CN114317984A - Method for selectively soaking zinc by utilizing cyclone classification-ionic liquid-ultrasonic synergy - Google Patents
Method for selectively soaking zinc by utilizing cyclone classification-ionic liquid-ultrasonic synergy Download PDFInfo
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Abstract
The invention discloses a method for selectively soaking zinc by utilizing cyclone classification-ionic liquid-ultrasound synergy, belonging to the technical field of hydrometallurgy. The method adopts the steps of zinc-containing dust and mud fractional enrichment, ionic liquid synthesis and selective leaching of zinc. In the method, the zinc-containing dust and mud are pretreated by using the special-shaped hydrocyclone to obtain the fine-grain zinc-rich dust and mud, so that the high-efficiency leaching of zinc is facilitated, and meanwhile, the opening and dispersion of flocs in the zinc-containing dust and mud are facilitated; the ionic liquid and ultrasonic synergistic leaching system has selective dissolving capacity on ZnO, the obtained zinc-containing leaching solution has high purity, and the problems of complex components, difficult separation and the like in the traditional leaching system are solved.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a method for selectively soaking zinc by utilizing cyclone classification-ionic liquid-ultrasound synergy.
Background
In recent years, with the rapid development of China's industry, the demand of various fields on zinc resources is continuously increased, the proportion of China's zinc consumption in global zinc consumption is 15.18% in 2000, and is more than 50% in 2020, and the total output reaches 642 ten thousand tons. At present, the recovery of zinc from zinc-containing wastes is becoming an important way to obtain zinc resources, and zinc-containing dust and mud, as a typical waste, has become an important raw material source for regenerating zinc with the rapid development of the steel industry. However, the zinc-containing waste has wide sources and huge quality difference, and is very easy to cause secondary pollution, resource waste and the like, so that the regeneration process is difficult and serious, and therefore, the development of the green, efficient and clean leaching technology of the zinc-containing dust mud has important significance for the resource utilization of the zinc-containing solid waste.
For leaching and extracting zinc from zinc-containing waste materials, the conventional method comprises acid leaching and alkali leaching, but a large amount of other metal substances such as iron, calcium and the like in the zinc-containing dust mud are dissolved while the zinc is dissolved by the acid leaching, so that the subsequent impurity removal process is complicated; when alkaline leaching is used, an alkaline solution can only dissolve zinc oxide in zinc-containing dust mud, but a small part of zinc ferrite cannot be dissolved, and ammonia is volatile, so that higher zinc leaching rate cannot be obtained; meanwhile, both acid and alkali have certain corrosiveness, so that instrument and equipment are corroded in the treatment process, and particularly, when useful minerals are recovered from solid wastes, secondary pollution is caused, so that the technical application is limited. The ionic liquid is a eutectic mixture formed by self-association of a hydrogen bond acceptor and a hydrogen bond donor by virtue of a hydrogen bond formed by accepting or donating electrons after the hydrogen bond acceptor and the hydrogen bond donor are mixed according to a certain stoichiometric ratio, and the mixture is liquid at normal temperature. As a novel green ionic liquid, the ionic liquid has excellent physicochemical properties of biodegradability, low price, no need of purification, 100 percent of atom utilization rate in the synthesis process and the like. Ultrasonic treatment refers to a process of changing and accelerating the physical and chemical states of a reaction substance by using energy generated by ultrasonic waves, and accelerating the rate of a chemical reaction.
The zinc-containing dust mud is mostly derived from smoke dust discharged in the steel production process, a wet dust removal method is mostly adopted for treating the smoke dust, and organic agents are added in the process to flocculate and agglomerate the smoke dust, so the zinc-containing dust mud is mostly in a lump shape, the contents of valuable elements in different granularity groups in the zinc-containing dust mud are different, more than 80% of zinc exists in a-15 um fine fraction, other elements such as iron and carbon exist in a +40um coarse fraction, and the grading pretreatment of the zinc-containing dust mud by utilizing a hydrocyclone not only is favorable for the efficient extraction of the valuable metal elements, but also is favorable for the opening and dispersion of the flocs.
Different metal oxides have different solubilities in different ionic liquids, the cavitation effect, the impact effect, the micro-jet effect and the like of the ultrasound can reduce the thickness of a boundary layer and increase the interface reaction area, and meanwhile, a chemical reaction channel can be widened, the chemical reaction speed is accelerated, and the transfer process of substances is strengthened. The above-mentioned properties of ionic liquids and ultrasound make them increasingly useful in the field of separations, and in particular in the field of metal leaching.
