CN113355527B - Treatment method of high-sulfur smelting slag - Google Patents
Treatment method of high-sulfur smelting slag Download PDFInfo
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- CN113355527B CN113355527B CN202110512950.2A CN202110512950A CN113355527B CN 113355527 B CN113355527 B CN 113355527B CN 202110512950 A CN202110512950 A CN 202110512950A CN 113355527 B CN113355527 B CN 113355527B
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of 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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
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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
- C22B15/00—Obtaining copper
- C22B15/0002—Preliminary treatment
- C22B15/0004—Preliminary treatment without modification of the copper constituent
- C22B15/0008—Preliminary treatment without modification of the copper constituent 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
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- 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
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Abstract
The invention discloses a treatment method of high-sulfur smelting slag, which comprises the following steps: mixing the high-sulfur smelting slag and the solution, feeding the mixture into a reaction kettle, heating the mixture to a certain temperature, stopping heating, starting heat preservation when the temperature is reduced to 105-115 ℃, maintaining the temperature for a period of time, stopping heat preservation, taking out the materials in the kettle when the temperature is reduced to room temperature, firstly passing through a 20-30-mesh screen, wherein oversize is coarse sulfur, and undersize is subjected to solid-liquid separation to obtain filter residue and filtrate, wherein the filter residue is enrichment of valuable metals such as bismuth, lead, copper, zinc, nickel and the like, and the valuable metals are recycled, and the filtrate is sent to wastewater treatment. The method can separate the elemental sulfur in the high-sulfur smelting slag, enables valuable metals in the smelting slag to be obviously enriched, becomes metal concentrate with refining value, and has the characteristics of short flow, good elemental sulfur separation effect, low cost, simplicity, easiness in implementation and the like.
Description
Technical Field
The invention belongs to the technical field of comprehensive resource recycling and hydrometallurgy, and particularly relates to a treatment method of high-sulfur smelting slag.
Background
In the metal smelting industry, smelting slag with high elemental sulfur content and a certain amount of valuable metals is often generated, such as arsenic filter cake oxidation cleaning residue, zinc concentrate pressure leaching residue, nickel matte oxygen pressure acid leaching residue and the like, the elemental sulfur content in the smelting slag is generally about 70%, the metal content is 10-20%, the smelting slag also contains a certain amount of arsenic, the smelting slag belongs to solid dangerous waste and cannot be randomly disposed, but the smelting slag has better comprehensive recycling value due to the fact that the smelting slag often contains the valuable metals such as bismuth, lead, copper, zinc, nickel and the like.
For the treatment of such smelting slag, at present, a wet leaching method is generally adopted to extract valuable metals therein to obtain valuable metal concentrates with low arsenic and elemental sulfur contents, for example, a certain factory adopts a pressure cooking dearsenification-chlorine salt leaching-neutralization precipitation-liquid alkali transformation method to extract bismuth in arsenic filter cake oxidation cleaning residues, but such treatment methods often have the problems of long treatment process, low valuable metal recovery rate, high treatment cost, difficult treatment of leaching residues and the like, and a replacement process is urgently needed.
There are also some patents reporting pyrometallurgical treatment of slag with high elemental sulfur content, the common methods are roasting and distillation. The roasting method is to burn the elemental sulfur in smelting into sulfur oxide (SOx) in a high temperature furnace for removal, and the distillation method is to sublimate the sulfur in the material into sulfur vapor by heating under the vacuum condition for removal. The roasting method is difficult to be applied industrially due to the problems of poor combustion controllability, serious acid corrosion, arsenic pollution and the like, the distillation method can produce high-grade sulfur products, but the equipment investment is large, the operation cost is high, the operation of collecting the sulfur products is difficult to control, the desulfurization effect is general, and the obtained sulfur products are also very cheap, so the method cannot be really applied to industrial production.
Disclosure of Invention
The invention discloses a treatment method of high-sulfur smelting slag, which aims to solve any one of the above and other potential problems in the prior art.
In order to solve the technical problems, the technical scheme of the invention is as follows: a method for treating high-sulfur smelting slag includes mixing raw materials with a solution, heating the mixture in a reaction kettle to a certain temperature, melting and dispersing elemental sulfur in the raw materials into the solution, cooling the mixture to 105-115 ℃ near the melting point of sulfur, carrying out aging reaction for a period of time, gradually separating out the elemental sulfur dispersed in the solution in the aging reaction process, condensing most of the elemental sulfur into large-particle coarse sulfur, and sulfurizing and leaching out a small part of residual small-particle elemental sulfur into the solution, so that more than 98% of elemental sulfur in the raw materials is separated and removed through one-step reaction, valuable metals are enriched in leached filter residues, and metal concentrate with extraction value is obtained.
