CN114317984B - Method for selectively zinc dipping by utilizing cyclone classification-ionic liquid-ultrasonic synergy - Google Patents
Method for selectively zinc dipping by utilizing cyclone classification-ionic liquid-ultrasonic synergy Download PDFInfo
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Abstract
The invention discloses a method for selectively zinc leaching by utilizing cyclone classification-ionic liquid-ultrasonic synergy, and belongs to the technical field of hydrometallurgy. The method adopts the steps of zinc-containing dust mud grading enrichment, ionic liquid synthesis and zinc selective leaching. In the method, the special-shaped hydrocyclone is utilized to pretreat the zinc-containing dust mud to obtain fine-particle zinc-rich dust mud, which is beneficial to efficient leaching of zinc and opening and dispersion of flocs in the zinc-containing dust mud; the ionic liquid and ultrasonic collaborative leaching system has selective dissolving capability 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 zinc leaching by utilizing cyclone classification-ionic liquid-ultrasonic cooperation.
Background
With the rapid development of the industry in China in recent years, the demand of zinc resources in various fields is continuously increased, the zinc consumption in China accounts for 15.18% in 2000 and more than 50% in 2020, and the total yield reaches 642 ten thousand tons. At present, the recovery of zinc from zinc-containing waste is becoming an important way to obtain zinc resources, and zinc-containing dust sludge is a typical waste material, and has become an important raw material source for regenerating zinc along with the rapid development of the iron and steel industry. However, the zinc-containing waste material has wide sources and huge quality differences, and is difficult and heavy in the regeneration process due to secondary pollution, resource waste and the like which are very easy to cause, so that the development of the green, efficient and clean leaching technology of the zinc-containing dust mud has important significance for recycling the zinc-containing solid waste.
For leaching and extracting zinc from zinc-containing waste, the current common methods are acid leaching and alkaline leaching, but the acid leaching dissolves zinc and simultaneously dissolves a large amount of iron, calcium and other metal substances in zinc-containing dust mud, so that the subsequent impurity removal process is complex; when alkaline leaching is used, because the alkaline solution only dissolves zinc oxide in the zinc-containing dust mud, but a small part of zinc ferrite cannot be dissolved, and ammonia is easy to volatilize, a higher zinc leaching rate cannot be obtained; meanwhile, acid and alkali have certain corrosiveness, equipment and instruments can be corroded in the treatment process, and particularly secondary pollution caused when useful minerals are recovered from solid wastes can limit the application of the technology. The ionic liquid is a eutectic mixture formed by self-association of a hydrogen bond acceptor and a hydrogen bond donor by means of accepting or forming a hydrogen bond with electrons after the hydrogen bond acceptor and the hydrogen bond donor are mixed according to a certain stoichiometric ratio, and is in a liquid state 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% of atomic utilization rate in the synthesis process and the like. Ultrasonic treatment refers to the process of changing and accelerating the physical and chemical states of reaction substances and accelerating the chemical reaction rate by utilizing energy generated by ultrasonic waves.
The zinc-containing dust mud mostly comes from dust discharged in the steel production process, the dust is mostly treated by adopting a wet dust removal method, and organic medicaments are added to flocculate and agglomerate the dust in the process, so that the zinc-containing dust mud is mostly in a lump, the contents of valuable elements in different granularity groups in the zinc-containing dust mud are different, more than 80% of zinc exists in-15 um fine fraction, other valuable elements such as iron and carbon exist in +40um coarse fraction, and the grading pretreatment of the zinc-containing dust mud by utilizing a hydrocyclone is not only beneficial to the efficient extraction of valuable metal elements, but also beneficial to the opening and dispersion of flocculation.
Different metal oxides have different solubilities in different ionic liquids, and the cavitation effect, impact effect, micro-jet effect and the like of the ultrasonic can reduce the thickness of a boundary layer and increase the interface reaction area, and can widen a chemical reaction channel, accelerate the chemical reaction speed and strengthen the transfer process of substances. The above characteristics of ionic liquids and ultrasound have led to their increasing use in the separation field, in particular in the field of metal leaching extraction.
In the existing zinc-containing dust and sludge zinc leaching technology, the conventional acid or ammonia leaching process agent has the problems of high cost of the leaching agent, difficult preservation, poor leaching selectivity, low leaching rate, easy secondary pollution, complex reaction conditions and the like. Therefore, the research and development of the method with simple leaching process, high leaching rate, low price of the leaching agent, easy preparation and good leaching selectivity is the key problem to be solved by researchers in the field when the method is applied to the efficient leaching of zinc-containing waste.