In the existing zinc-containing dust and mud zinc leaching technology, the conventional acid or ammonia leaching process agent has the problems of high cost of the leaching agent, difficult storage, poor leaching selectivity, low leaching rate, easy secondary pollution, complex reaction conditions and the like. Therefore, researches and developments of a method which has simple leaching process, high leaching rate, low cost of leaching agent, easy preparation and good leaching selectivity, and the method is applied to the high-efficiency leaching of zinc-containing waste materials, and is the problem to be mainly solved by researchers in the field.
Therefore, a method for selectively soaking zinc by using cyclone classification-ionic liquid-ultrasound synergy is designed.
Disclosure of Invention
The invention aims to solve the problems of high cost, difficult storage, poor leaching selectivity, low leaching rate, easy secondary pollution, complex reaction conditions and the like of the existing conventional acid or ammonia leaching process agent by using the rotational flow grading-ionic liquid-ultrasonic synergetic selective zinc leaching method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for selectively soaking zinc by utilizing cyclone classification-ionic liquid-ultrasound synergy comprises the following steps:
s1: and (3) zinc-containing dust and mud grading and enriching: the zinc-containing dust and mud are enriched by a special-shaped hydrocyclone in a grading way, fine particles and middle-grade high-zinc dust and mud are used for leaching and extracting zinc, and coarse-grained low-zinc dust and mud are used for extracting other valuable metals such as iron, carbon and the like;
s2: synthesis of ionic liquid: putting a certain amount of hydrogen bond receptor choline chloride and hydrogen bond donor into a vacuum drying oven for drying treatment, fully mixing the dried hydrogen bond receptor choline chloride and the dried hydrogen bond donor according to the molar ratio of 1:2-4, putting the mixture into a beaker, and putting the beaker into the vacuum drying oven for vacuum drying to obtain uniform and transparent solution;
s3: selectively leaching zinc-containing dust: mixing the ions and the zinc-containing dust mud according to a certain liquid-solid ratio, carrying out ultrasonic treatment, carrying out leaching reaction in a constant-temperature water bath kettle after the ultrasonic treatment, and carrying out solid-liquid separation after the reaction to obtain a high-purity zinc-containing leachate.
Preferably, the classification area of the hydrocyclone is composed of a cylindrical section and two conical sections with different cone angles, a concentric double-overflow pipe structure is adopted, and the depth of an inner overflow pipe is adjustable; the zinc-containing dust and mud is enriched by a hydrocyclone in a grading mode, the grading granularity is 0.018mm, fine particles and middle-grade high-zinc dust and mud are used for leaching and extracting zinc, and coarse-grained low-zinc dust and mud are used for extracting other valuable metals such as iron, carbon and the like.
Preferably, the drying oven is set with parameters of 353K, -0.05MPa, and is dried for 12 h.
Preferably, the hydrogen bond acceptor is choline chloride; the hydrogen bond donor is one or more of malonic acid, thiourea, ethylene glycol, urea and oxalic acid hydrate.
Preferably, the solid-to-liquid ratio of the ionic liquid to the zinc-containing dust mud in the leaching process is 1: 4-20, wherein the ionic liquid used as the leaching agent is a hydrogen bond acceptor choline chloride and a hydrogen bond donor according to a molar ratio of 1:2-4, mixing.
Preferably, the ultrasonic treatment is carried out by placing an ultrasonic probe 1.5-2cm below the liquid surface, wherein the ultrasonic frequency is 20Khz, the ultrasonic power is 300-600W, the diameter of an amplitude transformer is 3-18mm, and the ultrasonic time is 30-60 min.
Preferably, the leaching reaction temperature is 70-100 ℃, the solid-liquid reaction time is 10-60 minutes, and the stirring speed is 200-400 rpm.
Compared with the prior art, the invention provides a method for selectively soaking zinc by utilizing cyclone classification-ionic liquid-ultrasound synergy, which has the following beneficial effects:
the method utilizes the ultrasound to process the mixture of the ionic liquid and the zinc-containing dust mud, strengthens the degree and the speed of liquid-solid two-phase reaction, has the zinc leaching rate of over 95 percent, high leaching efficiency, low reaction temperature and low liquid-solid ratio, can obtain the high-purity zinc-containing leaching liquid, and reduces the production cost of recovered zinc.