The embodiment of the disclosure specifically discloses a treatment method of high-sulfur smelting slag, which specifically comprises the following steps:
s1) mixing high-sulfur smelting slag with the solution L, feeding the mixture into a reaction kettle, heating the mixture to a certain temperature, and stopping heating;
and S2) starting heat preservation when the temperature of the materials in the kettle in the S1) is reduced to 105-115 ℃, maintaining for a period of time, and then stopping heat preservation.
And S3) when the temperature of the materials in the kettle is reduced to room temperature in the step S2), taking out the materials in the kettle, firstly, screening the materials by a screen with 20-30 meshes, wherein oversize materials are crude sulfur, and undersize materials are subjected to solid-liquid separation to obtain filter residues and filtrate, wherein the filter residues are metal concentrate, and the filtrate is used as a vulcanizing agent and is sent to wastewater treatment.
According to the embodiment of the disclosure, the high-sulfur smelting slag in S1) is smelting slag with high elemental sulfur content, such as arsenic filter cake oxidation cleaning residue, zinc concentrate pressure leaching residue, nickel matte oxygen pressure leaching residue and the like.
According to the embodiment of the disclosure, the solution L in S1) is one or a combination of several of a sodium sulfite solution, a sodium bisulfite solution and a sodium metabisulfite solution, the sulfur ion concentration in the solution L is 1.5-4.5 mol/L, and the solution L and the high-sulfur smelting slag are mixed according to a volume mass ratio of 3-8.
According to the embodiment of the present disclosure, the certain temperature in S1) is 130 to 160 ℃.
According to the embodiment of the disclosure, the heat preservation maintaining time in the S2) is 0.5-5 h.
According to the embodiment of the disclosure, the method can separate and remove the elemental sulfur in the high-sulfur smelting slag, and the removal rate is more than 98%.
The invention has the beneficial effects that: by adopting the technical scheme, the method can separate over 98 percent of elemental sulfur in the high-sulfur smelting slag in one step, simultaneously enrich over 95 percent of valuable metals in the leached filter residue, obtain metal concentrate with refining value, and has the characteristics of short flow, good elemental sulfur separation effect, low cost, simplicity, easiness in implementation and the like.
Drawings
FIG. 1 is a flow chart of a high sulfur smelting slag treatment method of the present invention.
Detailed Description
For a further understanding of the contents of the present invention, reference will now be made in detail to the following examples.
As shown in fig. 1, the embodiment of the present disclosure specifically discloses a method for treating high-sulfur smelting slag, which includes converting most elemental sulfur in raw materials into crude sulfuric acid through a one-step reaction, sulfidizing and leaching a small amount of elemental sulfur into a solution, wherein the elemental sulfur removal rate is above 98%, so that valuable metals are enriched in leached filter residues, and metal concentrates with extraction value are obtained.
The disclosed embodiment specifically discloses a treatment method of high-sulfur smelting slag, which specifically comprises the following steps:
s1) mixing high-sulfur smelting slag with the solution L, feeding the mixture into a reaction kettle, heating the mixture to a certain temperature, and stopping heating;
and S2) starting heat preservation when the temperature of the materials in the kettle in the S1) is reduced to 105-115 ℃, maintaining for a period of time, and then stopping heat preservation.
And S3) when the temperature of the materials in the kettle is reduced to room temperature in the step S2), taking out the materials in the kettle, firstly, screening the materials by a screen with 20-30 meshes, wherein oversize materials are crude sulfur, and undersize materials are subjected to solid-liquid separation to obtain filter residues and filtrate, wherein the filter residues are metal concentrate, and the filtrate is used as a vulcanizing agent and is sent to wastewater treatment.
According to the embodiment of the disclosure, the high-sulfur smelting slag in S1 is smelting slag with high elemental sulfur content, such as arsenic filter cake oxidation cleaning residue, zinc concentrate pressure leaching residue, nickel matte oxygen pressure leaching residue and the like.
