CN114196835B - Method for selectively leaching tin from tin-containing metallurgical slag - Google Patents
Method for selectively leaching tin from tin-containing metallurgical slag Download PDFInfo
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- CN114196835B CN114196835B CN202111550394.4A CN202111550394A CN114196835B CN 114196835 B CN114196835 B CN 114196835B CN 202111550394 A CN202111550394 A CN 202111550394A CN 114196835 B CN114196835 B CN 114196835B
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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
- C22B7/04—Working-up slag
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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
- C22B25/00—Obtaining tin
- C22B25/04—Obtaining tin by wet processes
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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
- C22B25/00—Obtaining tin
- C22B25/06—Obtaining tin from scrap, especially tin scrap
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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
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- 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 selectively leaching tin from tin-containing metallurgical slag, which comprises the steps of carrying out leaching reaction on tin-containing metallurgical slag powder and a leaching agent containing organic carboxylic acid, and then carrying out solid-liquid separation to obtain tin-containing leaching solution; the method can realize the high-efficiency enrichment and separation of tin in the tin-containing metallurgical slag, the extraction rate of the tin is higher than 95 percent, the leaching selectivity of the tin is good, the tin-containing metallurgical slag can be treated in a wide variety, the method is environment-friendly, the operation is simple, and the production cost is low, and the method can be used for industrial production.
Description
Technical Field
The invention relates to a method for recovering tin from tin-containing metallurgical slag, in particular to a method for selectively leaching tin from tin-containing metallurgical slag, and belongs to the field of hydrometallurgy.
Background
Tin is one of the earliest metals produced and used by humans, has a low melting point, can form an alloy with various metals, is nontoxic and corrosion-resistant, and has the characteristics of good ductility, attractive appearance and the like. Tin is a rare and expensive heavy metal, its valuable tin ore species is single, and 50 or more tin minerals have been found, but only cassiterite and tetrahedrite are industrially valuable, with about 95% of the metallic tin being from cassiterite. With the continuous development of economy, the consumption of tin is increased year by year, and the problems of the reduction of the grade of tin ore, the deficiency of subsequent resources and the exhaustion of resources are faced at home and abroad to different degrees. The amount of tin waste in the industrial production process or life is continuously increasing, and the resource reserves are gradually decreasing. The recycling of tin secondary resources has attracted global attention. Some nonferrous metal ores are often accompanied with a small amount of tin elements, various solid wastes are generated in the smelting process, wherein the grade of tin is more than 0.3wt.%, and the tin is higher than the exploitation grade of common tin ores, and has a certain recovery value. For example, in the zinc hydrometallurgy process, the added zinc sulfide ore contains about 0.01 percent of tin element, and after oxidizing roasting and three-stage leaching, the tin is enriched in leaching slag, and the tin grade is 0.3 to 0.7 percent. The recovery of tin from tin-containing smelting slag not only can utilize tin secondary resources to supplement the shortages of world primary tin ore resources, but also can save energy and protect environment from pollution, and simultaneously can reduce industrial production cost.
Aiming at the characteristics of low grade, fine granularity, complex valence state and composition of tin-containing metallurgical slag, the current treatment method for the tin-containing metallurgical slag comprises a pyrogenic process and a wet process.
The pyrogenic process utilizes the characteristic of low boiling points of stannous oxide, stannous sulfide and stannous chloride, and mainly comprises a vulcanization volatilization method, a reduction volatilization method, a chlorination volatilization method and the like. For example, in chinese patent CN102899502a, the tin-containing zinc leaching slag is placed in a fuming furnace to undergo high-temperature reduction volatilization at 1200-1350 ℃, and zinc-tin-indium smoke dust is subjected to acid washing and impurity removal, and then is subjected to reduction smelting again, so as to obtain crude tin with tin content of 92%. Since 1963, the cloud and south tin industry company developed a chloridizing volatilization method, and applied patent CN86101034 can economically and effectively enrich tin from complex low-grade tin-containing materials, the tin volatilization rate reaches more than 94%, and the effect of separating tin and iron in hard heads can be achieved. The pyrogenic process can effectively treat low-grade high-impurity complex lean tin materials, but sulfur and chlorine are harmful elements, and harmful gas SO is generated in the roasting process 2 And HCl, etc., which causes serious secondary pollution and equipment corrosion. In addition, the recovery of tin by pyrometallurgy requires high grade (3.6% -6.5%), high energy consumption and serious pollution.
