CN109467131B - Method for extracting metals from electroplating sludge in form of synthetic ferrite crystals - Google Patents

Method for extracting metals from electroplating sludge in form of synthetic ferrite crystals Download PDF

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CN109467131B
CN109467131B CN201811227248.6A CN201811227248A CN109467131B CN 109467131 B CN109467131 B CN 109467131B CN 201811227248 A CN201811227248 A CN 201811227248A CN 109467131 B CN109467131 B CN 109467131B
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electroplating sludge
crystals
ferrite
sludge
extracting metals
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CN109467131A (en
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林璋
刘炜珍
翁长周
邓洪
刘学明
吉绪新
黎维
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South China University of Technology SCUT
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
    • 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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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Treatment Of Sludge (AREA)

Abstract

The invention belongs to the technical field of electroplating sludge treatment, and discloses a method for extracting metals from electroplating sludge in a form of synthesized ferrite crystals. Adding sodium hydroxide, sodium carbonate and ferric chloride hexahydrate aqueous solution into the electroplating sludge, and uniformly mixing and dispersing to obtain mixed solution; and (3) carrying out heat treatment on the obtained mixed solution at 50-180 ℃, naturally cooling to room temperature after the heat treatment is finished, standing, pouring out supernatant, centrifuging, washing and drying the obtained solid slag, adding hydrochloric acid for acid washing, separating the solid slag from acid washing liquid, washing with deionized water, and drying to obtain ferrite crystals. The invention solves the problems of high cost, complex operation, secondary pollution generation, unclear subsequent application and the like of the current method for recovering heavy metals in sludge, and realizes the extraction of the metal-containing sludge in a material way.