The invention uses the choline chloride base acid ionic liquid as a leaching agent, can leach zinc from zinc-containing dust containing various components, has higher selectivity on valuable metal zinc, is basically insoluble on other components in the zinc-containing dust, and realizes the selective extraction of zinc.
The method applies the ionic liquid to zinc-containing dust mud for zinc extraction, synthesizes the ionic liquid as a metallurgical dust mud leaching agent, has higher cost, strong corrosivity and toxicity, is not easy to store, is easy to cause secondary pollution by the traditional acid leaching or ammonia leaching method, has simple synthesis and preparation process of the choline chloride-malonic acid ionic liquid, low price of raw materials, no toxicity and pollution, can be recycled after certain treatment and realizes green and safe production compared with the traditional leaching agent.
Drawings
FIG. 1 is a molecular structure diagram of the optimized choline chloride-malonic acid ionic liquid synthesized by the invention;
fig. 2 is a process flow diagram of an embodiment of the method for selectively leaching zinc in zinc-containing dust mud by using the cooperation of a hydrocyclone, ionic liquid and ultrasound.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
In the present invention, all parts and percentages are by weight, unless otherwise specified, and the equipment and materials used are commercially available or commonly used in the art. The methods in the following examples are conventional in the art unless otherwise specified.
A method for selectively soaking zinc by utilizing cyclone classification-ionic liquid-ultrasound synergy comprises the following steps:
(1) pretreating zinc-containing dust: the zinc-containing dust and mud are enriched by a special-shaped hydrocyclone in a grading way, fine particles and middle-grade high-zinc dust and mud are used for leaching and extracting zinc, and coarse-grained low-zinc dust and mud are used for extracting other valuable metals such as iron, carbon and the like.
(2) Synthesizing an ionic liquid: putting a certain amount of choline chloride and malonic acid in a vacuum drying oven for drying treatment, and setting parameters of 353K, -0.05MPa and 12 h. And (3) fully mixing the dried choline chloride and the dried malonic acid according to the molar ratio of 1:2, putting the mixture into a beaker, and putting the beaker into a vacuum drying oven for vacuum drying to obtain a uniform and transparent solution.
(3) Selectively leaching zinc-containing dust: mixing ionic liquid and zinc-containing dust mud according to a certain liquid-solid ratio, carrying out ultrasonic treatment, carrying out leaching reaction in a constant-temperature water bath kettle after ultrasonic treatment, and carrying out solid-liquid separation after reaction to obtain high-purity zinc-containing leachate;
the hydrocyclone is a special-shaped hydrocyclone and adopts a multi-section cone angle design, a classification area is composed of a cylinder section and two conical sections with cone angles of 45 degrees and 120 degrees respectively, a concentric double-overflow pipe structure is adopted, and the depth of an inner overflow pipe is adjustable.
The ultrasonic treatment refers to applying high-energy ultrasonic waves to a mixture of the ionic liquid and the zinc-containing dust mud, wherein an ultrasonic probe is arranged 1-2cm below the liquid surface, the ultrasonic frequency is 20Khz, the ultrasonic power is 300-600W, and the diameter of an amplitude transformer is 3-18 mm.
The ultrasonic treatment of the invention can change the physical and chemical properties of reactants, reduce the cover of impurities on target reactants and is beneficial to improving the reaction rate; the dosage of the ionic liquid is reduced, and the leaching rate of zinc in the zinc-containing dust and mud is improved. The leaching rate of zinc is affected differently by different ultrasonic parameters, the ultrasonic probe is placed 1.5cm below the liquid level of the liquid-solid mixture, the diameter of the amplitude transformer is 10mm, the ultrasonic power is 450W, and the leaching rate of the obtained zinc is highest.
In the leaching separation, zinc-containing dust mud containing various components is fully mixed with ionic liquid, and then is subjected to ultrasonic treatment and liquid-solid phase full mixing reaction, and the selective leaching of zinc in the zinc-containing dust mud is realized by utilizing the difference of the solubility of different metal compounds in the ionic liquid, so that the purity of the zinc in the leaching liquid is improved. In the method, the ionic liquid synthesis preparation process is simple, the cost is low, the leaching selectivity is good, the leaching process is green, efficient and pollution-free, and the method is suitable for industrial production and application.
The invention can be applied to different types of zinc-containing dust and sludge and zinc-containing dust and sludge obtained under various dust removing conditions, and the zinc-containing dust and sludge in the following embodiments has different metal contents of all components due to different steel smelting processes and dust removing conditions.
