CN112093818A - Method for preparing high-purity zinc sulfate from zinc-containing waste - Google Patents
Method for preparing high-purity zinc sulfate from zinc-containing waste Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/06—Sulfates
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for preparing high-purity zinc sulfate from zinc-containing waste, which comprises the steps of pretreating a zinc sulfate solution containing impurities such as copper, manganese, iron, lead, chromium, cadmium, aluminum, nickel and the like at the temperature of 40-80 ℃ and the pH value of 2.5-6.5 by using a persulfuric acid substance as a reaction promoter, filtering and separating, adding zinc powder into filtrate for reduction, and filtering and separating again to obtain the zinc sulfate solution with high purity. The method can effectively remove copper, manganese, iron, lead, chromium, cadmium, aluminum and nickel in the zinc sulfate solution obtained from the zinc-containing solid waste raw material, increase the yield of zinc sulfate, does not introduce ions influencing subsequent processing, has simple process and low cost, does not need complex equipment, and has good industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of solid waste resource utilization, and particularly relates to a method for preparing high-purity zinc sulfate from zinc-containing waste.
Background
Along with the development of economy, the utilization of solid waste resources is more and more concerned, wherein, the zinc-containing noble metal flue gas and zinc-containing lead dust in steel plants, metallurgical zinc-containing dust mud, blast furnace dust, electric furnace dust, blast furnace gas mud, converter OG mud and phosphatized sludge, lead-zinc tailings, zinc-containing electroplating wastewater, lead-zinc smelting wastewater, hot galvanizing wastewaterHigh-concentration waste liquid and waste dry batteries discharged from factories, waste copper-zinc alloy filter materials, waste copper-zinc alloy catalysts in the production of aldehyde and ketone by alcohol dehydrogenation and the like become the main sources of three wastes containing zinc, and the three wastes are often accompanied by impurity element ions such as copper, manganese, iron, lead, chromium, aluminum, nickel and the like, so that the high-purity zinc sulfate product prepared by using the three wastes and the application of the high-purity zinc sulfate product are restricted. For example, when the cobalt content in zinc sulfate is more than 1mg/L, the current effect of a zinc electrolysis system is reduced, and hardening phenomenon occurs in severe cases. When the content of copper and insulator exceeds the standard, high-purity 0 cannot be synthesized#And (3) zinc products. When the content of manganese, iron, lead, chromium, aluminum and nickel ions exceeds the standard, the synthesized zinc sulfide product is greatly discounted in the aspects of chromaticity, coverage rate and the like. Therefore, the zinc hydrometallurgy process has strict regulation on the content of impurity elements in a zinc sulfate solution, the content of impurities in finished zinc sulfate is not higher than 0.8ppm, and the requirement on the content of impurities in some application fields is lower.
At present, the zinc powder replacement method is still a classic process for removing manganese, iron, lead, chromium, aluminum and nickel from a zinc sulfate solution, wherein forward purification and reverse purification are widely applied in the process. But the two purification directions have the defects of multi-stage operation, long process flow, high cost and the like. Zn/Zn2+、Cd/Cd2+、Cr/Cr3+、Co/Co2+、Ni/Ni2+And Cu/Cu2+The standard electrode potentials of the zinc powder are-0.763V, -0.403V, -0.913V, -0.277V, -0.257V and 0.377V respectively, and it can be seen that the zinc powder replaces cobalt firstly and then nickel, copper, cadmium and the like, so that copper is easy to remove, cadmium is slightly difficult, and a reverse dissolution phenomenon easily occurs due to improper operation, thereby affecting normal production; and a small amount of copper ions are required to be provided in addition to the nickel process, thereby increasing the processing cost and time. Chinese patent CN107253801B discloses a method for removing organic matters in water by combining potassium permanganate pre-oxidation and biological manganese oxidation, under the action of potassium permanganate pre-oxidation, although organic matters in water can be efficiently removed, bivalent manganese is generated, so that heavy metal pollution is caused to the water, and the bivalent manganese pollution generated in the potassium permanganate pre-oxidation process is eliminated by performing post-treatment on the water through manganese oxidizing bacteria; chinese patent application CN103214119A discloses a method for removing bromide ions in drinking water containing bromide ions, which can effectively control the generation of bromine disinfection byproducts in the subsequent ozone oxidation bromate and disinfection stage under the combined action of potassium permanganate pre-oxidation, polyaluminium