Therefore, a method for selectively zinc dipping by utilizing cyclone classification-ionic liquid-ultrasonic synergy is designed.
Disclosure of Invention
The invention aims to solve the problems of high leaching agent cost, difficult preservation, poor leaching selectivity, low leaching rate, easy secondary pollution, complex reaction conditions and the like of the conventional acid or ammonia leaching process agent, and provides a synergistic selective zinc leaching method by utilizing cyclone classification-ionic liquid-ultrasonic.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for selectively zinc dipping by utilizing cyclone classification-ionic liquid-ultrasonic cooperation comprises the following steps:
s1: classifying and enriching zinc-containing dust mud: classifying and enriching zinc-containing dust mud by using a special-shaped hydrocyclone, wherein fine particles and middle-particle-level high-zinc-dust mud are used for leaching and extracting zinc, and coarse-particle low-zinc-dust mud is used for extracting other valuable metals such as iron, carbon and the like;
s2: synthesizing an ionic liquid: placing a certain amount of hydrogen bond acceptor choline chloride and a hydrogen bond donor into a vacuum drying oven for drying treatment, taking the dried hydrogen bond acceptor choline chloride and hydrogen bond donor to be fully mixed according to the molar ratio of 1:2-4, placing into a beaker, and placing into the vacuum drying oven for vacuum drying to obtain a uniform transparent solution;
s3: zinc-containing dust mud selective leaching: mixing ions 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 after ultrasonic treatment, and carrying out solid-liquid separation after the reaction to obtain the high-purity zinc-containing leaching solution.
Preferably, the classifying area of the hydrocyclone consists 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 mud is graded and enriched by a hydrocyclone, the grading granularity is 0.018mm, fine grains and intermediate grain-level zinc-containing dust mud are used for leaching and extracting zinc, and coarse grain low-zinc-containing dust mud is used for extracting other valuable metals such as iron, carbon and the like.
Preferably, the parameters of the drying box are 353K, -0.05MPa, and the drying box is dried for 12 hours.
Preferably, the hydrogen bond acceptor is choline chloride; the hydrogen bond donor is one or more of malonic acid, thiourea, 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 hydrogen bond acceptor choline chloride and hydrogen bond donor according to the mol ratio of 1: 2-4.
Preferably, the ultrasonic treatment adopts an ultrasonic probe to be placed at a position of 1.5-2cm below the liquid level, 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 30-60min.
Preferably, the leaching reaction temperature is 70-100 ℃, the solid-liquid reaction time is 10-60 minutes, and the stirring speed is 200-400rpm.
Compared with the prior art, the invention provides a method for selectively zinc leaching by utilizing cyclone classification-ionic liquid-ultrasonic synergy, which has the following beneficial effects:
according to the invention, the ionic liquid and zinc-containing dust and sludge mixture is treated by utilizing ultrasonic waves, the liquid-solid two-phase reaction degree and rate are enhanced, the zinc leaching rate can reach more than 95%, the leaching efficiency is high, the reaction temperature is low, the liquid-solid ratio is low, the high-purity zinc-containing leaching solution can be obtained, and the production cost of zinc recovery is reduced.
The invention uses the chloridized choline base acid ionic liquid as the leaching agent, can leach zinc from the zinc-containing dust mud containing various components, has higher selectivity to valuable metal zinc, is basically insoluble to other components in the zinc-containing dust mud, and realizes the selective extraction of zinc.
According to the invention, the ionic liquid is applied to zinc-containing dust mud to extract zinc, and the ionic liquid is synthesized to be used as a metallurgical dust mud leaching agent, and the leaching agent by the traditional acid leaching or ammonia leaching method has the advantages of higher cost, corrosiveness, stronger toxicity, difficult storage and easy secondary pollution.
Drawings
FIG. 1 is a molecular structure diagram of the choline chloride-malonic acid ionic liquid synthesized by the invention after optimization;
FIG. 2 is a schematic process flow diagram of one embodiment of a method for selectively leaching zinc from zinc-bearing dust sludge using hydrocyclone-ionic liquid-ultrasonic co-operation.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
In the present invention, unless otherwise specified, all parts and percentages are by weight, and the equipment, materials, etc. used are commercially available or are conventional in the art. The methods in the following examples are conventional in the art unless otherwise specified.
