingPreparing a zinc-manganese ferrite precursor: the Fe content in the ferrous sulfate, zinc sulfate and manganese sulfate solutions obtained above was determined by flame atomic absorption photometry 2+ 、Zn 2+ 、Mn 2+ According to the proportion of iron ions, zinc ions and manganese ions in the ferrite to be prepared, extracting ferrous sulfate solution, zinc sulfate solution and manganese sulfate solution according to a stoichiometric ratio, mixing the ferrous sulfate solution, the zinc sulfate solution and the manganese sulfate solution together, adding a precipitator, adjusting the pH value of the reaction solution to 3-5 by using ammonia water, and filtering the obtained precipitate after the reaction is finished to obtain a ferrite precursor;
(3) Preparing a ferrite product: the ferrite precursor is presintered in an inert atmosphere, and then is ground, tabletted and roasted at high temperature to obtain the required ferrite final product.
2. The method of claim 1, wherein: in the step (1), the specific operation of separating the iron shell by a magnetic separation method is that the battery shell with ferromagnetism is adsorbed on the surface of the iron shell by a magnet and then removed to obtain separation; the temperature for roasting the washed magnetic separation residues is 800-950 ℃, and the time is not less than 0.5h; when sulfuric acid is used for dissolving various species, the concentration of the sulfuric acid solution is 0.5-4mol/L, and the mole number of the required sulfuric acid is not less than 1.1 times of the mole number of the dissolved species.
3. The method of claim 1, wherein: the precipitator in the step (2) is one of ammonium oxalate and ammonia water, the adding amount of the precipitator is not less than 1.1 times of the total mole number of the three metal salt ions, the temperature of the reaction solution is controlled to be not less than 40 ℃, the reaction time is not less than 0.5h, the generated yellow precipitate is filtered at room temperature, and the obtained precipitate is dried in vacuum to obtain the precursor of the ferrite.
4. The method of claim 1, wherein: the gas used for keeping the inert atmosphere in the step (3) is one of nitrogen and argon; the presintering temperature is 700-850 ℃, and the presintering time is not less than 1h; the high-temperature roasting temperature is not less than 850 ℃, and the roasting time is not less than 2h.
5. The method of claim 1 or 2 or 3 or 4, wherein: roasting the washed magnetic separation residues in the step (1) in a sealable roasting furnace with a tail gas treatment function; and (4) pre-burning and high-temperature roasting the ferrite precursor in the step (3) in a tubular electric furnace.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102070332A (en) * | 2010-11-29 | 2011-05-25 | 苏州天铭磁业有限公司 | Nano-crystal Mn-Zn ferrite magnetic material with high initial permeability and high thermal-magnetic sensitivity and preparation method of nano-crystal Mn-Zn ferrite magnetic material |
| CN104229898B (en) * | 2013-06-06 | 2016-03-23 | 湖南邦普循环科技有限公司 | Method for preparing high-purity manganese sulfate and zinc sulfate by using waste zinc-manganese batteries as raw materials |
| CN104649659A (en) * | 2013-11-21 | 2015-05-27 | 北京有色金属研究总院 | Manganese zinc ferrite with high saturation magnetic flux density and preparation method thereof |
| CN103664157B (en) * | 2013-11-28 | 2016-01-20 | 昆明理工大学 | A kind of method preparing high permeability MnZn ferrite |
| CN105503171A (en) * | 2015-12-23 | 2016-04-20 | 苏州冠达磁业有限公司 | Method for preparing high-performance Mn-Zn ferrite from waste dry cells |
| CN107352991B (en) * | 2017-07-04 | 2018-05-22 | 浙江大学 | A kind of nucleocapsid MnZn/nickel zinc complex ferrite and preparation method thereof |
| CN110661052A (en) * | 2018-07-01 | 2020-01-07 | 临沂春光磁业有限公司 | Production method for preparing wide-temperature low-power-consumption manganese-zinc ferrite powder |
| CN110511015A (en) * | 2019-09-30 | 2019-11-29 | 山东凯通电子有限公司 | The preparation method of manganese-zinc ferrite |
| CN113299937B (en) * | 2021-05-17 | 2022-07-12 | 成都工业学院 | Method for recycling waste zinc-manganese dry batteries and directly using waste zinc-manganese dry batteries in rechargeable zinc-manganese batteries |
| CN116875827B (en) * | 2023-07-12 | 2024-03-15 | 重庆上甲电子股份有限公司 | Method for preparing soft magnetic manganese zinc ferrite composite material by utilizing manganese-containing waste residues and zinc-containing waste residues generated in production of perillaldehyde |
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| JPH06260175A (en) * | 1993-03-04 | 1994-09-16 | Tdk Corp | Manufacture of ferrite |
| JPH0733442A (en) * | 1993-07-21 | 1995-02-03 | Sony Corp | Production of mn-zn ferrite |
| JPH0781941A (en) * | 1993-06-30 | 1995-03-28 | Tdk Corp | Production of ferrite |
| JPH0785897A (en) * | 1993-06-30 | 1995-03-31 | Tdk Corp | Method for useddry battery disposal |
| JPH0982340A (en) * | 1995-09-12 | 1997-03-28 | Nomura Kosan Kk | Manufacture of ferrite using waste dry battery |
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|---|---|---|---|---|
| JPH06260175A (en) * | 1993-03-04 | 1994-09-16 | Tdk Corp | Manufacture of ferrite |
| JPH0781941A (en) * | 1993-06-30 | 1995-03-28 | Tdk Corp | Production of ferrite |
| JPH0785897A (en) * | 1993-06-30 | 1995-03-31 | Tdk Corp | Method for useddry battery disposal |
| JPH0733442A (en) * | 1993-07-21 | 1995-02-03 | Sony Corp | Production of mn-zn ferrite |
| JPH0982340A (en) * | 1995-09-12 | 1997-03-28 | Nomura Kosan Kk | Manufacture of ferrite using waste dry battery |
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