CN1357938A - Comprehensive recovery and utilization method of waste NiCd battery - Google Patents
Comprehensive recovery and utilization method of waste NiCd battery Download PDFInfo
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- CN1357938A CN1357938A CN00127830A CN00127830A CN1357938A CN 1357938 A CN1357938 A CN 1357938A CN 00127830 A CN00127830 A CN 00127830A CN 00127830 A CN00127830 A CN 00127830A CN 1357938 A CN1357938 A CN 1357938A
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The present invention relates to the harmless disposed of waste NiCd battery and the reuse of matter. Waste NiCd battery after being detached and broken is vacuum heated, Cd and plastic are recovered through gasification and condensation, and the rest gas is active carbon treated and exhausted in the standard. Crushed waste battery is acid leached and filtered to obtain residue, which contains small amount of un-dissolved metal and may be returned for re-dissolution, and filtrate, which is oxidized or neutralized, and heated to prepare ferrite. The present invention realizes the comprehensive recovery and reuse of various heavy metals.
Description
A comprehensive recycling method of nickel-cadmium waste batteries relates to a technology for harmless treatment and recycling of nickel-cadmium and nickel-hydrogen storage waste batteries.
As is known to all, the waste batteries are discarded without being treated, so that the environment is polluted, and particularly, toxic heavy metal cadmium contained in the nickel-cadmium batteries is easy to enrich in plants, so that the human health is easily injured by food through water, soil and the like. The method adopts a simple vacuum metallurgy method for treatment, and has low energy consumption and operation cost and small secondary pollution, but the method does not recycle the useful substances in the waste batteries, thereby causing resource waste.
Therefore, people adopt two treatment methods of pyrometallurgy and hydrometallurgy to recycle nickel-cadmium waste batteries. Wherein the pyrometallurgical treatment method of the catalyst chemical company of Guanxi Japan mainly utilizes the characteristic of high vapor pressure of cadmium and oxides thereof and nickel separation. And (3) after the coating layer on the surface of the battery is stripped, oxidizing roasting is carried out at 900-1200 ℃, so that the nickel is separated into nickel cinder and cadmium oxide concentrated solution, the nickel cinder is used as a steel smelting raw material, and the cadmium oxide concentrated solution is leached and purified to be prepared into various cadmium salts or metals. Various crushed nickel cadmium cells were treated with a rotary furnace at 1260 ℃ by INMETCO, usa, and the collected gas was sprayed with water. The residue in the water, which contains a large amount of cadmium as well as lead and zinc, is sent to a cadmium refining plant for purification. The iron-nickel residue in the furnace is sent into an electric arc furnace to be melted to prepare iron-nickel alloy, and the non-toxic residue can be sold as building aggregate. The Tokyo resource company in the hydrometallurgical processing method peels off and crushes the battery coating layer, and leaches the battery coating layer and sludge slag together with sulfuric acid to remove impurities such as iron and the like. Then hydrogen sulfide is blown into the nickel-cadmium solution to form cadmium sulfide precipitate for separation, and sodium carbonate is added into the nickel-cadmium solution from which cadmium is removed to form nickel carbonate for sale. The waste nickel-cadmium battery hydrometallurgical recovery treatment of Dutch research institute is to crush and screen waste nickel-cadmium batteries, the coarse particles mainly comprise iron shells, plastics and paper, the coarse particles are divided into iron and non-iron parts through magnetic separation, then the iron and non-iron parts are respectively cleaned by hydrochloric acid, iron fragments after the cadmium is removed are removed, and iron-nickel alloy is produced, while the non-iron fragments are disposed of dangerous objects due to the cadmium. Leaching the fine particles with acid solution, disposing the residue as hazardous waste, and extracting cadmium from the filtrate with solvent. The cadmium-containing extract is re-extracted with dilute hydrochloric acid to produce a cadmium chloride solution. Finally, the cadmium is recovered by an electrolytic method.
It can be seen from the above recovery method of nickel cadmium battery that in both methods, except for the high energy consumption caused by the high heating temperature required by pyrometallurgical treatment, cadmium has toxicity, and the generated cadmium-containing waste gas and waste water must be strictly treated, so both methods have the disadvantages of long flow, high investment and operating cost, easy generation of serious secondary pollution, and low comprehensive benefit.
