CN110894577B - Method for improving leaching rate of zinc-cobalt slag produced by purifying electrolytic zinc solution - Google Patents

Method for improving leaching rate of zinc-cobalt slag produced by purifying electrolytic zinc solution Download PDF

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CN110894577B
CN110894577B CN201910855149.0A CN201910855149A CN110894577B CN 110894577 B CN110894577 B CN 110894577B CN 201910855149 A CN201910855149 A CN 201910855149A CN 110894577 B CN110894577 B CN 110894577B
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zinc
cobalt
cobalt slag
leaching
slag
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CN110894577A (en
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曾纪斌
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Guangdong Lichang New Material Co.,Ltd.
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/20—Obtaining zinc otherwise than by distilling
    • C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • C22B23/043—Sulfurated acids or salts thereof
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The invention discloses a method for improving leaching rate of zinc-cobalt residue produced by purifying electrolytic zinc solution. The invention adopts a method combining physics and chemistry, firstly, the zinc-cobalt slag is crushed to be below 48 mu m by physical crushing equipment, and CoZn is crushed13The (zinc-cobalt alloy) shell is covered, and then the acid leaching reaction area of the zinc-cobalt slag is increased in the presence of a dispersing agent, so that the zinc-cobalt slag is leached by more than 90% under dilute acid. Compared with the prior art, the invention has the following advantages and effects: (1) compared with the prior art, the method has the advantages that the ton treatment cost is lower; (2) the equipment is simple and the process is safe; (3) the usage of the sulfuric acid is more saved compared with other methods.

Description

Method for improving leaching rate of zinc-cobalt slag produced by purifying electrolytic zinc solution
Technical Field
The invention belongs to the technical field of comprehensive recycling of metal smelting, relates to a method for improving leaching rate of smelting slag by a wet method, and particularly relates to a method for improving leaching rate of zinc-cobalt slag produced by purifying electrolytic zinc solution.
Background
Cobalt is an important metal element. At present, the traditional fields of cobalt consumption and application mainly include battery materials, super heat-resistant alloys, tool steel, hard alloys and magnetic materials; cobalt, consumed in the form of compounds, is mainly used as catalysts, desiccants, reagents, pigments and dyes, and the like. Cobalt-60 is a widely used radioactive material, widely used in biochemistry for activation analysis; in plating, corrosion and catalysis for tracer studies; in medical treatment, it is used for radiological examination and treatment. The raw materials for producing cobalt can be divided into two categories of cobalt minerals and cobalt waste materials, wherein the cobalt waste materials are cobalt slag obtained from systems for smelting nickel, zinc and the like, or waste alloys, battery materials, catalysts and the like.
More than eighty percent of zinc is produced by a wet method all over the world, the zinc hydrometallurgy flow is zinc concentrate roasting, zinc is leached from produced roasted sand, zinc leachate is purified and decontaminated, and zinc is electrodeposited by zinc purification liquid. The zinc leachate purification and impurity removal process can generate various waste residues such as jarosite slag, lead-silver slag, copper-cadmium slag, zinc-cobalt slag and the like. Some of the waste residues are treated to different degrees (for example, lead-silver residues and copper-cadmium residues are comprehensively recovered with lead, silver, copper, zinc and other valuable elements by a wet method), but the zinc-cobalt residues and the like are not effectively treated. At present, zinc-cobalt slag generated by zinc smelting enterprises by a wet method is only subjected to simple acid washing and selective leaching. Because cobalt in the zinc-cobalt slag is mainly CoZn13The zinc-cobalt alloy exists in a form, so that only a small part of metal zinc in the nickel-cobalt slag can be leached out by acid cleaning, a small part of zinc is recovered, and the acid cleaning slagMost of the sold parts are purchased by zinc salt preparation enterprises with small scale, and because of small scale, large slag amount and incomplete environmental protection facilities, the environment is seriously polluted when the zinc-cobalt slag is treated.