A method for selectively zinc dipping by cyclone classification-ionic liquid-ultrasonic cooperation, which comprises the following steps:
(1) Zinc-containing dust mud pretreatment: the special-shaped hydrocyclone is utilized to carry out grading enrichment on zinc-containing dust mud, fine particles and intermediate-particle-level zinc-containing dust mud are used for leaching and extracting zinc, and coarse-particle low-zinc-containing dust mud is used for extracting other valuable metals such as iron, carbon and the like.
(2) Synthesizing an ionic liquid: and (3) drying a certain amount of choline chloride and malonic acid in a vacuum drying oven, and setting parameters of 353K, -0.05MPa and 12h. And (3) fully mixing the dried choline chloride and malonic acid according to a molar ratio of 1:2, putting the mixture into a beaker, and vacuum drying the mixture in a vacuum drying oven to obtain a uniform transparent solution.
(3) Zinc-containing dust mud selective leaching: mixing the ionic liquid and zinc-containing dust mud according to a certain liquid-solid ratio, performing ultrasonic treatment, performing leaching reaction in a constant-temperature water bath after ultrasonic treatment, and performing solid-liquid separation after the reaction to obtain high-purity zinc-containing leaching solution;
the hydrocyclone is a special-shaped hydrocyclone, adopts a design of multi-section cone angles, and the classification area is composed of a cylindrical section and two sections of cone sections with cone angles of 45 degrees and 120 degrees respectively, adopts a concentric double-overflow pipe structure, and has adjustable inner overflow pipe depth.
The ultrasonic treatment means that high-energy ultrasonic waves are applied to the mixture of the ionic liquid and the zinc-containing dust mud, wherein an ultrasonic probe is arranged at a position 1-2cm below the liquid surface, the ultrasonic frequency is 20Khz, the ultrasonic power is 300-600W, and the diameter of a luffing rod is 3-18mm.
The ultrasonic treatment can change the physical and chemical properties of the reactant, reduce the cover of the impurity to the target reactant, and is beneficial to the improvement of the reaction rate; the dosage of the ionic liquid is reduced, and the leaching rate of zinc in the zinc-containing dust mud is improved. The influence of different ultrasonic parameters on the leaching rate of zinc is different, an ultrasonic probe is arranged under the liquid level of the liquid-solid mixture by 1.5cm, the diameter of an amplitude transformer is 10mm, the ultrasonic power is 450W, and the obtained zinc leaching rate is highest.
In the leaching separation, after fully mixing zinc-containing dust mud containing various components with the ionic liquid, carrying out ultrasonic treatment, fully mixing liquid and solid phases for reaction, and utilizing the difference of solubility of different metal compounds in the ionic liquid, realizing selective leaching of zinc in the zinc-containing dust mud, thereby improving the purity of zinc in the leaching liquid. In the method, the ionic liquid is simple in synthesis and preparation process, low in cost, good in leaching selectivity, green in leaching process, efficient and pollution-free, and suitable for industrial production and application.
The invention can be applied to zinc-containing dust mud of different types and obtained under various dust removal conditions, and the zinc-containing dust mud in the following examples has different metal contents of each component due to different iron and steel smelting processes and dust removal conditions.
The following examples are directed to metallurgical dust and sludge, the main elemental components of which are as follows:
the zinc-containing waste is pretreated by a ball mill, and the granularity composition after ore grinding pretreatment is as follows:
example 1:
in the embodiment, the ionic liquid prepared by synthesizing choline chloride and malonic acid is used for leaching and extracting zinc in the zinc-containing dust mud, and the specific steps are as follows:
classifying and enriching zinc-containing dust mud: the zinc-containing dust mud is graded and enriched by using a special-shaped hydrocyclone, the grading granularity is 0.018mm, and the proportion of fine particles in the graded product to-300 meshes in the intermediate fraction product is 95%. The fine particles and the intermediate-size products are used for leaching and extracting zinc after being filtered and dehydrated.
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 353K, and drying the choline chloride and malonic acid for 12 hours under the condition that the relative vacuum degree is minus 0.05 Mpa. Weighing the dried choline chloride and malonic acid, adding the choline chloride and malonic acid into a 1L beaker according to a molar ratio of 1:2, fully mixing, placing the beaker into a 353K vacuum drying oven, and standing for 12 hours to obtain transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: 10g of zinc-containing dust mud sample is taken in a 300ml conical flask, and the prepared choline chloride-malonic acid ionic liquid is added according to the liquid-solid ratio of 8:1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, placing an ultrasonic probe at a position of 1.5cm below a page, wherein the diameter of an amplitude transformer is 6mm, the ultrasonic power is 450w, and the ultrasonic time is 50min; 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 all below 5%.