Description

Method for extracting metals from electroplating sludge in form of synthetic ferrite crystals
Technical Field
The invention belongs to the technical field of electroplating sludge treatment, and particularly relates to a method for extracting metals from electroplating sludge in a form of synthesized ferrite crystals.
Background
The electroplating sludge is typical metal-containing sludge, is dangerous solid waste generated in the production process of processing industries such as electroplating, electronic devices, circuit board surface treatment and the like, and comprises sludge generated by anode dissolution in an electrolytic cell, sludge obtained by filtration and sludge generated when wastewater is treated by using a chemical-precipitation method. The water content of the electroplating sludge is high, the particles are fine, and the size is only nano or micron. The electroplating sludge has complex components, contains a large amount of toxic heavy metals such as nickel, chromium, manganese, zinc, cadmium and the like, and the metals exist in amorphous state or hydroxide, carbonate, oxide and other states. If the electroplating sludge is stored for a long time without being treated, serious harm can be brought to the ecological environment, even more serious secondary pollution is brought to the surrounding environment, and the health of people is endangered.
At present, the treatment methods of the electroplating sludge mainly comprise a solidification method, a thermochemical treatment method, a smelting recovery method (pyrometallurgy) and a leaching recovery method (hydrometallurgy). The leaching recovery method comprises two steps of leaching metal and recovering metal in leachate, wherein the most common methods are an acid leaching method and an ammonia leaching method, and a developing biological leaching method is also provided; the latter includes extraction, precipitation, reduction, electrodeposition. The research on the leaching behavior of metals such as Cu, Ni, Cr, Zn and the like in electroplating sludge by using sulfuric acid and ammonia medium by Silva J E et al discovers that: although sulfuric acid leaching is more efficient than ammonia leaching, sulfuric acid leaching is selective and leaches other metals (e.g., Fe, Al, Ca, etc.) in addition to the target metal. In order to reduce pollution and realize resource utilization, the selective extraction of valuable metals in the electroplating sludge is very necessary. CN102399991A adopts a novel composite extraction system consisting of a novel green solvent, namely 'ionic liquid' and a heavy metal organic complexing agent to extract heavy metal nickel in electroplating sludge, and although no new waste is generated, the ionic liquid is expensive, the process cost is high, and the operation is complex. The technical scheme adopted by CN105907972A comprises an oxidation slurrying process, a P204 saponification leaching process, a nickel anolyte total stripping process, an iron stripping and hydrochloric acid regeneration process, a copper extraction electrodeposition process, a chromium precipitation process, a P204 nickel soap process, a P204 zinc extraction electrodeposition process, a nickel electrodeposition process, a calcium-nickel separation process, a magnesium-calcium separation process and an industrial circulating water treatment process. Although valuable metals in the electroplating sludge enter the organic phase through saponification leaching for extraction, the method is complex in process and long in working procedure, and is not a good method for extracting heavy metals in the electroplating sludge. CN101643243 adopts the processes of acid leaching, sulfuration separation and enrichment, hot-pressing leaching, extraction and purification, hot-pressing chromium oxidation, extraction of chromium salt, extraction of ferric chloride and the like to recover copper, nickel, zinc, chromium and iron from the electroplating sludge respectively, the step-by-step extraction steps are various, and the difficulty of heavy metal mixing and separation is large; CN103290222A utilizes the steps of acid leaching, filtering, impurity removal, pH adjustment for multiple times, evaporation crystallization and the like to recover copper and nickel from electroplating sludge, and a large amount of chemical agents are used in the process to generate fluoride precipitate to form new waste, so the method is not advisable. As can be seen from the above examples, the current method for recovering metals in electroplating sludge still has the problems of high cost, complex operation, incapability of separating other heavy metals due to simultaneous mixing, secondary pollution generation and the like, and still has a great space for improvement.
Disclosure of Invention
In view of the disadvantages and shortcomings of the prior art, the present invention aims to provide a method for extracting metals from electroplating sludge in the form of synthesized ferrite crystals.
The purpose of the invention is realized by the following technical scheme:
a method for extracting metals from electroplating sludge in the form of synthetic ferrite crystals, comprising the steps of:
(1) adding sodium hydroxide, sodium carbonate and ferric chloride hexahydrate aqueous solution into the electroplating sludge, and uniformly mixing and dispersing to obtain mixed solution;
(2) carrying out heat treatment on the mixed liquid in the step (1) at 50-180 ℃, naturally cooling to room temperature after the heat treatment is finished, standing, pouring out supernatant liquid, centrifuging, washing and drying the obtained solid slag;
(3) and (3) adding hydrochloric acid into the solid slag treated in the step (2) for acid washing, separating the solid slag from an acid washing solution, washing with deionized water, and drying to obtain a ferrite crystal.
Preferably, in the mixed solution in the step (1), the concentration of sodium carbonate is 0.5-3 mol/L; the concentration of the sodium hydroxide is 0.5-6 mol/L; the concentration of ferric chloride hexahydrate is 0.1-0.3 mol/L.
Preferably, the solid-liquid mass ratio of the mixed liquid obtained in the step (1) is 1 (0.5-10).
Preferably, the heat treatment in the step (2) refers to a direct heat treatment or a hydrothermal treatment.
Preferably, the heat treatment time in the step (2) is 0.5-24 h.
Preferably, the standing time in the step (2) is 0.5-48 h.
Preferably, the concentration of the hydrochloric acid in the step (3) is 0.1-2 mol/L.
Preferably, the solid-liquid mass ratio of the solid slag and the hydrochloric acid in the step (3) is 1 (0.5-5).
Preferably, the acid washing process in the step (3) is stirring for 0.5-3 hours and ultrasonic processing for 0.5-1 hour.
Preferably, the ferrite crystals obtained in step (3) are further ground and then directly subjected to magnetic separation by using a magnetic separator or a magnet. Obtaining ferrite crystals with higher purity.
The method of the invention is not limited to electroplating sludge and is applicable to the treatment of other metal-containing sludge.