The first step of wet recovery of Zn-Co slag is to leach the Zn-Co slag into solution completely, since the Co in the Zn-Co slag is mainly CoZn13The zinc particles are coated with the zinc (zinc-cobalt alloy) form, and the particle size is generally more than 5mm, so that the CoZn is difficult to be treated by the conventional wet acid leaching13(Zinc-cobalt alloy) leaching into solution (CN 106119560A; Lu nationality; research on comprehensive utilization of cobalt slag [ J ]]Non-ferrous metals (smelt section), 2004(1): 501-. In order to improve the leaching rate of cobalt in the zinc-cobalt slag, the following methods are commonly used in the current industrial production: (1) firstly, the zinc-cobalt slag is treated at high temperature by a pyrogenic process and then leached by a wet process, the pretreatment method has high cost, and the leaching effect is still not ideal after the high-temperature pretreatment; (2) the pressure oxidation acid leaching method is adopted for leaching, for example, CN101550485 discloses an oxygen pressure acid leaching method for treating zinc hydrometallurgy purified waste residues), but the technology has higher treatment cost, large production consumption, large waste water amount and no advantage for treating materials with higher zinc and cobalt contents; (3) ammonia leaching process (CN 1310242; Zhao Tiao, Tang-Rong. wet zinc smelting process for purifying cobalt slag [ J)]The university of China and south (Nature science edition), 2001, 32(4): 371-.
Disclosure of Invention
The invention aims to provide a method for improving the wet leaching rate of zinc-cobalt slag generated during the purification and cobalt removal of electrolytic zinc solution, which is realized by the following technical scheme: a method for improving the leaching rate of zinc-cobalt slag produced by purifying electrolytic zinc solution comprises the following steps:
(1) crushing zinc-cobalt slag: weighing the zinc-cobalt slag which is dried to the moisture content of less than 5 wt%, adding a dispersing agent according to the weight ratio of the zinc-cobalt slag to the dispersing agent =1000: 4-12, and crushing.
(2) Grading zinc-cobalt slag: and grading the crushed zinc-cobalt slag to obtain the zinc-cobalt slag with the particle size of less than 48 mu m (300 meshes).
(3) And carrying out acid leaching on the zinc-cobalt slag.
The drying mode in the step (1) is drying, the temperature is 90-100 ℃, and the moisture content is measured according to GB/T8899-.
The dispersant in the step (1) is one or more of polyethylene glycol (molecular weight 6000), sodium dodecyl benzene sulfonate or cetyl trimethyl ammonium bromide. And preferably, the dispersing agent is added according to the weight ratio of the zinc-cobalt slag to the dispersing agent =1000: 4-12.
The physical crushing equipment in the step (1) is one of a Raymond mill, a ball mill, an impact mill, a stirring mill, a vertical mill, a high-pressure roller mill, a vibration mill, a planetary mill and a jet mill.
And (3) grading by using a commercially available mineral grader.
The specific operation of the step (3) is as follows: soaking the zinc-cobalt slag by using dilute acid with the pH = 2.0-3.0, stirring at the speed of 200-300 rpm for 2-3 hours, and stirring at the temperature of 20-40 ℃. The dilute acid is sulfuric acid. The addition amount of the diluted acid is 4:1 (weight ratio) of the diluted acid to the zinc-cobalt slag, and the pH value of the diluted acid is preferably 2.0.
The inventor researches and analyzes and utilizes the characteristics and characteristics of the zinc-cobalt slag in detail. Specifically, cobalt in the zinc-cobalt slag is mainly CoZn13The zinc particles are coated with (zinc-cobalt alloy) form, and the particle diameter is generally more than 5mm, wherein, CoZn13The thickness of the (zinc-cobalt alloy) is generally about 0.2-0.3 mm, and the metal zinc is coated inside the (zinc-cobalt alloy). Based on the above, the present invention uses a physical pulverization method to pulverize spherical zinc-cobalt slag to less than 48 μm so as to crush CoZn13The (zinc-cobalt alloy) shell increases the acid leaching reaction area of the zinc-cobalt slag in the presence of a dispersant, so that the zinc-cobalt slag can be leached under dilute acid.
Thus, compared with the prior art, the invention has the following advantages and effects:
(1) the process of the present invention has a lower ton treatment cost than the prior art.
(2) The method of the invention has simple equipment and safe process.
(3) The method of the invention adopts less sulfuric acid than other methods.
(4) The method has high leaching rate of the zinc-cobalt slag, which reaches more than 90 percent.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The process equipment or devices not specifically noted in the following examples are conventional in the art; all pressure values and ranges refer to absolute pressures.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; it is also to be understood that a combined connection between one or more devices/apparatus as referred to in the present application does not exclude that further devices/apparatus may be present before or after the combined device/apparatus or that further devices/apparatus may be interposed between two devices/apparatus explicitly referred to, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
The evaluation methods involved therein are as follows: the element content test adopts Inductively Coupled Plasma-atomic emission spectrometry (ICP-AES); the moisture test is carried out by using the GB/T6284-.