The following examples are directed to metallurgical dust and sludge of steel, which contains the following main elements:
the zinc-containing waste material is pretreated by a ball mill, and the granularity after ore grinding pretreatment is as follows:
example 1:
in this embodiment, the method for leaching and extracting zinc from the zinc-containing dust mud by using the ionic liquid prepared by synthesizing choline chloride and malonic acid comprises the following specific steps:
and (3) zinc-containing dust and mud grading and enriching: the zinc-containing dust and mud are enriched by using a special-shaped hydrocyclone in a grading way, the grading granularity is 0.018mm, and the proportion of fine particles in a grading product to-300 meshes in an intermediate-grade product is 95%. The fine particles and the intermediate fraction products are filtered and dehydrated for leaching and extracting zinc.
Synthesizing an ionic liquid: drying a certain amount of choline chloride and malonic acid, placing the choline chloride and malonic acid into a vacuum drying oven, setting the temperature of the drying oven to be 353K, setting the relative vacuum degree to be-0.05 Mpa, and drying for 12 hours. Weighing dried choline chloride and malonic acid according to a molar ratio of 1:2, adding the dried choline chloride and malonic acid into a 1L beaker, fully mixing, placing the beaker into a 353K vacuum drying oven, and standing for 12 hours to obtain the transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: taking 10g of zinc-containing dust mud sample, putting the zinc-containing dust mud sample into a 300ml conical flask, and adding the prepared choline chloride-malonic acid ionic liquid according to the liquid-solid ratio of 8: 1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, wherein an ultrasonic probe is arranged at a position 1.5cm below a page, the diameter of a horn is 6mm, the ultrasonic power is 450w, and the ultrasonic time is 50 min; after ultrasonic treatment, the conical flask is placed in a constant-temperature water bath kettle, the temperature is 80 ℃, the leaching time is 1h, the leaching rate of zinc is 98.5%, and the leaching rates of other components are below 5%.
Example 2
In this embodiment, the method for extracting zinc from the zinc-containing dust mud by leaching the ionic liquid prepared by synthesizing choline chloride and urea comprises the following specific steps:
(1) and (3) zinc-containing dust and mud grading and enriching: the zinc-containing dust and mud are enriched by using a special-shaped hydrocyclone in a grading way, the grading granularity is 0.018mm, and the proportion of fine particles in a grading product to-300 meshes in an intermediate-grade product is 97%. The fine particles and the intermediate fraction products are filtered and dehydrated for leaching and extracting zinc.
(2) Synthesizing an ionic liquid: drying a certain amount of choline chloride and urea, putting the choline chloride and urea into a vacuum drying oven, setting the temperature of the drying oven to be 353K, setting the relative vacuum degree to be-0.05 Mpa, and drying for 12 hours. Weighing dried choline chloride and urea according to a molar ratio of 1:2, adding the dried choline chloride and urea into a 1L beaker, fully mixing, placing the beaker into a 333K vacuum drying oven, and standing for 12 hours to obtain the transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: taking 10g of zinc-containing dust mud sample, putting the zinc-containing dust mud sample into a 300ml conical flask, and adding the prepared choline chloride-malonic acid ionic liquid according to the liquid-solid ratio of 5: 1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, wherein an ultrasonic probe is arranged at a position 1.5cm below a page, the diameter of an amplitude transformer is 6mm, the ultrasonic power is 350w, and the ultrasonic time is 30 min; after ultrasonic treatment, the conical flask is placed in a constant-temperature water bath kettle for selective leaching, the temperature is 60 ℃, the leaching time is 30min, the leaching rate of zinc is 89.5%, and the leaching rate of other components is below 15%.
Example 3
In this embodiment, the method for leaching and extracting zinc from the zinc-containing dust mud by using the ionic liquid prepared by synthesizing choline chloride and malonic acid comprises the following specific steps:
(1) and (3) zinc-containing dust and mud grading and enriching: the zinc-containing dust and mud are enriched by using a special-shaped hydrocyclone in a grading way, the grading granularity is 0.018mm, and the proportion of fine particles in a grading product to-300 meshes in an intermediate-grade product is 96%. The fine particles and the intermediate fraction products are filtered and dehydrated for leaching and extracting zinc.