Example 2
In the embodiment, the ionic liquid prepared by synthesizing choline chloride and urea is used for leaching and extracting zinc in the zinc-containing dust mud, and the specific steps are as follows:
(1) Classifying and enriching zinc-containing dust mud: the zinc-containing dust mud is graded and enriched by using a special-shaped hydrocyclone, the grading granularity is 0.018mm, and the proportion of fine particles in the graded product to-300 meshes in the intermediate fraction product is 97%. The fine particles and the intermediate-size products are used for leaching and extracting zinc after being filtered and dehydrated.
(2) Synthesizing an ionic liquid: drying a certain amount of choline chloride and urea, placing the choline chloride and urea into a vacuum drying oven, setting the temperature of the drying oven to 353K, and drying the choline chloride and urea for 12 hours under the condition that the relative vacuum degree is minus 0.05 Mpa. Weighing the dried choline chloride and urea, adding the choline chloride and the urea into a 1L beaker according to a molar ratio of 1:2, fully mixing, placing the beaker into a 333K vacuum drying oven, and standing for 12 hours to obtain transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: 10g of zinc-containing dust mud sample is taken in a 300ml conical flask, and the prepared choline chloride-malonic acid ionic liquid is added according to a liquid-solid ratio of 5:1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, placing an ultrasonic probe at a position of 1.5cm below a page, wherein the diameter of an amplitude transformer is 6mm, the ultrasonic power is 350w, and the ultrasonic time is 30min; after ultrasonic treatment, the conical flask is placed in a constant-temperature water bath kettle for selective leaching, the leaching time is 30min at the temperature of 60 ℃, the leaching rate of zinc is 89.5%, and the leaching rate of other components is below 15%.
Example 3
In the embodiment, the ionic liquid prepared by synthesizing choline chloride and malonic acid is used for leaching and extracting zinc in the zinc-containing dust mud, and the specific steps are as follows:
(1) Classifying and enriching zinc-containing dust mud: the zinc-containing dust mud is graded and enriched by using a special-shaped hydrocyclone, the grading granularity is 0.018mm, and the proportion of fine particles in the graded product to-300 meshes in the intermediate fraction product is 96%. The fine particles and the intermediate-size products are used for leaching and extracting zinc after being filtered and dehydrated.
(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 353K, and drying the choline chloride and malonic acid for 12 hours under the condition that the relative vacuum degree is minus 0.05 Mpa. Weighing the dried choline chloride and malonic acid, adding the choline chloride and malonic acid into a 1L beaker according to a molar ratio of 1:2, fully mixing, placing the beaker into a 353K vacuum drying oven, and standing for 12 hours to obtain transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: 10g of zinc-containing dust mud sample is taken in a 300ml conical flask, and the prepared choline chloride-malonic acid ionic liquid is added according to the liquid-solid ratio of 8:1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, placing an ultrasonic probe at a position 1cm below a page, wherein the diameter of an amplitude transformer is 6mm, the ultrasonic power is 500w, and the ultrasonic time is 50min; 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%, and the leaching rates of other components are all below 5%.
Example 4
In the embodiment, the ionic liquid prepared by synthesizing choline chloride and malonic acid is used for leaching and extracting zinc in the zinc-containing dust mud, and the specific steps are as follows:
(1) Classifying and enriching zinc-containing dust mud: the zinc-containing dust mud is graded and enriched by using a special-shaped hydrocyclone, the grading granularity is 0.018mm, and the proportion of fine particles in the graded product to-300 meshes in the intermediate fraction product is 98%. The fine particles and the intermediate-size products are used for leaching and extracting zinc after being filtered and dehydrated.
(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 353K, and drying the choline chloride and malonic acid for 12 hours under the condition that the relative vacuum degree is minus 0.05 Mpa. Weighing the dried choline chloride and malonic acid, adding the choline chloride and malonic acid into a 1L beaker according to a molar ratio of 1:2, fully mixing, placing the beaker into a 353K vacuum drying oven, and standing for 12 hours to obtain transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: 10g of zinc-containing dust mud sample is taken in a 300ml conical flask, and the prepared choline chloride-malonic acid ionic liquid is added according to a liquid-solid ratio of 15:1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, placing an ultrasonic probe at a position of 1.5cm below a page, wherein the diameter of an amplitude transformer is 6mm, the ultrasonic power is 450w, and the ultrasonic time is 50min; 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 all below 5%.