Example 1
The zinc-cobalt slag used in this example contained 63.13 wt% water, 5.32 wt% zinc, and 0.64 wt% cobalt.
(1) Crushing zinc-cobalt slag: taking 1000kg of zinc-cobalt slag, drying the zinc-cobalt slag at 100 ℃ until the water content is 0 wt%, weighing 631.3kg, adding 3.16kg of dispersant polyethylene glycol (molecular weight 6000) according to the weight ratio of the zinc-cobalt slag to the dispersant =1000:5, and then crushing the zinc-cobalt slag by a Raymond mill.
(2) Grading zinc-cobalt slag: the crushed zinc-cobalt slag was classified by a commercially available mineral classifier to obtain 966kg of zinc-cobalt slag having a particle size of less than 48 μm (300 mesh).
(3) Leaching zinc-cobalt slag: 500kg of zinc-cobalt slag with the particle size of less than 48 mu m (300 meshes) is taken, the zinc-cobalt slag is leached by sulfuric acid with the pH =2.0 according to the liquid-solid ratio of 4:1 (weight ratio), the stirring speed is 200 rpm, the stirring time is 3 hours, and the stirring temperature is 40 ℃.
(4) And (3) measuring the leaching rate of the zinc-cobalt slag: and (4) carrying out filter pressing on the mixed solution obtained in the step (3) by using a commercial filter press to obtain a zinc-cobalt leaching solution, conveying a sample, and measuring the content of zinc and cobalt in the solution.
At the same time, the leaching rates were compared with those in the absence of pulverization (other conditions were the same as above), and the leaching rates in the pressure oxidation acid leaching and the ammonia leaching. Wherein, the pressure oxidation acid leaching method adopts a method reported in CN101550485[ P ]. 2009 (Zhang Guangdong product, Han Bao Ling, Square Mega honing, etc.) for treating zinc hydrometallurgy purified waste residue; the ammonia leaching is carried out by a method reported by Zhao Ting Kai, Tang-Rong, wet zinc smelting and cobalt slag purification new treatment process [ J ]. school newspaper of Zhongnan university (Nature science edition)). The extraction rates of the respective methods are compared and shown in Table 1.
TABLE 1 leaching ratio (%)
Zn Co
Leaching rate in example 1 94.91 92.68
No crushing leaching rate 54.94 43.77
Pressure oxidation acid leaching rate 86.20 74.50
Leaching rate of ammonia leaching 88.23 85.21
Example 2
The zinc-cobalt slag used in this example contained 66.54 wt% water, 5.17 wt% zinc, and 0.52 wt% cobalt.
(1) Crushing zinc-cobalt slag: taking 1000kg of zinc-cobalt slag, drying the zinc-cobalt slag at 90 ℃ until the water content is 5 wt%, weighing 351.33kg, adding 2.81kg of sodium dodecyl benzene sulfonate serving as a dispersant according to the weight ratio of zinc-cobalt slag to dispersant =1000:8, and then crushing the zinc-cobalt slag by using a ball mill.
(2) Grading zinc-cobalt slag: the crushed zinc-cobalt slag was classified by a commercially available mineral classifier to obtain 985kg of zinc-cobalt slag having a particle size of less than 48 μm (300 mesh).
(3) Leaching zinc-cobalt slag: 500kg of zinc-cobalt slag with the particle size of less than 48 mu m (300 meshes) is taken, 2000 kg of sulfuric acid with the pH =2.0 is used for leaching the zinc-cobalt slag, the stirring speed is 300 rpm, the stirring time is 2 hours, and the stirring temperature is 24 ℃.
(4) And (3) measuring the leaching rate of the zinc-cobalt slag: and (4) carrying out filter pressing on the mixed solution obtained in the step (3) by using a commercial filter press to obtain a zinc-cobalt leaching solution, conveying a sample, and measuring the content of zinc and cobalt in the solution.
At the same time, the leaching rates were compared with those in the absence of pulverization (other conditions were the same as above), and the leaching rates in the pressure oxidation acid leaching and the ammonia leaching. The pressure oxidation acid leaching and the ammonia leaching are as described above. The extraction rates of the respective methods are compared as shown in Table 2.