(2) Synthesizing an ionic liquid: drying a certain amount of choline chloride and malonic acid, placing the choline chloride and malonic acid into a vacuum drying oven, setting the temperature of the drying oven to be 353K, setting the relative vacuum degree to be-0.05 Mpa, and drying for 12 hours. Weighing dried choline chloride and malonic acid according to a molar ratio of 1:2, adding the dried choline chloride and malonic acid into a 1L beaker, fully mixing, placing the beaker into a 353K vacuum drying oven, and standing for 12 hours to obtain the transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: taking 10g of zinc-containing dust mud sample, putting the zinc-containing dust mud sample into a 300ml conical flask, and adding the prepared choline chloride-malonic acid ionic liquid according to the liquid-solid ratio of 8: 1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, wherein an ultrasonic probe is arranged at a position 1cm below a page, the diameter of an amplitude transformer is 6mm, the ultrasonic power is 500w, and the ultrasonic time is 50 min; after ultrasonic treatment, the conical flask is placed in a constant-temperature water bath kettle, the temperature is 80 ℃, the leaching reaction time is 1h, the leaching rate of zinc is 92.5 percent, and the leaching rates of other components are below 5 percent.
Example 4
In this embodiment, the method for leaching and extracting zinc from the zinc-containing dust mud by using the ionic liquid prepared by synthesizing choline chloride and malonic acid comprises the following specific steps:
(1) and (3) zinc-containing dust and mud grading and enriching: the zinc-containing dust and mud are enriched by using a special-shaped hydrocyclone in a grading way, the grading granularity is 0.018mm, and the proportion of fine particles in a grading product to-300 meshes in an intermediate-grade product is 98%. The fine particles and the intermediate fraction products are filtered and dehydrated for leaching and extracting zinc.
(2) Synthesizing an ionic liquid: drying a certain amount of choline chloride and malonic acid, placing the choline chloride and malonic acid into a vacuum drying oven, setting the temperature of the drying oven to be 353K, setting the relative vacuum degree to be-0.05 Mpa, and drying for 12 hours. Weighing dried choline chloride and malonic acid according to a molar ratio of 1:2, adding the dried choline chloride and malonic acid into a 1L beaker, fully mixing, placing the beaker into a 353K vacuum drying oven, and standing for 12 hours to obtain the transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: taking 10g of zinc-containing dust mud sample, putting the zinc-containing dust mud sample into a 300ml conical flask, and adding the prepared choline chloride-malonic acid ionic liquid according to the liquid-solid ratio of 15: 1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, wherein an ultrasonic probe is arranged at a position 1.5cm below a page, the diameter of a horn is 6mm, the ultrasonic power is 450w, and the ultrasonic time is 50 min; after ultrasonic treatment, the conical flask is placed in a constant-temperature water bath kettle, the temperature is 80 ℃, the leaching reaction time is 1h, the leaching rate of zinc is 98.8%, and the leaching rates of other components are below 5%.
Example 5
In this embodiment, the method for extracting zinc from the zinc-containing dust mud by leaching the ionic liquid prepared by synthesizing choline chloride and ethylene glycol comprises the following specific steps:
(1) and (3) zinc-containing dust and mud grading and enriching: the zinc-containing dust and mud are enriched by using a special-shaped hydrocyclone in a grading way, the grading granularity is 0.018mm, and the proportion of fine particles in a grading product to-300 meshes in an intermediate-grade product is 96%. The fine particles and the intermediate fraction products are filtered and dehydrated for leaching and extracting zinc.
(2) Synthesizing an ionic liquid: drying a certain amount of choline chloride and malonic acid, placing the choline chloride and malonic acid into a vacuum drying oven, setting the temperature of the drying oven to be 353K, setting the relative vacuum degree to be-0.05 Mpa, and drying for 12 hours. Weighing dried choline chloride and ethylene glycol according to a molar ratio of 1:2, adding the dried choline chloride and the ethylene glycol into a 1L beaker, fully mixing, placing the beaker in a 383K vacuum drying oven, and standing for 12 hours to obtain the transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: taking 10g of zinc-containing dust mud sample, putting the zinc-containing dust mud sample into a 300ml conical flask, and adding the prepared choline chloride-ethylene glycol ionic liquid according to the liquid-solid ratio of 10: 1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, wherein an ultrasonic probe is arranged at a position 1cm below a page, the diameter of an amplitude transformer is 6mm, the ultrasonic power is 400w, and the ultrasonic time is 45 min; after ultrasonic treatment, the conical flask is placed in a constant-temperature water bath kettle, the temperature is 80 ℃, the leaching reaction time is 1h, the leaching rate of zinc is 90.5%, and the leaching rate of other components is below 20%.
