A method for producing sulfur from sulfur-containing materials

Abstract

This application relates to the field of hydrometallurgical technology, specifically to a method for producing sulfur from sulfur-containing materials. The preparation method includes the following steps: (1) oxygen pressure treatment, (2) stepped cooling, (3) sieving, and (4) washing. This application uses sulfur-containing materials as raw materials, performs two stepped cooling processes after oxygen pressure treatment, and then sieves the slurry. The slurry undersized is returned to the oxygen pressure treatment process, and the sulfur particles are washed to obtain sulfur of different particle sizes. This application maximizes the utilization value of sulfur in sulfur-containing materials. No waste gas, waste liquid, or waste residue is generated during the preparation process. The product has high purity, short production cycle, and high product yield, thus improving the utilization value of sulfur in sulfur-containing materials.

Description

Technical Field

[0001] This application relates to the field of hydrometallurgical technology, specifically to a method for producing sulfur from sulfur-containing materials. Background Technology

[0002] Sulfur, as an indispensable basic non-metallic raw material, has extremely wide applications, covering core chemical products (such as industrial sulfuric acid, rubber vulcanizing agents, and gunpowder), pesticide manufacturing, daily chemical products, agricultural bactericides and amendments, and food processing bleaching and preservation that requires strict control. Currently, sulfur acquisition mainly relies on natural sulfur ore mining or industrial synthesis, with the specific choice depending on resource endowment (sulfur ore, associated gas from petroleum, smelting flue gas, etc.), cost-effectiveness, and target purity requirements. For pyrite, a typical sulfur-bearing ore with abundant reserves but complex processing, the mainstream industrial process is as follows: first, the sulfur element in the ore is converted into gaseous sulfur dioxide through high-temperature oxidation calcination or specific reduction roasting; then, the flue gas containing sulfur dioxide is purified and undergoes multi-stage conversion using the Claus process under the action of a catalyst, ultimately condensing and recovering the sulfur element in the form of liquid sulfur. However, this process suffers from a series of significant drawbacks: It is lengthy and complex (involving multiple stages such as high-temperature roasting, flue gas purification, multi-stage catalytic conversion, and condensation recovery, resulting in large equipment investments and difficult management and maintenance), leading to a low overall sulfur recovery rate and resource waste; it poses significant environmental and safety hazards (generating and requiring the treatment of highly toxic gases such as sulfur dioxide and hydrogen sulfide, operating in harsh environments, and generating heavy metal-containing waste residue and acidic waste gas / wastewater, resulting in high end-of-pipe treatment costs and enormous energy consumption); it has high overall production costs (combined with high investment, high energy consumption, high environmental protection investment, and low recovery rate); and it has poor raw material adaptability (sensitive to ore grade, harmful impurities such as arsenic / mercury / lead content, and physical properties, further deteriorating efficiency and profitability when processing low-quality or complex ores). These factors collectively constrain the resource utilization efficiency and sustainable development of this process.

[0003] While patent literature proposes a new process for directly recovering sulfur from pyrite (involving the conversion of S → hydrogen sulfide → sulfur and the use of ferric sulfate reagent) to address the shortcomings of traditional methods, it still faces challenges such as complex processes, difficult control, high costs, low sulfur utilization value, and unclear economic benefits. Currently, sulfur mainly comes from petrochemicals or as a by-product of smelting. Other methods for extracting sulfur from sulfur-containing materials also have their drawbacks: the oxidation process for sulfuric acid is complex, has a long process flow, and high transportation and storage costs, making it unsuitable for areas without sulfuric acid sales channels; pyrometallurgical roasting for sulfur production requires high-concentration SO2 flue gas, which needs to be converted into gypsum for recovery at low concentrations, resulting in high costs and low recovery rates; while directly converting sulfur into sulfur avoids the sulfuric acid storage and transportation problems, typical processes (such as pressurized enrichment → flotation concentrate → hot filtration for sulfur extraction) have long processes and low efficiency (total recovery rate of only about 50%). The pressurization process requires high precision control and is difficult to operate. Furthermore, the generated sulfur particles are small, poorly dispersed in the slag, and severely encapsulated, leading to difficulties in recovery and easy pipe blockage problems, thus limiting both environmental friendliness and economic viability. In addition, existing technologies require hot filtration of the leaching residue to obtain sulfur during sulfur production. However, the hot filtration equipment used must be resistant to high temperatures and corrosion, and is not easy to filter. The filtration device is prone to damage, has high maintenance costs, is complex to operate, has a long process, and operates at high temperatures with a certain degree of corrosiveness.