chloride and ferric chloride, and has wide application prospect, but the decomposition of potassium permanganate in the reaction process is greatly influenced by the acidity of the system, and the pH value needs to be controlled between 6-9; the system is alkaline and easy to generate manganese acid radicals, the acid is easy to generate divalent manganese ions, and manganese dioxide precipitates can be generated only under the neutral condition of pH 6-9. The potassium permanganate used as an oxidant has strict requirements on the pH condition of the system and is difficult to control. And when the water body contains too high concentration of iron and manganese ions, the quality of the textile, printing and paper making industries is greatly influenced, and the color and luster of the product are reduced. In the aspect of pipeline transportation, in an iron-rich environment, manganese ions are easy to attach to a pipeline and are oxidized, iron and manganese precipitates are further generated, the water delivery capacity of the pipeline is reduced, the peeling of the precipitates has great influence on the quality of tap water, the red water phenomenon or the black water phenomenon is easy to occur, even the blockage is caused, and the service life of the pipeline is reduced. When chlorine is used as a reaction promoter, the acidity adaptability is increased, but the storage is difficult and the storage equipment is high in risk of corrosion.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing high-purity zinc sulfate from zinc-containing waste, which utilizes a persulfuric acid substance as a reaction promoter and zinc powder as a reducing agent to remove impurities such as manganese, iron, lead, chromium, aluminum, cobalt, nickel and calcium from the zinc-containing solid waste in a synergistic manner so as to prepare the high-purity zinc sulfate; after the hair promoter and the reducing agent are added, the yield can be improved, and substances or elements which are harmful and influence the use of zinc sulfate in the later period are not introduced. Secondly, the zinc-containing waste is utilized to prepare high-purity zinc sulfate, so that on one hand, the source of metal products is increased, and great economic value is brought; on the other hand, the pollution of ions such as copper, manganese, iron, lead, chromium, cadmium, aluminum, cobalt and nickel released by the zinc-containing waste stacking and burying to the environment can be greatly reduced, which has important significance for reducing the comprehensive cost of the actual operation of the industry, improving the market competitiveness and coordinating and sustainable development of the industrial production and the ecological environment.
In order to achieve the technical purpose, the invention provides a method for preparing high-purity zinc sulfate from zinc-containing waste, which comprises the steps of pretreating zinc sulfate solution containing impurities such as copper, manganese, iron, lead, chromium, cadmium, aluminum, nickel, cobalt, calcium and the like by utilizing a persulfate at the temperature of 40-80 ℃ and under the condition that the pH value is 2.5-6.5, removing a certain amount of iron and aluminum and a certain amount of calcium, and taking the persulfate as a reaction promoter to precipitate and separate out the iron, the calcium and the aluminum in the form of chloropicroaluminium, aluminum-vanadium-hydroxide, ferric sulfate, aluminum-copper-nickel ore and aluminum-fluorgypsum. And then filtering and separating to obtain filtrate, continuously adding zinc powder into the filtrate, reducing metals such as copper, manganese, iron, lead, chromium, aluminum, cobalt, nickel, calcium and the like in the filtrate solution into metal simple substances, and filtering and separating to obtain high-purity zinc sulfate solution with high purity and various impurity ions lower than 0.8 ppm.
In an optimized scheme, the persulfuric acid substance comprises one or more of potassium persulfate, sodium persulfate, ammonium persulfate and persulfuric acid. Wherein, if the sodium persulfate is formed by combining a plurality of persulfates, the percentage of the sodium persulfate is more than 70 percent.
According to the optimized scheme, the molar mass ratio of the addition amount of the persulfuric acid substance to the total amount of impurity metals in the zinc sulfate solution is 1: 1-2: 1.
According to the optimized scheme, the persulfuric acid substance is used as a reaction promoter, and the stirring reaction time of pretreatment is 60-180 min.
The optimized scheme is as follows: the granularity of the zinc powder is 40-200 meshes, and the content of the zinc powder is 70-99.99%; preferably, the particle size of the zinc powder is 40-200 meshes, the purity of the zinc powder is selected according to the purity of the zinc sulfate to be prepared, and if the purity of the zinc powder is low but the purity requirement of the zinc sulfate is high, multiple times of circulating treatment are needed to meet the requirement.
According to the optimized scheme, zinc powder is added to reduce and stir for 40-60 min.