According to the embodiment of the disclosure, the solution L in S1 is one or a combination of several of a sodium sulfite solution, a sodium bisulfite solution and a sodium metabisulfite solution, the sulfur ion concentration in the solution L is 1.5-4.5 mol/L, and the solution L and the high-sulfur smelting slag are mixed according to a volume mass ratio of 3-8.
According to the embodiment of the present disclosure, the certain temperature in S1 is 130 to 160 ℃.
According to the embodiment of the disclosure, the heat preservation maintaining time in the S2 is 0.5-5 h.
According to the embodiment of the disclosure, the method can separate and remove the elementary sulfur in the high-sulfur smelting slag, and the removal rate is more than 98%.
According to the embodiment of the disclosure, the leached filter residue is valuable metal concentrate, valuable metals can be recycled without retreatment, and the leachate is subjected to wastewater treatment.
Example 1
Mixing nickel matte leaching residue (main elements including 66.98 wt% of elemental sulfur, 10.53 wt% of Ni10, 6.87 wt% of Pb, 5.41 wt% of Cu5, and 2.50 wt%) with Na2SO3Mixing the solution, controlling the liquid-solid ratio to be 3, feeding the mixed slurry into a reaction kettle, heating to 160 ℃, stopping heating, cooling to 110 ℃ in the kettle, keeping the temperature, reacting for 2 hours, stopping heating, cooling to room temperature in the kettle, taking out the material, sieving with a 20-mesh sieve, wherein oversize is crude sulfur, the content of elemental sulfur is 98.10%, and undersize is subjected to liquid-solid separation to obtain filter residue and filtrate, wherein the mass percent of main elements of the filter residue is: 4.07 percent of elemental sulfur, 35.53 percent of Ni35.53 percent of Pb 24.87 percent of Cu16.41 percent of As1.48 percent of the copper, 98.21 percent of elemental sulfur removal rate and 96.3 percent, 98.9 percent and 95.1 percent of recovery rate of nickel, lead and copper respectively.
Example 2
The zinc concentrate pressure leaching slag (the mass percentage of main elements is 74.19 percent of elemental sulfur, 5.09 percent of Zno, 2.12 percent of Cu2, 3.48 percent of Pb3, 1.78 percent of As1) and Na2S2O5Mixing the solution, controlling the liquid-solid ratio to be 6, feeding the mixed slurry into a reaction kettle, heating to 140 ℃, stopping heating, heating and preserving heat after the temperature in the kettle is reduced to 112 ℃, maintaining the reaction for 3 hours, stopping preserving heat, taking out the material after the temperature in the kettle is reduced to room temperature, sieving with a 30-mesh sieve, wherein oversize is crude sulfur, the content of elemental sulfur is 98.92%, and undersize is subjected to liquid-solid separation to obtain filter residue and filtrate, wherein the filter residue comprises the following main elements in percentage by mass: 6.07 percent of elemental sulfur, 42.53 percent of Zn16.38 percent of Cu16.84 percent of Pb and 0.58 percent of As0, 98.61 percent of elemental sulfur removal rate and 95.1 percent, 95.8 percent and 97.9 percent of recovery rate of zinc, copper and lead respectively.
Example 3
Oxidizing and cleaning arsenic filter cake (main elements of 89.21% of elemental sulfur, as2.17%, cu1.20% and Bi 2.06%) and Na2SO3And NaHSO3Mixing the raw materials according to the mass ratio of 1The method comprises the following steps of (1) mixing solutions, controlling the liquid-solid ratio to be 6, feeding the mixed slurry into a reaction kettle, heating to 150 ℃, stopping heating, heating and keeping the temperature after the temperature in the kettle is reduced to 108 ℃, keeping the reaction for 2.5 hours, stopping heat preservation, taking out materials after the temperature in the kettle is reduced to room temperature, sieving by a 30-mesh sieve, wherein oversize products are crude sulfur, the content of elemental sulfur is 99.12%, and undersize products are subjected to liquid-solid separation to obtain filter residues and filtrate, wherein the filter residues comprise the following main elements in percentage by mass: 8.65% of elemental sulfur, 0.37% of As0.37%, 15.35% of Cu and 29.80% of Bi29, 99.41% of elemental sulfur removal rate and 97.30% and 98.45% of recovery rates of copper and bismuth respectively.
The invention and its embodiments have been described above schematically, without limitation, and the figures shown in the drawings represent only one of the embodiments of the invention. The scope of the present invention is not limited thereto, and equivalents and modifications according to the technical solution of the present invention and the inventive concept thereof are intended to be included in the scope of the present invention.