The principle of the invention is as follows: the raw slag of the electroplating sludge has the water content of more than 50 percent, fine particles and complex components, contains a large amount of metals such as calcium, iron, nickel, copper, chromium, magnesium, aluminum, zinc and the like, and the metals mostly exist in an amorphous state or exist in states of calcium sulfate dihydrate, calcium sulfate hemihydrate, metal oxides and the like. In the step (1), the regulation and control agents (sodium hydroxide, sodium carbonate and ferric chloride hexahydrate) are dissolved quickly by uniformly mixing and dispersing, and sludge particles are fully contacted with the agents; during the heat treatment in the step (2), the sodium carbonate is hydrolyzed in two steps, carbonate ions in the sodium carbonate are combined with heavy metals (such as calcium ions) to generate carbonate which is easy to dissolve in acid (and then is removed by acid cleaning), hydroxide ions in the sodium carbonate and sodium hydroxide promote the combination of the heavy metal ions in the electroplating sludge and iron elements in ferric chloride hexahydrate to achieve the effects of phase change and crystal growth regulation, so that insoluble metals in the sludge are separated from a solid phase and transferred into a liquid phase, and form ferrite crystals MFe with regular appearance with the added iron elements2O4(M ═ Ni, Zn, Mn, Co, Mg, etc.). In the subsequent standing process, small crystals of the new phase formed in the raw slag gradually grow into large crystals due to the change of the solubility along with the temperature and the crystal growth rule, and are subsequently washed and dried to obtain ferrite and ferrite-containing crystalsMixed slag of a small amount of impurities; the impurities such as calcium carbonate and the like formed in the acid washing process in the step (3) are washed away, and the acid washing is more thorough by magnetic stirring and ultrasonic, so that the purer ferrite can be obtained. The ferrite with the spinel structure has good chemical stability, thermal stability, magnetic property and electrical property, and can be widely applied to microwave devices, sensors, catalysis, magnetism and other aspects.
Compared with the prior art, the method has the following advantages and beneficial effects:
(1) the invention solves the problems of high cost, complex operation, secondary pollution generation, unclear subsequent application and the like of the current method for recovering heavy metals in sludge, and realizes the extraction of the metal-containing sludge in a material way.
(2) According to the method, through a simple two-step process of 'hydrothermal and acid washing', metals in the sludge are directly separated in the form of high-value material ferrite crystals, the extraction rate of target metals is very high, for example, the extraction rate of nickel ions reaches more than 94%, and the purity of the obtained ferrite crystals is high and reaches about 90%; and the obtained ferrite product with the spinel structure has good chemical stability, thermal stability, magnetic property and electrical property, and can be applied to microwave devices, sensors, catalysis, magnetism and the like.
(3) The treatment method has the advantages of simple process, low cost, no secondary pollution, definite subsequent application, realization of resource extraction and direct utilization of the sludge, and higher social benefit and economic benefit.
Drawings
FIG. 1 is an external view of a raw sludge of an electroplating sludge before treatment and a treated product in example 1 of the present invention.
FIG. 2 is an XRD pattern of the raw sludge before treatment and the treated product in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
(1) 4g of electroplating sludge is taken, sodium hydroxide, sodium carbonate and ferric chloride hexahydrate aqueous solution are added to ensure that the solid-to-liquid ratio (w/w) is 1:10, the concentration of sodium carbonate in the obtained mixed solution is 3mol/L, the concentration of sodium hydroxide is 6mol/L, and the concentration of ferric chloride hexahydrate is 0.3mol/L, and the mixture is fully stirred and uniformly mixed.
(2) Transferring the mixed solution obtained in the step (1) into a hydrothermal kettle, closing the hydrothermal kettle, setting the temperature to 180 ℃, keeping the temperature for 24 hours, stopping heating, naturally and slowly cooling to room temperature, and standing for 24 hours; and after standing, pouring out supernatant containing low-concentration heavy metal from the upper layer, centrifugally washing and dehydrating the solid residue after the hydrothermal treatment, and drying the filter residue to obtain a tan or black solid.
(3) Taking 2g of the solid sample obtained in the step (2), adding hydrochloric acid to ensure that the solid-to-liquid ratio (w/w) is 1:5 and the concentration of the hydrochloric acid is 2mol/L, magnetically stirring for 60min, and stopping after ultrasonic treatment for 30 min; separating the solid slag from the pickling solution, washing the obtained nickel ferrite crystal filter residue with deionized water and drying; and carrying out magnetic separation recovery treatment or direct utilization on the nickel ferrite crystal filter residue.
The appearance of the raw sludge before treatment and the product after treatment in this example is shown in FIG. 1, and it can be seen from FIG. 1 that the product after treatment is in the form of black powder. The XRD patterns of the raw electroplating sludge before treatment and the product obtained after treatment in this example are shown in FIG. 2, and the XRD pattern of the product in FIG. 2 shows that the component of the product is nickel ferrite.
The extraction rate of nickel in the electroplating sludge of the embodiment reaches 93.76 percent, and the purity of the obtained nickel ferrite crystal is about 88 percent.
Example 2
Putting 4kg of electroplating sludge into a hydrothermal kettle, adding sodium hydroxide, sodium carbonate and ferric chloride hexahydrate aqueous solution to ensure that the solid-to-liquid ratio (w/w) is 1:0.5, ensuring that the concentration of sodium carbonate in the obtained mixed solution is 0.5mol/L, the concentration of sodium hydroxide is 0.5mol/L and the concentration of ferric chloride hexahydrate is 0.1mol/L, fully stirring, closing the hydrothermal kettle, setting the temperature to be 50 ℃, preserving heat for 0.5h, stopping heating, and standing for 0.5 h. The other processes were the same as in example 1.
The extraction rate of nickel in the electroplating sludge of the embodiment reaches 79.30%, and the purity of the obtained nickel ferrite crystal is about 67%.
Example 3
Putting 10kg of electroplating sludge into a hydrothermal kettle, adding sodium hydroxide, sodium carbonate and ferric chloride hexahydrate aqueous solution to ensure that the solid-to-liquid ratio (w/w) is 1:5, ensuring that the concentration of sodium carbonate in the obtained mixed solution is 2mol/L, the concentration of sodium hydroxide is 3mol/L and the concentration of ferric chloride hexahydrate is 0.2mol/L, fully stirring, closing the hydrothermal kettle, setting the temperature to be 120 ℃, preserving heat for 12h, stopping heating and standing for 24 h. The other processes were the same as in example 1.
The extraction rate of nickel in the electroplating sludge of the embodiment reaches 85.27%, and the purity of the obtained nickel ferrite crystal is about 78%.
Example 4
Putting 1 ton of electroplating sludge into a hydrothermal kettle, adding sodium hydroxide, sodium carbonate and ferric chloride hexahydrate aqueous solution to ensure that the solid-to-liquid ratio (w/w) is 1:5, ensuring that the concentration of sodium carbonate in the obtained mixed solution is 2.5mol/L, the concentration of sodium hydroxide is 3mol/L and the concentration of ferric chloride hexahydrate is 0.2mol/L, fully stirring, closing the hydrothermal kettle, setting the temperature to be 120 ℃, preserving heat for 24 hours, stopping heating, and standing for 12 hours. The other processes were the same as in example 1.
The extraction rate of nickel in the electroplating sludge of the embodiment reaches 87.97%, and the purity of the obtained nickel ferrite crystal is about 75%.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (8)