According to the optimized scheme, the molar mass ratio of the addition amount of the zinc powder to the total amount of impurity metals in the filtrate solution is 1: 1-1.5: 1.
The zinc-containing waste is zinc sulfate solution containing impurities such as copper, manganese, iron, lead, chromium, cadmium, aluminum, cobalt, nickel, calcium and the like, wherein the method can treat the initial concentrations of the impurity elements such as copper, manganese, iron, lead, chromium, cadmium, aluminum, cobalt, nickel and calcium as Cu:0 mg/L-500 mg/L, Mn: 0.01 mg/L-150 mg/L, Fe: 0.01 mg/L-120 mg/L, Pb: 0.01-50 mg/L, Cr: 0.01 mg/L-350 mg/L, Cd:0.1 mg/L-300 mg/L, Al: 0.01 mg/L-120 mg/L, Co: 0.01 mg/L-150 mg/L, Ni:0.01 mg/L to 50g/L, Ca: 0.01mg/L to 30 mg/L.
In the technical scheme of the invention, the effect of adopting the persulfuric acid substance as the reaction promoter is better than that of adopting potassium permanganate or chlorine. When the persulfuric acid substance is used as a reaction promoter, the yield of zinc sulfate can be increased, and the later application of the zinc sulfate cannot be influenced; if ammonium persulfate, persulfuric acid and zinc powder are taken as impurity-removing introductants, impurities can be removed, and the yield of zinc sulfate can be increased.
The technical principle of the invention is as follows:
firstly, the reaction promoter has certain activation energy and can effectively reduce certain reaction conditions at lower temperature (0-50 ℃) for initiating polymerization reaction; when the persulfuric acid substance is used as a reaction promoter, the persulfuric acid substance is slightly influenced by pH, and the phenomenon that the potassium permanganate causes complex and various impurity ions at the later stage due to different pH (the product under the acidic condition is a + 2-valent manganese ion salt, and the product is neutral or alkaline MnO2). Aluminum (-1.50V) according to the redox potential of the metal>Manganese (-1.18V)>Chromium (-0.913V)>Iron (-0.771V)>Zinc (-0.762V)>Cadmium (-0.403V)>Copper (-0.377V)>Nickel (-0.246V)>Cobalt (-0.28V)>Lead (-0.126V) makes it difficult to remove manganese, iron and aluminum from the zinc sulphate solution. However, the persulfuric acid substance is used as a reaction promoter, so that the subsequent products can be effectively controlled, and new impurities are prevented from being introduced; also provides certain reaction activation energy for the subsequent reduction of the zinc powder, and reduces the reaction conditions. A large number of experiments prove that after persulfuric acid substances are added into zinc sulfate solution containing impurities such as copper, manganese, iron, lead, chromium, aluminum, cobalt, nickel, calcium and the like at the temperature of 40-80 ℃ and the pH value of 2.5-6.5 to serve as a reaction promoter for reaction and filtration, the impurities can be removed and the sulfuric acid can be improved through reduction by zinc powderPurity of zinc.
Based on the reasons, the method provided by the invention can better utilize the persulfuric acid substance as a reaction promoter to prepare high-purity zinc sulfate, and remove impurity elements such as copper, manganese, iron, lead, chromium, cadmium, aluminum, cobalt, nickel, calcium and the like.
Compared with the existing zinc powder single reduction replacement, metal-based alloy, potassium permanganate chlorine and other treatment processes, the method has the following advantages:
(1) after the adopted single persulfuric acid substance or the mixed persulfuric acid substance is treated, the reaction initiation efficiency in the system is high, the solution reaction potential can be effectively reduced, further, iron, calcium and aluminum are precipitated in advance, the reaction potential of residual impurity ions is reduced, and the zinc powder reduction efficiency is improved.
(2) High purification efficiency, low consumption of persulfuric acid substances and low use cost.
(3) The purification efficiency is high, the precipitated metal impurities are not re-dissolved, impurities harmful to later-stage use of the purified product are not introduced, and the used reagent can also increase the product yield. The ammonium persulfate, the persulfuric acid and the zinc powder are removed, and the yield of zinc sulfate is increased; the sodium sulfate and potassium sulfate generated by removing impurities from the potassium persulfate and the sodium persulfate do not influence the later application of the zinc sulfate.