The wet process and the combined process comprise an acid method and an alkali method, and the alkali method adopts the principle that alkali substances such as sodium hydroxide, sodium carbonate, sodium peroxide and the like are used for converting Sn in the slag into Na 2 SnO 3 For example, patent CN201510689263.2 uses NaOH solution and oxidant to treat regenerated lead smelting slag containing 30-75% lead and 5-10% tin, and the leaching solution is concentrated and crystallized after impurity removal to obtain sodium stannate product with content more than 99%. However, tin dioxide is difficult to dissolve in acid and alkali under general conditions, so that the consumption of the alkali is large, and the temperature required in alkaline leaching is high. Therefore, the patent 201610867463.7 adopts an oxygen pressure alkaline leaching method, and the reaction temperature is controlled to be 150-250 ℃ and the oxygen partial pressure is controlled to be 0.5-1.5 MPa in a high-pressure reaction kettle, so that the removal rate of tin reaches more than 98.0%. The alkaline process has the defects that other elements (Sb, pb, as and the like) are leached in large quantity while tin elements are leached, the alkali consumption is large, and the subsequent impurity removal process is complex and tedious. The acid process is usually carried out by high concentrationLeaching tin element with hydrochloric acid or sulfuric acid at high temperature, such as water-soluble leaching of 98% sulfuric acid for electric furnace smoke in patent CN102140580B, and SnCl in patent 201510043995.4 4 The HCl-additive system leaches tin, using hydrochloric acid at concentrations up to 8mol/L. The acid method process has the defects of harsh acid leaching conditions, severe corrosion of HCl to equipment and more impurity elements in leaching liquid.
In summary, the prior art has the defects of harsh reaction conditions, complex and cumbersome subsequent separation process, poor tin selectivity, high energy consumption, serious pollution, high equipment requirement and the like. Therefore, the development of a method for selectively leaching tin from tin-containing metallurgical slag has very important practical significance for realizing the comprehensive utilization of refractory tin-containing materials and accelerating the large-scale utilization of tin-containing secondary resources.
Disclosure of Invention
Aiming at the defects of the method for recovering tin in tin-containing metallurgical slag in the prior art, the invention aims to provide the method for leaching tin in the tin-containing metallurgical slag by the wet method, which has high leaching rate of tin in the tin-containing metallurgical slag, good leaching selectivity of tin, wide variety of treatable tin-containing metallurgical slag, environmental friendliness, simple operation and production cost and can be used for industrial production.
In order to achieve the technical aim, the invention provides a method for selectively leaching tin from tin-containing metallurgical slag, which comprises the steps of carrying out leaching reaction on tin-containing metallurgical slag powder and a leaching agent, and then carrying out solid-liquid separation to obtain tin-containing leaching solution; the leachable agent comprises an organic carboxylic acid.
The key of the technical scheme of the invention is that a special leaching agent is adopted, so that tin elements in a complex metal system of the tin-containing metallurgical slag can be leached out with high selectivity and high efficiency, and other metal elements commonly existing in the tin-containing metallurgical slag, such as zinc, lead, calcium, magnesium, iron, aluminum and the like, are left in the slag, thereby realizing the high-efficiency separation of tin from other metal elements in the leaching source process and providing favorable conditions for the subsequent tin purification and enrichment process and the preparation of high-purity tin products.