Example 5
In the embodiment, the ionic liquid prepared by synthesizing choline chloride and ethylene glycol is used for leaching and extracting zinc in the zinc-containing dust mud, and the specific steps are as follows:
(1) Classifying and enriching zinc-containing dust mud: the zinc-containing dust mud is graded and enriched by using a special-shaped hydrocyclone, the grading granularity is 0.018mm, and the proportion of fine particles in the graded product to-300 meshes in the intermediate fraction product is 96%. The fine particles and the intermediate-size products are used for leaching and extracting zinc after being filtered and dehydrated.
(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 353K, and drying the choline chloride and malonic acid for 12 hours under the condition that the relative vacuum degree is minus 0.05 Mpa. Weighing the dried choline chloride and ethylene glycol, adding the choline chloride and the ethylene glycol into a 1L beaker according to a molar ratio of 1:2, fully mixing, placing the beaker into a 383K vacuum drying oven, and standing for 12 hours to obtain transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: 10g of zinc-containing dust mud sample is taken in a 300ml conical flask, and the prepared choline chloride-ethylene glycol ionic liquid is added according to the liquid-solid ratio of 10:1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, placing an ultrasonic probe at a position 1cm below a page, wherein the diameter of an amplitude transformer is 6mm, the ultrasonic power is 400w, and the ultrasonic time is 45min; 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 the embodiment, the ionic liquid prepared by synthesizing choline chloride and thiourea is used for leaching and extracting zinc in the zinc-containing dust mud, and the specific steps are as follows:
(1) Classifying and enriching zinc-containing dust mud: the zinc-containing dust mud is graded and enriched by using a special-shaped hydrocyclone, the grading granularity is 0.018mm, and the proportion of fine particles in the graded product to-300 meshes in the intermediate fraction product is 95%. The fine particles and the intermediate-size products are used for leaching and extracting zinc after being filtered and dehydrated.
(2) Synthesizing an ionic liquid: drying a certain amount of choline chloride and thiourea, putting the choline chloride and thiourea into a vacuum drying oven, setting the temperature of the drying oven to 353K, and drying the choline chloride and thiourea for 12 hours under the condition that the relative vacuum degree is minus 0.05 Mpa. Weighing the dried choline chloride and malonic acid, adding the choline chloride and malonic acid into a 1L beaker according to a molar ratio of 1:2, fully mixing, placing the beaker into a 373K vacuum drying oven, and standing for 12 hours to obtain transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: 10g of zinc-containing dust mud sample is taken in a 300ml conical flask, and the prepared choline chloride-malonic acid ionic liquid is added according to the liquid-solid ratio of 8:1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, placing an ultrasonic probe at a position 1cm below a page, wherein the diameter of an amplitude transformer is 6mm, the ultrasonic power is 500w, and the ultrasonic time is 50min; 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 all below 20%.
Example 7
In the embodiment, the ionic liquid prepared by synthesizing choline chloride and malonic acid is used for leaching and extracting zinc in the zinc-containing dust mud, and the specific steps are as follows:
(1) Classifying and enriching zinc-containing dust mud: the zinc-containing dust mud is graded and enriched by using a special-shaped hydrocyclone, the grading granularity is 0.018mm, and the proportion of fine particles in the graded product to-300 meshes in the intermediate fraction product is 97%. The fine particles and the intermediate-size products are used for leaching and extracting zinc after being filtered and dehydrated.
(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 353K, and drying the choline chloride and malonic acid for 12 hours under the condition that the relative vacuum degree is minus 0.05 Mpa. Weighing the dried choline chloride and malonic acid, adding the choline chloride and malonic acid into a 1L beaker according to a molar ratio of 1:2, fully mixing, placing the beaker into a 353K vacuum drying oven, and standing for 12 hours to obtain transparent and uniform ionic liquid at room temperature.
(3) Selective leaching of zinc: 10g of zinc-containing dust mud sample is taken in a 300ml conical flask, and the prepared choline chloride-malonic acid ionic liquid is added according to the liquid-solid ratio of 8:1. Carrying out ultrasonic treatment on the liquid-solid two-phase mixture, placing an ultrasonic probe at a position 1cm below a page, wherein the diameter of an amplitude transformer is 3mm, the ultrasonic power is 350w, and the ultrasonic time is 40min; 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 all below 5%.
The invention combines the Materials Studio software to carry out structural optimization and simulation calculation on the hydrogen bond acceptor and the hydrogen bond donor of the ionic liquid, and is verified by experiments.