Claims (4)
1. A high-sulfur smelting slag treatment method comprises the steps of uniformly mixing high-sulfur smelting slag and a solution L, heating, cooling to a precipitation temperature, keeping the temperature, stopping keeping the temperature, taking out materials in a kettle after the temperature is reduced to room temperature, passing through a screen, taking coarse sulfur as oversize products, carrying out solid-liquid separation on undersize products to obtain filter residues and filtrate, recycling valuable metals and treating the filtrate with wastewater, wherein the filter residues are valuable metal enrichments of bismuth, lead, copper, zinc and nickel, and the method is characterized by comprising the following steps:
s1) mixing the high-sulfur smelting slag with the solution L, feeding the mixture into a reaction kettle, heating the mixture to 130-160 ℃, stopping heating,
the solution L is one or a combination of sodium sulfite solution, sodium bisulfite solution and sodium metabisulfite solution;
mixing the solution L and the high-sulfur smelting slag according to the volume mass ratio of 3-8;
the elemental sulfur in the high-sulfur smelting slag is 66.98-89.71%;
s2) starting heat preservation when the temperature of the materials in the kettle in the S1) is reduced to 105-115 ℃, maintaining for a period of time, then stopping heat preservation,
s3) taking out the materials in the kettle after the temperature of the materials in the kettle in the S2) is reduced to room temperature,
the mixture is sieved by a 20-30 mesh sieve, oversize products are coarse sulfur, solid-liquid separation is carried out on undersize products, filter residues and filtrate are obtained, the filter residues are metal concentrate, and the filtrate is used as a vulcanizing agent and is sent to wastewater treatment.
2. The method according to claim 1, characterized in that the high-sulfur smelting slag in S1) is arsenic filter cake oxidation cleaning residue, zinc concentrate pressure leaching residue or nickel matte oxygen pressure acid leaching residue produced in smelting with high elemental sulfur content.
3. The method as claimed in claim 1, wherein the heat-preserving maintaining time in S2) is 0.5 to 5 hours.
4. The method according to claim 1, characterized in that the method is capable of separating and removing the elemental sulfur in the high-sulfur smelting slag with a removal rate of more than 98%.
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| CN114427035B (en) * | 2022-01-27 | 2023-07-28 | 江苏北矿金属循环利用科技有限公司 | Synergistic extraction and harmless treatment method for valuable components of zinc smelting high-sulfur slag and application thereof |
| CN114715854B (en) * | 2022-03-31 | 2023-05-23 | 常熟理工学院 | Method for recycling elemental sulfur from high-sulfur slag by zinc-oxygen pressure leaching |
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| RU103799U1 (en) * | 2010-05-17 | 2011-04-27 | Государственное образовательное учреждение высшего профессионального образования "Уральский государственный университет - УПИ имени первого Президента России Б.Н. Ельцина" | REEXTRACTOR FOR EXTRACTION OF ELEMENT SULFUR |
| CN110387464A (en) * | 2019-07-19 | 2019-10-29 | 江西铜业技术研究院有限公司 | A method of it will be enriched in sulphur arsenic in the complex materials of elemental sulfur and removes |
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| CN101648700B (en) * | 2009-09-09 | 2011-01-05 | 中南大学 | Method for separating and recycling sulfur, iron and selenium from selenic acid mud |
| CN101734626A (en) * | 2009-11-23 | 2010-06-16 | 长沙有色冶金设计研究院 | Method for recovering sulfur element from zinc sulphide concentrate direct leaching residues |
| CN101838088B (en) * | 2010-01-28 | 2012-04-18 | 中国恩菲工程技术有限公司 | Anode mud treatment method of preparing metallic nickel by copper sulphide |
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| CN109082528B (en) * | 2018-07-27 | 2020-01-31 | 郴州雄风环保科技有限公司 | Wet extraction process for high-sulfur gold, silver and lead materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU103799U1 (en) * | 2010-05-17 | 2011-04-27 | Государственное образовательное учреждение высшего профессионального образования "Уральский государственный университет - УПИ имени первого Президента России Б.Н. Ельцина" | REEXTRACTOR FOR EXTRACTION OF ELEMENT SULFUR |
| CN110387464A (en) * | 2019-07-19 | 2019-10-29 | 江西铜业技术研究院有限公司 | A method of it will be enriched in sulphur arsenic in the complex materials of elemental sulfur and removes |
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