Table 2 zinc cobalt leaching ratio (%)
Zn Co
Leaching rate in this example 92.54 90.36
No crushing leaching rate 53.57 42.68
Pressure oxidation acid leaching rate 84.05 72.64
Leaching rate of ammonia leaching 86.02 83.08
It can be seen from the results that, by using the method of this example, the leaching rates of zinc and cobalt are both greater than 90 wt.%, which is significantly higher than those of the samples without pulverization in the other two methods.
Example 3
The zinc-cobalt slag used in this example contained 68.52 wt% water, 5.67 wt% zinc, and 0.49 wt% cobalt.
(1) Crushing zinc-cobalt slag: taking 1000kg of zinc-cobalt slag, drying the zinc-cobalt slag at 100 ℃ until the water content is 0 wt%, weighing 314.8kg, adding 3.15kg of hexadecyl trimethyl ammonium bromide serving as a dispersant according to the weight ratio of zinc-cobalt slag to dispersant =1000:10, and then crushing the zinc-cobalt slag by using an impact mill.
(2) Grading zinc-cobalt slag: the crushed zinc-cobalt slag was classified by a commercially available mineral classifier to obtain 977kg of zinc-cobalt slag having a particle size of less than 48 μm (300 mesh).
(3) Leaching zinc-cobalt slag: 500kg of zinc-cobalt slag with the particle size of less than 48 mu m (300 meshes) is taken, 2000 kg of sulfuric acid with the pH =3.0 is used for leaching the zinc-cobalt slag, the stirring speed is 200 rpm, the stirring time is 3 hours, and the stirring temperature is 26 ℃.
(4) And (3) measuring the leaching rate of the zinc-cobalt slag: and (4) carrying out filter pressing on the mixed solution obtained in the step (3) by using a commercial filter press to obtain a zinc-cobalt leaching solution, conveying a sample, and measuring the content of zinc and cobalt in the solution.
At the same time, the leaching rates were compared with those in the absence of pulverization (other conditions were the same as above), and the leaching rates in the pressure oxidation acid leaching and the ammonia leaching. The pressure oxidation acid leaching and the ammonia leaching are as described above. The extraction rates of the respective methods are compared as shown in Table 3.
Table 3 zinc cobalt leaching ratio (%)
Zn Co
Leaching rate in this example 93.49 91.29
No crushing leaching rate 54.12 43.11
Pressure oxidation acid leaching rate 84.91 73.38
Leaching rate of ammonia leaching 86.91 83.93
Example 4
The zinc-cobalt slag used in the present example contains 70.2 wt% of water, 4.96 wt% of zinc and 0.83 wt% of cobalt.
(1) Crushing zinc-cobalt slag: taking 1000kg of zinc-cobalt slag, drying the zinc-cobalt slag at 95 ℃ until the water content is 2.5 wt%, weighing 305.5kg, adding 1.53kg of dispersant polyethylene glycol (molecular weight 6000) according to the weight ratio of the zinc-cobalt slag to the dispersant =1000:5, and then crushing the zinc-cobalt slag by a stirring mill.
(2) Grading zinc-cobalt slag: the crushed zinc-cobalt slag was classified by a commercially available mineral classifier to obtain 983kg of zinc-cobalt slag having a particle size of less than 48 μm (300 mesh).
(3) Leaching zinc-cobalt slag: 500kg of zinc-cobalt slag with the particle size of less than 48 mu m (300 meshes) is taken, 2000 kg of sulfuric acid with the pH =3.0 is used for leaching the zinc-cobalt slag, the stirring speed is 300 rpm, the stirring time is 2 hours, and the stirring temperature is 28 ℃.
(4) And (3) measuring the leaching rate of the zinc-cobalt slag: and (4) carrying out filter pressing on the mixed solution obtained in the step (3) by using a commercial filter press to obtain a zinc-cobalt leaching solution, conveying a sample, and measuring the content of zinc and cobalt in the solution.
At the same time, the leaching rates were compared with those in the absence of pulverization (other conditions were the same as above), and the leaching rates in the pressure oxidation acid leaching and the ammonia leaching. The pressure oxidation acid leaching and the ammonia leaching are as described above. The extraction rates of the respective methods are compared and shown in Table 4.