(4) Compared with potassium permanganate, chlorine and other treatment processes, the persulfuric acid substance is slightly interfered by the pH of the system, and the production problems of complex and various products or inconvenient storage and the like caused by the change of the pH are avoided.
(5) Copper, manganese, iron, lead, chromium, cadmium, aluminum, cobalt, nickel and calcium in a zinc sulfate solution obtained from a zinc-containing solid waste raw material are effectively removed, the yield of zinc sulfate is increased, ions influencing subsequent processing are not introduced, the process is simple, the operation is simple, the cost is low, the process conditions are mild, the industrial application is easy, and the method has a good industrial application prospect.
Detailed Description
The specific embodiments of the present invention will be further described with reference to examples.
Example 1
The metallurgical zinc-containing dust and sludge of a certain ferrous metallurgy plant is acidified (Zn:70g/L, Cu:120mg/L, Mn:73mg/L, Cd:249mg/L, Ni:20mg/L, Co:23.4mg/L, Fe:80mg/L, Al:75mg/L, pH 2.5). Adding sodium persulfate according to 1.5 times of the molar mass of the copper, the manganese, the aluminum and the iron, stirring and reacting at 60 ℃ for 120min, and filtering; and adding zinc powder (99%) which is 1 time of 200 meshes of the molar mass of cadmium, nickel and cobalt into the obtained filtrate, placing the filtrate in the same temperature environment, stirring the mixture for 50min, finishing the reaction, carrying out vacuum filtration, and collecting the filtrate and filter residue. 0mg/L of Cu, 0.56mg/L of Mn, 0.11mg/L of Cd, 0.02mg/L of Ni, Co: 0.06mg/L, 0mg/L of Fe, 0.45mg/L of Al, and the impurity removal rate exceeds 98 percent.
Example 2
After certain lead-zinc tailings are acidified (Zn:20g/L, Cu:120mg/L, Mn:93mg/L, Pb:20mg/L, Co:23.4mg/L, Fe:20mg/L, pH 4). Adding sodium persulfate according to 2 times of the molar mass of the copper, the manganese and the iron, stirring and reacting at 60 ℃ for 120min, and filtering; and adding zinc powder (99%) with the molar mass of 1 time 200 meshes of the cadmium and the cobalt into the filtrate, treating for 50min in the same temperature environment, finishing the reaction, carrying out vacuum filtration, and collecting the filtrate and filter residue. The final filtrate Cu is 0mg/L, Mn is 0.21mg/L, Pb: 0.04mg/L, Co: 0.02mg/L, Fe:0mg/L, and the impurity removal rate exceeds 99.11 percent.
Example 3
Aiming at zinc-containing electroplating wastewater of a certain electroplating plant (Zn:35.15g/L, Cu:320mg/L, Mn:53mg/L, Cr:249mg/L, Fe:80mg/L, Al:75mg/L, pH 4.5). Adding sodium persulfate according to 1.5 times of the molar mass of the copper, the manganese, the aluminum and the iron, stirring and reacting at 60 ℃ for 120min, and filtering; and adding zinc powder (99%) with the molar mass of 1 time 200 meshes of the chromium into the filtrate, treating for 50min in the same temperature environment, finishing the reaction, carrying out vacuum filtration, and collecting the filtrate and filter residue. Cu in the final filtrate: 0mg/L, Mn:0.05mg/L, Cr: 0.08mg/L, 0mg/L of Fe, 0.06mg/L of Al, and the impurity removal rate exceeds 99.22 percent.
Example 4
Aiming at smelting waste water (Zn:240.6mg/L, Pb:7.5mg/L, Cu:3.2mg/L, Cd: 35mg/L, pH 5) of a certain lead-zinc smelting plant. Adding sodium persulfate according to 1.5 times of the molar mass of copper, stirring and reacting at 60 ℃ for 120min, and filtering; and adding zinc powder (80%) 200 meshes which is 1.5 times of the molar mass of lead, arsenic and cadmium into the filtrate, treating for 50min in the same temperature environment, finishing the reaction, carrying out vacuum filtration, and collecting the filtrate and filter residue. The final filtrate contains Pb 0.001mg/L, Cu 0mg/L, Cd 0.001mg/L, and the impurity removal rate exceeds 99%.