As a preferred embodiment, the organic carboxylic acid is at least one of oxalic acid, citric acid, tartaric acid, gluconic acid, tannic acid, and malic acid. The organic carboxylic acid preferred by the technical scheme of the invention has excellent selectivity on leaching of tin, can form stable soluble complex with tin, and can form indissoluble or slightly soluble complex with other impurity elements such as calcium, magnesium, zinc, lead, iron and the like, so that the metal ions can be precipitated in a slag phase, thereby realizing the selective and efficient leaching of tin.
As a preferable scheme, the concentration of the organic carboxylic acid in the leaching agent is 8-100 g/L. The concentration of the organic carboxylic acid in the leaching agent is more preferably 10-60 g/L. When the concentration of the leaching agent is too low, the leaching rate of tin is low, the recovery efficiency is low, and when the concentration of the leaching agent is too high, the excessive leaching agent does not play a leaching role, so that raw materials are wasted.
As a preferred embodiment, the leaching agent comprises sulfuric acid and/or hydrogen peroxide. A small amount of sulfuric acid and/or hydrogen peroxide can be added into the leaching agent as an auxiliary agent for leaching tin, and the auxiliary agent has good matching property with organic carboxylic acid and can accelerate the leaching of tin. These adjuvants promote the leaching of tin from tin-bearing metallurgical slag by organic carboxylic acids through different principles of action. For example, the addition of small amounts of sulfuric acid is mainly used to increase H in the leachable agent + The concentration is further improved, the potential range in which tin in the leaching solution can stably exist is further improved, and a proper amount of H 2 O 2 Can oxidize organic carboxylic acid leaches, e.g. H 2 O 2 Oxidizing oxalic acid produces peroxyoxalic acid, which accelerates the coordination reaction.
As a preferable scheme, the total concentration of sulfuric acid and hydrogen peroxide in the leaching agent is lower than 2mol/L. The total concentration of sulfuric acid and hydrogen peroxide in the leaching agent is more preferably 0.25-1 mol/L. Too high a concentration of sulfuric acid can cause simultaneous leaching of other metal ions, and further purification and impurity removal are required when tin is recovered from the leachate. H 2 O 2 When the addition amount is too large, sn in the leachate may be added 2+ Oxidation to SnO 2 And (5) precipitation. Too little of the leaching aid is added to have the effect of promoting tin leaching.
As a preferred embodiment, the conditions of the leaching reaction are: the liquid-solid ratio is 5-15 mL/g, the temperature is 30-100 ℃ and the time is 2-60 min. Further preferably, the conditions of the leaching reaction are: the liquid-solid ratio is 8-10 mL/g, the temperature is 50-100 ℃ and the time is 10-30 min.
As a preferable scheme, the tin-containing metallurgical slag is at least one of tin-containing smoke dust, zinc leaching slag, copper smelting slag and lead smelting slag.
As a preferable scheme, the grade of tin element in the tin-containing metallurgical slag is 0.2-7 wt.%.
As a preferred scheme, the tin-containing metallurgical slag powder is obtained by subjecting tin-containing metallurgical slag to a pretreatment process including cleaning, drying, mechanical crushing or wet grinding and drying. Washing tin-containing metallurgical slag with water or dilute acid, drying at above 100 ℃ until the weight is no longer changed, and mechanically crushing until the granularity is less than 0.75 mu m and accounts for 60-80%. Or adopting a direct wet grinding method, wherein the specific conditions are as follows: mineral water (acid) ratio 1: 1-2, and the ball-to-material ratio is 10-30: 1, the time is 10-60 min. The tin-containing metallurgical slag often contains soluble impurities, and the dissolution of the impurities in the subsequent leaching process can be effectively reduced by using a water washing or dilute acid washing process. The washed tin-containing metallurgical slag is ground to be beneficial to increasing the specific surface area, so that the tin-containing metallurgical slag can fully react with the leaching agent, and the reaction rate is accelerated.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
according to the technical scheme, the special leaching agent is used, so that the leaching agent has high selectivity and high leaching rate for leaching tin in tin-containing smelting slag, the leaching rate of tin can reach more than 95%, the effective separation of tin and impurity elements is realized, the impurities in the tin-containing leaching solution are obviously reduced, and the capability reduction of a subsequent enrichment process and the influence on the purity of products are avoided.