Table 4 example 4 zinc cobalt leaching rate (%)
Zn Co
Leaching rate in this example 94.44 92.22
No crushing leaching rate 54.67 43.55
Pressure oxidation acid leaching rate 85.77 74.13
Leaching rate of ammonia leaching 87.79 84.78
Example 5
The zinc-cobalt slag used in this example contained 61.83 wt% water, 6.52 wt% zinc and 0.81 wt% cobalt.
(1) Crushing zinc-cobalt slag: taking 1000kg of zinc-cobalt slag, drying the zinc-cobalt slag at 97 ℃ until the water content is 2.0 wt%, weighing 389.33kg, adding 2.34kg of sodium dodecyl benzene sulfonate serving as a dispersant according to the weight ratio of zinc-cobalt slag to dispersant =1000:6, and then crushing the zinc-cobalt slag by using a vertical mill.
(2) Grading zinc-cobalt slag: the crushed zinc-cobalt slag was classified by a commercially available mineral classifier to obtain 969kg of zinc-cobalt slag having a particle size of less than 48 μm (300 mesh).
(3) Leaching zinc-cobalt slag: 500kg of zinc-cobalt slag with the particle size of less than 48 mu m (300 meshes) is taken, 2000 kg of sulfuric acid with the pH =2.5 is used for leaching the zinc-cobalt slag, the stirring speed is 200 rpm, the stirring time is 3 hours, and the stirring temperature is 30 ℃.
(4) And (3) measuring the leaching rate of the zinc-cobalt slag: and (4) carrying out filter pressing on the mixed solution obtained in the step (3) by using a commercial filter press to obtain a zinc-cobalt leaching solution, conveying a sample, and measuring the content of zinc and cobalt in the solution.
At the same time, the leaching rates were compared with those in the absence of pulverization (other conditions were the same as above), and the leaching rates in the pressure oxidation acid leaching and the ammonia leaching. The pressure oxidation acid leaching and the ammonia leaching are as described above. The extraction rates of the respective methods are compared as shown in Table 5.
TABLE 5 example 5 leaching rate (%)
Zn Co
Leaching rate in this example 95.38 93.14
No crushing leaching rate 55.21 43.99
Pressure oxidation acid leaching rate 86.63 74.87
Leaching rate of ammonia leaching 88.67 85.64
Example 6
The zinc-cobalt slag used in the present example contains 64.73 wt% of water, 5.68 wt% of zinc and 0.53 wt% of cobalt.
(1) Crushing zinc-cobalt slag: 1000kg of zinc-cobalt slag is taken, the zinc-cobalt slag is dried at 98 ℃ until the water content is 1.3 wt%, the weight is 357.29kg, 2.5kg of hexadecyl trimethyl ammonium bromide serving as a dispersant is added according to the weight ratio of the zinc-cobalt slag to the dispersant =1000:7, and then the zinc-cobalt slag is crushed by a high-pressure roller mill.
(2) Grading zinc-cobalt slag: the crushed zinc-cobalt slag was classified by a commercially available mineral classifier to obtain 975kg of zinc-cobalt slag having a particle size of less than 48 μm (300 mesh).
(3) Leaching zinc-cobalt slag: 500kg of zinc-cobalt slag with the particle size of less than 48 mu m (300 meshes) is taken, 2000 kg of sulfuric acid with the pH =2.5 is used for leaching the zinc-cobalt slag, the stirring speed is 300 rpm, the stirring time is 2 hours, and the stirring temperature is 33 ℃.
(4) And (3) measuring the leaching rate of the zinc-cobalt slag: and (4) carrying out filter pressing on the mixed solution obtained in the step (3) by using a commercial filter press to obtain a zinc-cobalt leaching solution, conveying a sample, and measuring the content of zinc and cobalt in the solution.
At the same time, the leaching rates were compared with those in the absence of pulverization (other conditions were the same as above), and the leaching rates in the pressure oxidation acid leaching and the ammonia leaching. The pressure oxidation acid leaching and the ammonia leaching are as described above. The extraction rates of the various methods are compared in Table 6
Table 6 example 6 leaching rate (%)
Zn Co
Leaching rate in this example 95.86 93.61
No crushing leaching rate 55.49 44.21
Pressure oxidation acid leaching rate 87.06 75.25
Leaching rate of ammonia leaching 89.11 86.06
Example 7
The zinc-cobalt slag used in this example contained 68.89 wt% water, 8.77 wt% zinc, and 0.92 wt% cobalt.