The invention aims to provide a method for recycling and comprehensively utilizing nickel-cadmium and nickel-hydrogen storage waste batteries with less pollution and low energy consumption.
The invention is carried out by mixing various waste nickel-cadmium batteries together, and breaking the shell; the nickel-hydrogen storage battery is disassembled. Then, the battery is subjected to vacuum heating treatment for 2 hours at the temperature of 600-750 ℃ and under the condition of 20-30 mmHg, cadmium, plastics and the like are gasified and volatilized, and the gas is condensed to recover cadmium and then is subjected to activated carbon purification treatment to reach the standard and be discharged; then, in order to recover other metals in the waste battery, crushing the battery after vacuum heating treatment, and dissolving heavy metals such as nickel, iron and the like in the crushed battery by using nitric acid with the concentration of 10-50%, sulfuric acid with the concentration of 10-40%, or mixed acid of nitric acid with the concentration of 10% and hydrochloric acid with the concentration of 20% which is 1-6 times of the weight of the battery to form leachate; then filtering the leaching solution, wherein filter residues are a small amount of undissolved metals, and continuously adding the acid into the leaching solution for further digesting the metals; adding alkali and ferrous sulfate into the filtrate, and preparing ferrite by chemical precipitation. Finally, obtaining the ferrite product with wide application by centrifugation and drying. The centrifuged effluent is reused for dissolving the dilute acid configuration of the waste battery.
The chemical precipitation method adopted by the invention refers to an oxidation method and a neutralization method. The oxidation method is that ferrous sulfate is added into the filtrate of the leachate of the waste battery, and the weight of the filtrate is that the crushed waste battery and FeSO are added4·7H2And (3) neutralizing the O (W/W) at a ratio of 1: 2-6 with alkali until the pH value is 8-9 to generate a colloidal suspension containing the metal ion hydroxide precipitate, adjusting the pH value to 10.0-12.0, heating at 60-100 ℃ for 0.5-5.0 hours at a constant temperature, and uniformly blowing pure air for 20-90 minutes to oxidize the intermediate precipitate to generate ferrite. The ion reaction equation is as follows: in the formula M2+(M+) Is heavy metal ion Ni2+、Cd2+Etc. of the structural formula M2+Fe3+O4(M+ 1/2Fe5/2 3+O4). R is Na+、K+、NH4 +。
The reaction mechanism of the oxidation process is as follows: when the precipitated hydroxide generates soluble divalent metal hydroxy complex through ionization equilibrium, the divalent hydroxy complex reacts with oxygen to generate trivalent hydroxy complex, and then the divalent and trivalent metal hydroxy complexes react with each other to generate colloidal suspension in the form of solid solution, and under the condition of heating or heating oxygenation, the colloidal suspension is converted into the spinel-type ferrite which is difficult to dissolve.
The neutralization method comprises the steps of firstly adding ferrous sulfate into filtrate obtained by filtering the leachate, wherein the addition amount of the ferrous sulfate is waste battery amount and FeSO4·7H2Preparing ferrite preparation liquid by using O (W/W) in a ratio of 1: 2-6, adding strong base solution, adjusting the pH of the preparation liquid to 9.0-12.5, heating to 50-100 ℃, keeping the temperature for 0.5-3 hours, continuously stirring to obtain ferrite crystal precipitate, washing and filtering to obtain a wet ferrite product, and drying at 90 ℃ to obtain the ferrite product.
The invention has the following advantages:
1. because the vacuum heating treatment is adopted, airis prevented from participating in the operation, the generated flue gas amount is small, the purification is easy, the flue gas treatment scale is greatly reduced, and the secondary pollution is small. The centrifugal effluent is circulated, so that the standard discharge treatment cost is reduced, and the investment cost and the operation cost are reduced. The process of the invention has low energy consumption, and the power consumption for processing the nickel-cadmium battery is 1.0 KWh/kg.