1. A method for extracting metals from electroplating sludge in the form of synthetic ferrite crystals is characterized by comprising the following steps:
(1) adding sodium hydroxide, sodium carbonate and ferric chloride hexahydrate aqueous solution into the electroplating sludge, and uniformly mixing and dispersing to obtain mixed solution;
(2) carrying out heat treatment on the mixed liquid in the step (1) at 50-180 ℃, naturally cooling to room temperature after the heat treatment is finished, standing, pouring out supernatant liquid, centrifuging, washing and drying the obtained solid slag;
(3) adding hydrochloric acid into the solid slag treated in the step (2) for acid washing, separating the solid slag from acid washing liquid, washing with deionized water, and drying to obtain ferrite crystals;
in the mixed solution in the step (1), the concentration of sodium carbonate is 0.5-3 mol/L; the concentration of the sodium hydroxide is 0.5-6 mol/L; the concentration of ferric chloride hexahydrate is 0.1-0.3 mol/L;
the solid-liquid mass ratio of the mixed liquid obtained in the step (1) is 1 (0.5-10).
2. The method of claim 1 for extracting metals from electroplating sludge in the form of crystals of synthetic ferrite, wherein: the heat treatment in the step (2) refers to direct heat treatment or hydrothermal treatment.
3. The method of claim 1 for extracting metals from electroplating sludge in the form of crystals of synthetic ferrite, wherein: the heat treatment time in the step (2) is 0.5-24 h.
4. The method of claim 1 for extracting metals from electroplating sludge in the form of crystals of synthetic ferrite, wherein: and (3) standing for 0.5-48 h in the step (2).
5. The method of claim 1 for extracting metals from electroplating sludge in the form of crystals of synthetic ferrite, wherein: the concentration of the hydrochloric acid in the step (3) is 0.1-2 mol/L.
6. The method of claim 1 for extracting metals from electroplating sludge in the form of crystals of synthetic ferrite, wherein: the solid-liquid mass ratio of the solid slag and the hydrochloric acid in the step (3) is 1 (0.5-5).
7. The method of claim 1 for extracting metals from electroplating sludge in the form of crystals of synthetic ferrite, wherein: in the step (3), the acid washing process comprises stirring for 0.5-3 hours and ultrasonic treatment for 0.5-1 hour.
8. The method of claim 1 for extracting metals from electroplating sludge in the form of crystals of synthetic ferrite, wherein: and (4) further grinding the ferrite crystals obtained in the step (3), and directly carrying out absorption separation by using a magnetic separator or a magnet.
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CN110527838B (en) * 2019-09-29 2021-07-20 华南理工大学 A method for synergistically extracting chromium from electroplating sludge with hydrothermal and oxidation
CN113120977B (en) * 2021-04-30 2023-06-23 佛山经纬纳科环境科技有限公司 Method for preparing nickel ferrite nano material from nickel-containing ferroelectric plating wastewater and application thereof

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