(1) Crushing zinc-cobalt slag: taking 1000kg of zinc-cobalt slag, drying the zinc-cobalt slag at 100 ℃ until the water content is 0 wt%, weighing 311.1kg, adding 2.49kg of dispersant polyethylene glycol (molecular weight 6000) according to the weight ratio of the zinc-cobalt slag to the dispersant =1000:8, and then crushing the zinc-cobalt slag by using a vibration mill.
(2) Grading zinc-cobalt slag: the crushed zinc-cobalt slag was classified by a commercially available mineral classifier to obtain 981kg of zinc-cobalt slag having a particle size of less than 48 μm (300 mesh).
(3) Leaching zinc-cobalt slag: 500kg of zinc-cobalt slag with the particle size of less than 48 mu m (300 meshes) is taken, 2000 kg of sulfuric acid with the pH =2.0 is used for leaching the zinc-cobalt slag, the stirring speed is 250 rpm, the stirring time is 3 hours, and the stirring temperature is 36 ℃.
(4) And (3) measuring the leaching rate of the zinc-cobalt slag: and (4) carrying out filter pressing on the mixed solution obtained in the step (3) by using a commercial filter press to obtain a zinc-cobalt leaching solution, conveying a sample, and measuring the content of zinc and cobalt in the solution.
At the same time, the leaching rates were compared with those in the absence of pulverization (other conditions were the same as above), and the leaching rates in the pressure oxidation acid leaching and the ammonia leaching. The pressure oxidation acid leaching and the ammonia leaching are as described above. The extraction rates of the various methods are compared in Table 7
TABLE 7 example 7 leaching rate (%)
Zn Co
Leaching rate in this example 96.33 94.07
No crushing leaching rate 55.76 44.43
Pressure oxidation acid leaching rate 87.49 75.62
Leaching rate of ammonia leaching 89.55 86.49
Example 8
The zinc-cobalt slag used in this example contained 65.52 wt% of water, 5.87 wt% of zinc and 0.33 wt% of cobalt.
(1) Crushing zinc-cobalt slag: taking 1000kg of zinc-cobalt slag, drying the zinc-cobalt slag at 95 ℃ until the water content is 5 wt%, weighing 362.04kg, adding 3.26kg of sodium dodecyl benzene sulfonate serving as a dispersant according to the weight ratio of zinc-cobalt slag to dispersant =1000:9, and then crushing the zinc-cobalt slag by using a planetary mill.
(2) Grading zinc-cobalt slag: the crushed zinc-cobalt slag was classified by a commercially available mineral classifier to obtain 969kg of zinc-cobalt slag having a particle size of less than 48 μm (300 mesh).
(3) Leaching zinc-cobalt slag: 500kg of zinc-cobalt slag with the particle size of less than 48 mu m (300 meshes) is taken, 2000 kg of sulfuric acid with the pH =3.0 is used for leaching the zinc-cobalt slag, the stirring speed is 250 rpm, the stirring time is 2 hours, and the stirring temperature is 38 ℃.
(4) And (3) measuring the leaching rate of the zinc-cobalt slag: and (4) carrying out filter pressing on the mixed solution obtained in the step (3) by using a commercial filter press to obtain a zinc-cobalt leaching solution, conveying a sample, and measuring the content of zinc and cobalt in the solution.
At the same time, the leaching rates were compared with those in the absence of pulverization (other conditions were the same as above), and the leaching rates in the pressure oxidation acid leaching and the ammonia leaching. The pressure oxidation acid leaching and the ammonia leaching are as described above. The extraction rates of the respective methods are compared and shown in Table 8.
Table 8 example 8 zinc cobalt leaching rate (%)
Zn Co
Leaching rate in this example 96.81 94.53
No crushing leaching rate 56.04 44.65
Pressure oxidation acid leaching rate 87.92 75.99
Leaching rate of ammonia leaching 89.99 86.91
Example 9
The zinc-cobalt slag used in this example contained 67.57 wt% water, 7.91 wt% zinc, and 0.57 wt% cobalt.