2. Because the acid is adopted to dissolve and leach the metal in the waste battery after heating and crushing, the filtrate filtered by the leaching solution is used for preparing the ferrite by adopting a chemical precipitation method, and the integral recycling of the metal is really realized. The invention has high recovery rate of waste batteries, and almost all substances can be recycled as resources except organic matters such as plastics and the like.
3. The composite ferrite product prepared by the method can be used as a magnetic material, has stable performance and is not dissolved out under the condition that the pH value is 3-10.
Drawings
FIG. 1 is a schematic view of the process of the present invention
FIG. 2 is a schematic diagram of the process flow of preparing ferrite by neutralization method of the invention
FIG. 3 is a schematic diagram of the process flow of preparing ferrite by oxidation method of the present invention
FIG. 4 is an X-ray diffraction image of a ferrite product of the present invention
The invention is described in detail below with reference to the figures and examples
Example 1
Referring to fig. 1 and 2, various nickel-cadmium batteries and nickel storage batteries are first mixed together. In order to prevent the expansion of gas during high-temperature heating, the simple crushing of the shell is facilitated to volatilize the gas. Then vacuum heating the crushed batteries in a vacuum heating furnace at 750 ℃ and 20mmHg for 2 hours, carbonizing and volatilizing plastics and organic matters contained in the waste batteries in the heating process, and generating gasThe body is purified by active carbon into gas which meets the emission standard and is discharged. The gasified cadmium and the cadmium after the decomposition of the cadmium oxide are condensed and separated to obtain cadmium powder. And crushing the battery subjected to vacuum heating treatment to obtain battery powder and heavy metal chips such as nickel, iron and the like, and putting the battery powder and the heavy metal chips into 20-50% nitric acid with 2-4 times of volume to dissolve and leach the heavy metals. Filtering the leaching solution to obtain a small amount of undissolved metal scrap filter residue, and continuously adding acid to dissolve the metal scrap filter residue. Adding FeSO (ferric oxide) which is 4-6 times of the weight of the crushed waste batteries into the filtrate4·7H2And O, preparing a ferrite preparation solution, adding a NaOH solution to adjust the pH value to 9.0-12.5, heating to 80-90 ℃, keeping the temperature for 2 hours, continuously stirring to obtain ferrite precipitate, performing centrifugal separation to obtain a product, wherein the heavy metal content of effluent basically meets the discharge standard, the product can be recycled, and effluent which does not meet the standard is refluxed and continuously treated.
The nickel-cadmium battery is heated for 2 hours under the conditions of 750 ℃ and 20mmHg, and the cadmium recovery rate reaches more than 95 percent. Taking a button-shaped nickel-cadmium battery (NF-H) as an example, the concentration of cadmium before treatment is 11075ppm, the concentration of cadmium after treatment is 332ppm, and the recovery rate of cadmium reaches 97%.
The nickel-cadmium battery after vacuum heat treatment basically realizes harmlessness because most of cadmium is recovered. Plastics, organic matters and other volatile matters contained in the waste batteries are removed in the heating treatment process.
Example 2
Referring to fig. 2, the process for preparing ferrite by oxidation method is as follows: firstly, crushing the battery subjected to vacuum heating treatment to obtain battery powder and metal scraps, placing the battery powder and the metal scraps in a sulfuric acid solution with the volume 1-4 times that of the battery scraps and the concentration of 20-30%, dissolving and leaching the metal under the condition of normal temperature stirring, filtering the leachate to obtain filter residues which are a small amount of undissolved metal scraps, and continuously adding the filter residues into the dilute acid for dissolution. Adding ferrous sulfate into the filtrate in the amount of the crushed waste nickel-cadmium battery to FeSO4·7H2And (3) preparing ferrite preparation liquid by using O (W/W) in a ratio of 1: 2-6. And then adding a KOH solution, adjusting the pH value of the preparation solution to 9 to prepare a colloidal suspension, adjusting the pH value to 10.5-11.5, heating at the constant temperature of 75-80 ℃ for 3 hours, uniformly blowing pure air for 60 minutes to oxidize the colloidal suspension to generate ferrite precipitate, washing, performing suction filtration, and drying at the temperature of 90 ℃ to prepare a ferrite crude product.