[0004] In summary, existing technologies suffer from drawbacks such as complex processes, low production efficiency, high energy consumption and costs, environmental pollution, poor raw material adaptability, low sulfur recovery rate, and high operational difficulty. Therefore, there is an urgent need for a solution that can simplify processes, improve efficiency, reduce energy consumption and costs, enhance environmental friendliness and applicability, and improve sulfur recovery rate. Summary of the Invention

[0005] Therefore, the technical problem to be solved by this application is to overcome the above-mentioned defects in the prior art, thereby providing a method for producing sulfur from sulfur-containing materials.

[0006] Therefore, this application achieves the above objectives through the following technical solution:

[0007] This application provides a method for producing sulfur from sulfur-containing materials, the process flow of which is shown below. Figure 1 It includes the following steps:

[0008] S1, sulfur-containing materials are mixed with acid solution to form a slurry, which is then subjected to oxygen pressure treatment to obtain slurry A. The oxygen pressure treatment is carried out at a temperature of 130~165℃ for a time of 0.75~4.0h and a pressure of 0.1~0.8MPa.

[0009] S2, the slurry A is cooled once, with the final temperature controlled at 120~145℃ and the holding time being 30~60min. Then, it is cooled a second time, with the final temperature controlled at 80~105℃, to obtain slurry B.

[0010] S3, slurry B is screened to obtain slurry C and sulfur particles;

[0011] S4, the sulfur particles are washed to obtain a sulfur product.

[0012] As an example, the temperature of the oxygen pressure treatment can be 130℃, 132℃, 134℃, 138℃, 136℃, 140℃, 144℃, 146℃, 148℃, 150℃, 152℃, 154℃, 156℃, 158℃, 160℃, 162℃, 165℃, or within any range of the above values; the time of the oxygen pressure treatment can be 0.75h, 0.80h, 0.85h, 0.9h, 0.95h, 1h, 1.25h, 1.5h, 1.75h, 2h, 2.25h, 2.5h, 2.75h, 3h, 3.25h, 3.5h, 3.75h, 4h, or within any range of the above values. The pressure of the oxygen pressure treatment can be 0.1 MPa, 0.15 MPa, 0.2 MPa, 0.25 MPa, 0.3 MPa, 0.35 MPa, 0.4 MPa, 0.45 MPa, 0.5 MPa, 0.55 MPa, 0.6 MPa, 0.65 MPa, 0.7 MPa, 0.75 MPa, 0.8 MPa, or within any range of the above values.

[0013] As an example, the endpoint temperature of the first cooling step can be 120℃, 122℃, 124℃, 126℃, 128℃, 130℃, 132℃, 134℃, 136℃, 138℃, 140℃, 142℃, 145℃, or within any range of the above values; the holding time after the first cooling step can be 30min, 35min, 40min, 45min, 50min, 55min, 60min, or within any range of the above values; the cooling time of the first cooling step can be 0.2h, 0.4h, 0.6h, 0.8h, 1.0h, 1.2h, 1.4h, 1.6h, 1.8h, 2.0h, or within any range of the above values.

[0014] As an example, the endpoint temperature of the secondary cooling can be 80℃, 82℃, 84℃, 86℃, 88℃, 90℃, 92℃, 94℃, 96℃, 98℃, 100℃, 102℃, 105℃, or within any range of the above values; the cooling time of the secondary cooling can be 0.2h, 0.4h, 0.6h, 0.8h, 1.0h, or within any range of the above values.