(1) Crushing zinc-cobalt slag: 1000kg of zinc-cobalt slag is taken, the zinc-cobalt slag is dried at 97 ℃ until the water content is 1.2 wt%, the weight is 328.19kg, 3.28kg of dispersant cetyl trimethyl ammonium bromide is added according to the weight ratio of the zinc-cobalt slag to the dispersant =1000:10, and then the zinc-cobalt slag is crushed by an air flow crusher.
(2) Grading zinc-cobalt slag: the crushed zinc-cobalt slag is classified by a commercial mineral classifier to obtain 997kg of zinc-cobalt slag with the grain size of less than 48 mu m (300 meshes).
(3) Leaching zinc-cobalt slag: 500kg of zinc-cobalt slag with the particle size of less than 48 mu m (300 meshes) is taken, 2000 kg of sulfuric acid with the pH =2.0 is used for leaching the zinc-cobalt slag, the stirring speed is 200 rpm, the stirring time is 3 hours, and the stirring temperature is 20 ℃.
(4) And (3) measuring the leaching rate of the zinc-cobalt slag: and (4) carrying out filter pressing on the mixed solution obtained in the step (3) by using a commercial filter press to obtain a zinc-cobalt leaching solution, conveying a sample, and measuring the content of zinc and cobalt in the solution.
At the same time, the leaching rates were compared with those in the absence of pulverization (other conditions were the same as above), and the leaching rates in the pressure oxidation acid leaching and the ammonia leaching. The pressure oxidation acid leaching and the ammonia leaching are as described above. The extraction rates of the respective methods are compared and shown in Table 9.
TABLE 9 example 9 leaching rate (%)
Zn Co
Leaching rate in this example 97.28 95.00
No crushing leaching rate 56.31 44.86
Pressure oxidation acid leaching rate 88.36 76.36
Leaching rate of ammonia leaching 90.44 87.34
From the above examples, it is shown that if the same procedure is used without crushing the sample, the leaching rates are very low, and the leaching rates of zinc and cobalt are all between 40-60%, whereas with the method of the present invention, the leaching rates of zinc and cobalt are all greater than 90 wt%, and can reach 97.28% and 95.00% at the highest, respectively, and the leaching rates obtained in each example are higher than those obtained in the other two methods, i.e., pressure oxidation acid leaching and ammonia leaching.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (5)

1. A method for improving the leaching rate of zinc-cobalt slag produced by purifying electrolytic zinc solution is characterized by comprising the following steps:
(1) crushing zinc-cobalt slag: drying the zinc-cobalt slag until the water content is below 5 wt%, adding a dispersing agent according to the weight ratio of the zinc-cobalt slag to the dispersing agent =1000: 5-10, and then crushing the zinc-cobalt slag; the dispersant is one of polyethylene glycol with molecular weight of 6000, sodium dodecyl benzene sulfonate or cetyl trimethyl ammonium bromide;
(2) grading zinc-cobalt slag: grading the crushed zinc-cobalt slag to obtain zinc-cobalt slag with the particle size of less than 48 mu m;
(3) acid leaching is carried out on the zinc-cobalt slag, namely the zinc-cobalt slag is leached out by dilute acid with the pH = 2.0-3.0, the stirring speed is 200-300 rpm, the stirring time is 2-3 hours, and the stirring temperature is 20-40 ℃.
2. The method for improving the leaching rate of the residues generated in the purification of the electrolytic zinc solution for producing the zinc and cobalt according to claim 1, which is characterized in that: the drying temperature in the step (1) is 90-100 ℃, and the moisture determination is carried out according to GB/T8899-.
3. The method for improving the leaching rate of the zinc-cobalt slag produced by purifying the electrolytic zinc solution according to claim 1, which is characterized in that: the crushing equipment in the step (1) is one of a Raymond mill, a ball mill, an impact mill, a stirring mill, a vertical mill, a high-pressure roller mill, a vibration mill, a planetary mill and a jet mill.
4. The method for improving the leaching rate of the residues generated in the purification of the electrolytic zinc solution for producing the zinc and cobalt according to claim 1, which is characterized in that: and (3) grading is completed by adopting a mineral grader.
5. The method for improving the leaching rate of the residues generated in the purification of the electrolytic zinc solution for producing the zinc and cobalt according to claim 1, which is characterized in that: and (4) the dilute acid in the step (3) is sulfuric acid, and the addition amount of the dilute acid is 4:1 in weight ratio to the zinc-cobalt slag.
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