Example 6
In this embodiment, choline chloride and thiourea are synthesized to prepare ionic liquid for leaching and extracting zinc from zinc-containing dust mud, and the specific steps are as follows:
(1) and (3) zinc-containing dust and mud grading and enriching: the zinc-containing dust and mud are enriched by using a special-shaped hydrocyclone in a grading way, the grading granularity is 0.018mm, and the proportion of fine particles in a grading product to-300 meshes in an intermediate-grade product is 95%. The fine particles and the intermediate fraction products are filtered and dehydrated for leaching and extracting zinc.
(2) Synthesizing an ionic liquid: drying a certain amount of choline chloride and thiourea, putting the choline chloride and the thiourea into a vacuum drying oven, setting the temperature of the drying oven to be 353K, setting the relative vacuum degree to be-0.05 Mpa, and drying for 12 hours. Weighing dried choline chloride and malonic acid according to a molar ratio of 1:2, adding the dried choline chloride and malonic acid into a 1L beaker, fully mixing, placing the beaker into a 373K vacuum drying oven, and standing for 12 hours to obtain the transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: taking 10g of zinc-containing dust mud sample, putting the zinc-containing dust mud sample into a 300ml conical flask, and adding the prepared choline chloride-malonic acid ionic liquid according to the liquid-solid ratio of 8: 1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, wherein an ultrasonic probe is arranged at a position 1cm below a page, the diameter of an amplitude transformer is 6mm, the ultrasonic power is 500w, and the ultrasonic time is 50 min; after ultrasonic treatment, the conical flask is placed in a constant-temperature water bath kettle, the temperature is 80 ℃, the leaching reaction time is 1h, the leaching rate of zinc is 82.5%, and the leaching rates of other components are below 20%.
Example 7
In this embodiment, the method for leaching and extracting zinc from the zinc-containing dust mud by using the ionic liquid prepared by synthesizing choline chloride and malonic acid comprises the following specific steps:
(1) and (3) zinc-containing dust and mud grading and enriching: the zinc-containing dust and mud are enriched by using a special-shaped hydrocyclone in a grading way, the grading granularity is 0.018mm, and the proportion of fine particles in a grading product to-300 meshes in an intermediate-grade product is 97%. The fine particles and the intermediate fraction products are filtered and dehydrated for leaching and extracting zinc.
(2) Synthesizing an ionic liquid: drying a certain amount of choline chloride and malonic acid, placing the choline chloride and malonic acid into a vacuum drying oven, setting the temperature of the drying oven to be 353K, setting the relative vacuum degree to be-0.05 Mpa, and drying for 12 hours. Weighing dried choline chloride and malonic acid according to a molar ratio of 1:2, adding the dried choline chloride and malonic acid into a 1L beaker, fully mixing, placing the beaker into a 353K vacuum drying oven, and standing for 12 hours to obtain the transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: taking 10g of zinc-containing dust mud sample, putting the zinc-containing dust mud sample into a 300ml conical flask, and adding the prepared choline chloride-malonic acid ionic liquid according to the liquid-solid ratio of 8: 1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, wherein an ultrasonic probe is arranged at a position 1cm below a page, the diameter of an amplitude transformer is 3mm, the ultrasonic power is 350w, and the ultrasonic time is 40 min; after ultrasonic treatment, the conical flask is placed in a constant-temperature water bath kettle, the temperature is 80 ℃, the leaching time is 1h, the leaching rate of zinc is 91.5%, and the leaching rates of other components are below 5%.
The invention combines Materials Studio software to carry out structure optimization and simulation calculation on the hydrogen bond acceptor and the hydrogen bond donor of the ionic liquid, and tests prove that the invention has the advantages of simple structure, convenient operation, low cost and high reliability.
The effects of example 1, example 3 and example 4 are shown: the same ionic liquid synthesized by the same hydrogen bond acceptor, the same hydrogen bond donor and the same molar ratio has different experimental results obtained by adopting different ultrasonic treatment parameters and different liquid-solid ratios;
the results of comparative example 3 and example 6 show that: under the same ultrasonic and reaction conditions, eutectic solution consisting of different hydrogen bond acceptors and hydrogen bond donors has larger difference between the selective leaching effect and the leaching rate of zinc;
the results of comparative example 2 and example 7 show that: the same ionic liquid synthesized by the same hydrogen bond acceptor, the same hydrogen bond donor and the same molar ratio has the same zinc selectivity effect and has larger difference in zinc leaching rate under the same leaching reaction condition.