Example 5
A high-concentration waste liquid (Zn:240.6mg/L, Fe:80.6mg/L, pH 2.5) discharged from a hot galvanizing factory was treated. Adding sodium persulfate according to 1.5 times of the molar mass of the iron, stirring and reacting at 60 ℃ for 60min, and filtering; and adding zinc powder (99%) with the molar mass of 0.5 time of that of iron and 200 meshes into the filtrate, treating the mixture for 50min in the same temperature environment, finishing the reaction, carrying out vacuum filtration, and collecting the filtrate and filter residue. The impurity removal rate of 0.001mg/L Fe in the finally obtained filtrate exceeds 99 percent.
Example 6
The acid-leaching waste liquid of the waste dry batteries (Zn:255.6mg/L, Mn:80.6mg/L, Cu:10.6mg/L, pH 6.5) was treated. Adding sodium persulfate according to 1.5 times of the molar mass of copper and manganese, stirring and reacting for 180min at the temperature of 60 ℃, and filtering; and adding zinc powder (80%) with the molar mass of 0.5 time of that of copper and manganese and 200 meshes into the filtrate, treating the mixture for 50min in the same temperature environment, finishing the reaction, carrying out vacuum filtration, and collecting the filtrate and filter residues. The Mn and Cu in the finally obtained filtrate are 0.03mg/L and 0.001mg/L respectively, and the impurity removal rate is over 99 percent.
Example 7
Aiming at the waste copper-zinc alloy filter material and the waste copper-zinc alloy catalyst acid leaching waste liquid in the production of aldehyde and ketone by alcohol dehydrogenation (Zn:255.6mg/L, Ni:20.6mg/L, Cu:40.6mg/L, Al:45mg/L, pH 4.5). Adding sodium persulfate according to 1.5 times of the molar mass of copper and aluminum, stirring and reacting at 60 ℃ for 180min, and filtering; and adding zinc powder (99%) with the molar mass of 40 meshes, which is 0.5 time of that of nickel and arsenic, into the filtrate, treating the mixture for 50min at the same temperature, finishing the reaction, performing vacuum filtration, and collecting the filtrate and filter residues. In the finally obtained filtrate, the ratio of Ni to Cu is 0.012mg/L L, the ratio of Cu to Cu is 0.001mg/L, and the ratio of As: 0.004mg/L, Al: 0.001mg/L, and the impurity removal rate exceeds 99 percent.
Conventional technical knowledge in the art can be used for the details which are not described in the present invention.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. A method for preparing high-purity zinc sulfate from zinc-containing waste comprises the following steps:
adding a persulfuric acid substance to pretreat impurity metals in the zinc sulfate solution at the temperature of 40-80 ℃ and under the condition that the pH value is 2.5-6.5, filtering and separating to obtain a filtrate, continuously adding zinc powder into the filtrate, and filtering and separating to obtain the high-purity zinc sulfate solution.
2. The method for preparing high-purity zinc sulfate from zinc-containing waste according to claim 1, characterized by comprising the following steps: the persulfuric acid substance comprises one or more than two of potassium persulfate, sodium persulfate, ammonium persulfate and persulfuric acid.
3. The method for preparing high-purity zinc sulfate from zinc-containing waste according to claim 2, characterized by comprising the following steps: the persulfuric acid substance is a combination of more than two of sodium persulfate, and the addition ratio of the sodium persulfate is more than 70%.
4. The method for preparing high-purity zinc sulfate from zinc-containing waste according to claim 1, characterized by comprising the following steps: the granularity of the zinc powder is 40-200 meshes, and the content of the zinc powder is 70-99.99%.
5. The method for preparing high-purity zinc sulfate from zinc-containing waste, according to claim 1, is characterized in that: the stirring reaction time of the pretreatment is 60-180 min; the reaction time is 40-60min after adding zinc powder.
6. The method for preparing high-purity zinc sulfate from zinc-containing waste according to claim 1, characterized by comprising the following steps: the molar mass ratio of the addition amount of the persulfuric acid substance to the total amount of impurity metals in the zinc sulfate solution is 1: 1-2: 1.
7. The method for preparing high-purity zinc sulfate from zinc-containing waste, according to claim 1, is characterized in that: the molar mass ratio of the addition amount of the zinc powder to the total amount of impurity metals in the filtrate is 1: 1-1.5: 1.
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| CN113511669A (en) * | 2021-07-13 | 2021-10-19 | 常州市武进康佳化工有限公司 | Recovery and purification process of blast furnace zinc ash for preparing zinc carbonate |
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Application publication date: 20201218 |
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