The technical scheme of the invention has wide variety of treatable tin-containing metallurgical slag, the concentration of the used acid, environmental friendliness, simple operation and production cost, and can be used for industrial production.
Detailed Description
The invention is further illustrated and described below in connection with specific examples. These examples are provided only for a better understanding of the present invention and are not intended to limit the scope of the present invention.
Example 1
Washing tin-containing metallurgical slag with water, drying at 100 ℃ for 12 hours, and mechanically crushing until the granularity is less than 0.75 mu m and 60% -80% to obtain tin-containing metallurgical slag powder (the components are shown in table 1); adding the powder into a mixed solution of 20g/L oxalic acid and 0.5mol/L sulfuric acid, and leaching at 60 ℃ for 30min; filtering out residues and leaching liquid after the reaction is finished, and collecting tin-containing leaching liquid.
And measuring the concentration of each element in the leaching solution, and calculating leaching rate to obtain the leaching solution with Sn leaching rate of 96.9%, fe leaching rate of 15.5% and Ca, zn, pb, al, mg leaching rate of less than 3%.
Table 1 certain tin-containing metallurgical slag composition, wt.%
Example 2
The tin-containing metallurgical slag is treated by 0.25mol/L H 2 SO 4 Cleaning, drying at 100 ℃ for 12 hours, and mechanically crushing until the granularity is less than 0.75 mu m and 60% -80% to obtain tin-containing metallurgical slag powder (the components are shown in table 1); adding the powder into 15g/L oxalic acid, 10g/L citric acid and 0.5mol/LH 2 O 2 Leaching in the mixed solution at 80 ℃ for 30min; filtering out residues and leaching liquid after the reaction is finished, and collecting tin-containing leaching liquid.
And measuring the concentration of each element in the leaching solution, and calculating leaching rate to obtain the leaching solution with Sn leaching rate of 98.1%, fe leaching rate of 5.6% and Ca, zn, pb, al, mg leaching rate of less than 3%.
At the same time, 0.5mol/LH is not added 2 O 2 As a control, tin-containing metallurgical slag is leached according to the above steps and a tin-containing leachate is obtained. And measuring the concentration of each element in the leaching solution, and calculating leaching rate to obtain the leaching solution with Sn leaching rate of 84.9%, fe leaching rate of 11.5% and Ca, zn, pb, al, mg leaching rate of less than 3%.
Example 3
The tin-containing metallurgical slag is treated by 0.25mol/LH 2 SO 4 Wet milling, mineral water (acid) ratio 1:1, ball-to-material ratio 10:1, for 15min to obtainTo tin-containing metallurgical slag powder (the components are shown in table 1), wherein the granularity is less than 0.75 mu m and accounts for 60% -80%; adding the powder into 30g/L tartaric acid, 5g/L tannic acid and 0.5mol/L H 2 SO 4 Leaching the mixed solution at 90 ℃ for 1h; filtering out residues and leaching liquid after the reaction is finished, and collecting tin-containing leaching liquid.
And measuring the concentration of each element in the leaching solution, and calculating leaching rate to obtain the leaching solution with Sn leaching rate of 96.5%, fe leaching rate of 6.6% and Ca, zn, pb, al, mg leaching rate of less than 3%.
Example 4
Wet grinding tin-containing metallurgical slag with water, wherein the mineral water ratio is 1:1, ball-to-material ratio 10:1, the time is 15min, and tin-containing metallurgical slag powder (the components are shown in the table 1) is obtained, wherein the granularity is smaller than 0.75 mu m and accounts for 60% -80%; adding the powder into 30g/L oxalic acid, 5g/L tartaric acid and 1mol/LH 2 SO 4 Leaching the mixed solution at 30 ℃ for 1h; filtering out residues and leaching liquid after the reaction is finished, and collecting tin-containing leaching liquid.