Finally, the concentration of the heavy metal in the filtrate is detected,and the heavy metal in the waste battery is almost completely recycled. The content of cadmium before and after synthesis is respectively reduced to 0.098-0.35 from 689; the nickel 4083 is reduced to 0.35-0.59. The filtrate separated by centrifugation or suction filtration can be recycled to prepare acid solution, and the effluent with the concentration of heavy metal ions not reaching the standard can be refluxed for continuous treatment. Therefore, the recovery process of the waste nickel-cadmium battery has no secondary pollution.
Performance test of ferrite products referring to FIG. 3, the ferrite products are analyzed by X-ray diffractionObviously, products synthesized by nickel-cadmium battery raw materials have obvious ferrite spinel diffraction peak shapes, namely the products are spinel type ferrites. The product has certain magnetism, wherein the waste nickel-cadmium battery quantity is FeSO4&7H2The ferrite product synthesized by O (W/W) ═ 1: 5-6 has stronger magnetism.
A toxic heavy metal leaching test of the ferrite product shows that toxic heavy metal cadmium is not dissolved out under the condition that the pH value is 3-10.
Claims (3)
1. The comprehensive recycling method of the waste nickel-cadmium battery is characterized by comprising the following steps: firstly, mixing various waste nickel-cadmium batteries and nickel-hydrogen storage batteries together, breaking or disassembling a shell, then carrying out vacuum heating treatment on the waste nickel-cadmium batteries and the nickel-hydrogen storage batteries at the temperature of 600-750 ℃ for 2 hours under the condition of 20-30 mmHg, gasifying and volatilizing cadmium, plastics and the like, condensing the gas, recovering the cadmium, and purifying the gas by using activated carbon to reach thestandard and discharge the gas; then crushing the battery after vacuum heating treatment, dissolving heavy metals such as nickel, iron and the like in the battery by using nitric acid with concentration of 10-50%, sulfuric acid with concentration of 10-40%, or mixed acid consisting of nitric acid with concentration of 10% and hydrochloric acid with concentration of 20% which is 1-6 times of the weight of the battery, filtering the leachate after the heavy metals are fully leached, returning and re-dissolving a small amount of undissolved metals as filter residues, adding alkali and ferrous sulfate into the filtrate to prepare ferrite through a chemical precipitation method, and finally, centrifuging and drying to obtain a ferrite product with wide application; and (5) centrifugally discharging water for recycling.
2. The comprehensive recycling method of waste nickel-cadmium batteries according to claim 1, characterized in that: the chemical precipitation method is a neutralization method, and ferrous sulfate is firstly added into filtrate obtained by filtering the leachate, wherein the addition amount of the ferrous sulfate is waste battery amount and FeSO4·7H2Preparing ferrite preparation liquid by using O (W/W) in a ratio of 1: 2-6, adding NaOH solution, adjusting the pH value of the preparation liquid to 9.0-12.5, heating to 50-100 ℃, keeping the temperature for 0.5-3.0 hours, continuously stirring to obtain ferrite crystal precipitate, washing and filtering to obtain a wet ferrite product, and drying at 90 ℃ to obtain a crude ferrite product.
3. The comprehensive recycling method of waste nickel-cadmium batteries according to claim 1, characterized in that: the chemical precipitation method is an oxidation method, and ferrous sulfate is firstly added into filtrate obtained by filtering the leachate, wherein the addition amount of the ferrous sulfate is waste battery amount and FeSO4·7H2Preparing ferrite preparation liquid by using O (W/W) in a ratio of 1: 2-6, adding NaOH solution, and adjusting the preparationPreparing colloidal suspension containing metal ion hydroxide precipitate with the pH value of 8-9, adjusting the pH value to 10-12, heating to 60-100 ℃, keeping the temperature for 0.5-5.0 hours, uniformly blowing pure air for 20-90 minutes to oxidize the precipitate to generate ferrite precipitate, washing and filtering to obtain a wet ferrite product, and drying at 90 ℃ to obtain a crude ferrite product.
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