Through multiple times of simulation calculation and the results show that the example 1 is the optimal condition when the molar ratio of the choline chloride to the malonic acid is 1:2, under proper reaction conditions, the selective leaching effect of zinc is optimal, and the leaching rate is highest.
Meanwhile, the selective leaching effect and leaching rate of zinc are comprehensively influenced by multiple factors of ionic liquid composition, ultrasonic parameters and reaction conditions, the ionic liquid synthesized by different hydrogen bond acceptors and hydrogen bond donors has larger difference of experimental results, and when the ultrasonic parameters and the leaching reaction conditions are changed, the factors can also generate interactive influence.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention and the equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (7)
1. A method for selectively soaking zinc by utilizing cyclone classification-ionic liquid-ultrasound synergy is characterized by comprising the following steps:
s1: and (3) zinc-containing dust and mud grading and enriching: the zinc-containing dust and mud are enriched by a special-shaped hydrocyclone in a grading way, fine particles and middle-grade high-zinc dust and mud are used for leaching and extracting zinc, and coarse-grained low-zinc dust and mud are used for extracting other valuable metals such as iron, carbon and the like;
s2: synthesis of ionic liquid: putting a certain amount of hydrogen bond receptor choline chloride and hydrogen bond donor into a vacuum drying oven for drying treatment, fully mixing the dried hydrogen bond receptor choline chloride and the dried hydrogen bond donor according to the molar ratio of 1:2-4, putting the mixture into a beaker, and putting the beaker into the vacuum drying oven for vacuum drying to obtain uniform and transparent solution;
s3: selectively leaching zinc-containing dust: mixing the ions and the zinc-containing dust mud according to a certain liquid-solid ratio, carrying out ultrasonic treatment, carrying out leaching reaction in a constant-temperature water bath kettle after the ultrasonic treatment, and carrying out solid-liquid separation after the reaction to obtain a high-purity zinc-containing leachate.
2. The method for selective zincing by utilizing cyclone classification-ionic liquid-ultrasound synergy as claimed in claim 1, characterized in that: the classification area of the hydrocyclone is composed of a cylindrical section and two conical sections with different cone angles, a concentric double-overflow pipe structure is adopted, and the depth of an inner overflow pipe is adjustable;
the zinc-containing dust and mud is enriched by a hydrocyclone in a grading mode, the grading granularity is 0.018mm, fine particles and middle-grade high-zinc dust and mud are used for leaching and extracting zinc, and coarse-grained low-zinc dust and mud are used for extracting other valuable metals such as iron, carbon and the like.
3. The method for selective zincing by utilizing cyclone classification-ionic liquid-ultrasound synergy as claimed in claim 2, characterized in that: the drying oven is set with parameters of 353K, -0.05MPa, and is dried for 12 h.
4. The method for selective zincing by utilizing cyclone classification-ionic liquid-ultrasound synergy as claimed in claim 3, characterized in that: the hydrogen bond receptor is choline chloride; the hydrogen bond donor is one or more of malonic acid, thiourea, ethylene glycol, urea and oxalic acid hydrate.
5. The method for selective zincing by utilizing cyclone classification-ionic liquid-ultrasound synergy as claimed in claim 4, characterized in that: the solid-liquid ratio of the ionic liquid to the zinc-containing dust mud in the leaching process is 1: 4-20, wherein the ionic liquid used as the leaching agent is a hydrogen bond acceptor choline chloride and a hydrogen bond donor according to a molar ratio of 1:2-4, mixing.
6. The method for selective zincing by utilizing cyclone classification-ionic liquid-ultrasound synergy as claimed in claim 5, characterized in that: the ultrasonic treatment is carried out by placing an ultrasonic probe 1.5-2cm below the liquid surface, wherein the ultrasonic frequency is 20Khz, the ultrasonic power is 300-600W, the diameter of an amplitude transformer is 3-18mm, and the ultrasonic time is 30-60 min.
7. The method for selective zincing by utilizing cyclone classification-ionic liquid-ultrasound synergy as claimed in claim 6, characterized in that: the leaching reaction temperature is 70-100 ℃, the solid-liquid reaction time is 10-60 minutes, and the stirring speed is 200-400 rpm.
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