And measuring the concentration of each element in the leaching solution, and calculating leaching rate to obtain the leaching solution with Sn leaching rate of 85.6%, fe leaching rate of 15.0% and Ca, zn, pb, al, mg leaching rate of less than 3%.
Example 5
Washing tin-containing metallurgical slag with water, drying at 100 ℃ for 12 hours, and mechanically crushing until the granularity is less than 0.75 mu m and 60% -80% to obtain tin-containing metallurgical slag powder (the components are shown in table 1); adding the powder into 36g/L oxalic acid, 0.5mol/L sulfuric acid and 0.2mol/LH 2 O 2 Leaching the mixed solution at 60 ℃ for 30min; filtering out residues and leaching liquid after the reaction is finished, and collecting tin-containing leaching liquid.
And measuring the concentration of each element in the leaching solution, and calculating leaching rate to obtain the leaching solution with Sn leaching rate of 98.9%, fe leaching rate of 16.9% and Ca, zn, pb, al, mg leaching rate of less than 3%.
Comparative example 1
The concentration of leachable agent in this comparative example is not within the preferred range.
Washing tin-containing metallurgical slag with water, drying at 100 ℃ for 12 hours, and mechanically crushing until the granularity is less than 0.75 mu m and 60% -80% to obtain tin-containing metallurgical slag powder (the components are shown in table 1); adding the powder into a mixed solution of 6g/L oxalic acid and 0.5mol/L sulfuric acid, and leaching at 90 ℃ for 1h; filtering out residues and leaching liquid after the reaction is finished, and collecting tin-containing leaching liquid.
And measuring the concentration of each element in the leaching solution, and calculating leaching rate to obtain the Sn leaching rate of 58.2%, the Fe leaching rate of 20.4% and the Ca, zn, pb, al, mg leaching rate of less than 3%.
Comparative example 2
The leaching reaction conditions in this comparative example were not within the preferred range.
Washing tin-containing metallurgical slag with water, drying at 100 ℃ for 12 hours, and mechanically crushing until the granularity is less than 0.75 mu m and 60% -80% to obtain tin-containing metallurgical slag powder (the components are shown in table 1); adding the powder into a mixed solution of 20g/L oxalic acid and 0.5mol/L sulfuric acid, and leaching at 25 ℃ for 10min; filtering out residues and leaching liquid after the reaction is finished, and collecting tin-containing leaching liquid.
And measuring the concentration of each element in the leaching solution, and calculating leaching rate to obtain the leaching solution with Sn leaching rate of 49.7%, fe leaching rate of 10.7% and Ca, zn, pb, al, mg leaching rate of less than 3%.
In conclusion, through analysis of comparative examples, the leaching agent and the auxiliary leaching agent are combined, the leaching agent has selectivity on leaching tin in tin-containing smelting slag, the leaching rate of tin can reach more than 95% under the preferable reaction condition, and the method has the advantages of simple process flow, low requirement on equipment and suitability for industrialized mass production.
Claims (1)
1. A method for selectively leaching tin from tin-containing metallurgical slag, which is characterized by comprising the following steps: carrying out leaching reaction on the tin-containing metallurgical slag powder and a leaching agent, and then carrying out solid-liquid separation to obtain a tin-containing leaching solution; the leaching agent comprises an organic carboxylic acid; the organic carboxylic acid is at least one of oxalic acid, citric acid, tartaric acid, gluconic acid, tannic acid and malic acid; the concentration of the organic carboxylic acid in the leaching agent is 8-100 g/L; the leaching agent comprises sulfuric acid and/or hydrogen peroxide; the leaching reaction conditions are as follows: the liquid-solid ratio is 5-15 mL/g, the temperature is 30-100 ℃ and the time is 2-60 min; the total concentration of sulfuric acid and hydrogen peroxide in the leaching agent is lower than 2mol/L; the tin-containing metallurgical slag is at least one of tin-containing smoke dust, zinc leaching slag, copper smelting slag and lead smelting slag; and the tin element grade in the tin-containing metallurgical slag is 0.2-7wt%.
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