From the effects of example 1, example 3 and example 4, it can be seen that: the same ionic liquid synthesized by the same hydrogen bond acceptor, the same hydrogen bond donor and the molar ratio adopts different ultrasonic treatment parameters and different liquid-solid ratios, and the obtained experimental results are different;
the results of comparative example 3 and example 6 show that: under the same ultrasonic and reaction conditions, different hydrogen bond acceptors and hydrogen bond donors form eutectic solutions, and the selective leaching effect and leaching rate of zinc are greatly different;
the results of comparative example 2 and example 7 are shown as follows: the same hydrogen bond acceptor, the hydrogen bond donor and the same ionic liquid synthesized in molar ratio have the same zinc selectivity effect under the same leaching reaction conditions, and the leaching rates of zinc are greatly different.
The simulation calculation and the results show that the example 1 is the optimal condition, when the mol ratio of choline chloride to 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 parameter and reaction conditions, the ionic liquids synthesized by different hydrogen bond acceptors and hydrogen bond donors have large difference in experimental results, and when the ultrasonic parameter and the leaching reaction conditions are changed, the factors can also generate interaction.
The present invention is not limited to the above-mentioned embodiments, and any person skilled in the art, based on the technical solution of the present invention and the inventive concept thereof, can be replaced or changed within the scope of the present invention.
Claims (4)
1. A method for selectively zinc dipping by utilizing cyclone classification-ionic liquid-ultrasonic cooperation is characterized by comprising the following steps:
s1: classifying and enriching zinc-containing dust mud: classifying and enriching zinc-containing dust mud by using a special-shaped hydrocyclone, wherein fine particles and intermediate particle-level zinc-containing dust mud are used for leaching and extracting zinc, and coarse particle low-zinc-containing dust mud is used for extracting iron and other valuable metals;
s2: synthesizing an ionic liquid: placing a certain amount of hydrogen bond acceptor choline chloride and a hydrogen bond donor into a vacuum drying oven for drying treatment, taking the dried hydrogen bond acceptor choline chloride and hydrogen bond donor to be fully mixed according to the molar ratio of 1:2-4, placing into a beaker, and placing into the vacuum drying oven for vacuum drying to obtain a uniform transparent solution;
s3: zinc-containing dust mud selective leaching: mixing ions 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 after ultrasonic treatment, and carrying out solid-liquid separation after the reaction to obtain high-purity zinc-containing leaching solution;
the solid-liquid ratio of the ionic liquid to the zinc-containing dust mud in the leaching process is 1:4-8;
the ultrasonic treatment is carried out by placing an ultrasonic probe at 1.5-2cm below the liquid surface, 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 30-60min;
the leaching reaction temperature is 70-100 ℃, the solid-liquid reaction time is 10-60 minutes, and the stirring speed is 200-400rpm.
2. The method for cooperatively and selectively zinc-leaching by utilizing cyclone classification-ionic liquid-ultrasonic according to claim 1, which is characterized in that: the classifying area of the special-shaped hydrocyclone consists 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 mud is graded and enriched by utilizing a special-shaped hydrocyclone, the grading granularity is 0.018mm, fine grains and middle grain-level high-zinc dust mud are used for leaching and extracting zinc, and coarse grain low-zinc dust mud is used for extracting iron and other valuable metals.
3. The method for cooperatively and selectively zincating by utilizing cyclone classification-ionic liquid-ultrasonic according to claim 2, which is characterized in that: setting parameters of the drying box, namely 353K, -0.05MPa, and drying for 12 hours.
4. A method for co-selective zincating with cyclone classification-ionic liquid-ultrasound according to claim 3, characterized in that: the hydrogen bond acceptor is choline chloride; the hydrogen bond donor is one or more of malonic acid, thiourea, glycol, urea and oxalic acid hydrate.
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| WO2012025568A2 (en) * | 2010-08-24 | 2012-03-01 | Akkuser Oy | Metal ion recovery from battery waste |
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| CN112063849A (en) * | 2020-04-28 | 2020-12-11 | 攀枝花学院 | Method for recovering zinc from blast furnace gas mud |
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| WO2012025568A2 (en) * | 2010-08-24 | 2012-03-01 | Akkuser Oy | Metal ion recovery from battery waste |
| CN110358923A (en) * | 2019-08-15 | 2019-10-22 | 昆明理工大学 | A method of indium is extracted using zinc oxide fumes and recycles zinc oxide fumes |
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