[0015] It should be noted that the segmented cooling is based on the phase diagram of sulfur at different temperatures. The first cooling ensures the nucleation of sulfur and that the sulfur form formed at that temperature is easy to separate from the slurry. The second cooling, on the basis of sulfur nucleation, allows the sulfur crystal nuclei to continue to grow, which is beneficial to the sulfur screening in subsequent processes.

[0016] In some alternative embodiments, the sulfur-containing material includes at least one of zinc sulfide ore, nickel sulfide ore, pyrite, or sulfur-containing anode mud.

[0017] In some alternative embodiments, the mass ratio of the acid solution to the sulfur-containing material is 3 to 10:1; as an example, the mass ratio of the acid solution to the sulfur-containing material can be 3:1, 3.5:1, 4:1, 4.5:1, 5:1, 5.5:1, 6:1, 6.5:1, 7:1, 7.5:1, 8:1, 8.5:1, 9:1, 9.5:1, 10:1, or within any range of the above values.

[0018] In some alternative embodiments, the mass ratio of acid to sulfur-containing material in the acid solution is 0.1 to 0.3:1; as an example, the mass ratio of acid to sulfur-containing material in the acid solution can be 0.1:1, 0.12:1, 0.14:1, 0.16:1, 0.18:1, 0.20:1, 0.22:1, 0.24:1, 0.26:1, 0.28:1, 0.3:1, or within any range of the above values.

[0019] Optionally, oxygen-containing gas is introduced during the oxygen pressure treatment step;

[0020] Optionally, the gas introduced during the oxygen pressure treatment is at least one of oxygen, air, and oxygen-enriched air;

[0021] Optionally, the screening method is mechanical screening;

[0022] As an example, the screening temperature can be 40℃, 42℃, 44℃, 46℃, 48℃, 40℃, 52℃, 54℃, 56℃, 58℃, 60℃, 62℃, 64℃, 66℃, 68℃, 70℃, or within any range of the above values; the screen mesh size can be 0.2mm, 0.5mm, 1mm, 1.5mm, 2mm, 2.5mm, 3mm, 3.5mm, 4mm, 4.5mm, 5mm, or within any range of the above values.

[0023] Optionally, the slurry C is reused in the mixing and conditioning step of step S1 to replace part of the acid solution;

[0024] Optionally, the acid in the acid solution includes sulfuric acid.

[0025] In some alternative embodiments, the ratio of sulfur particles to water used in the washing process is 5 to 20 g: 1 mL; as an example, the ratio of sulfur particles to water used in the washing process is 5 g: 1 mL, 8 g: 1 mL, 10 g: 1 mL, 12 g: 1 mL, 14 g: 1 mL, 16 g: 1 mL, 18 g: 1 mL, 20: 1 g / mL, or within any range of the above values;

[0026] In some alternative embodiments, the washing time is 10 to 30 minutes; as an example, the washing time can be 10 minutes, 12 minutes, 14 minutes, 16 minutes, 18 minutes, 20 minutes, 22 minutes, 24 minutes, 26 minutes, 28 minutes, 30 minutes, or within any of the above values.

[0027] Optionally, the sulfur product content is S≥95wt.%, and the average particle size of the sulfur product is 0.5~5 mm.

[0028] The technical solution of this application has the following advantages:

[0029] 1. The method for producing sulfur from sulfur-containing materials provided in this application, which involves oxygen pressure treatment followed by staged cooling, maximizes the recovery of sulfur resources. The resulting sulfur is easier to store and transport, improves the overall mineral yield, and significantly enhances the economic benefits of sulfide materials. Furthermore, by controlling the oxygen pressure and cooling process, the size of sulfur particles can be precisely controlled, improving dispersibility and solving the problem of sulfur particle encapsulation, thereby increasing the sulfur recovery rate to over 85%. This optimizes the utilization of sulfur-containing materials and yields high-quality sulfur. Simultaneously, the liquid and slag generated in the process are effectively recovered, with no waste gas, waste liquid, or waste slag produced. This reduces environmental pollution and creates economic benefits. The entire recovery process is short, convenient, and controllable, improving sulfur recovery efficiency. It solves the problems of insufficient processing space, low smelting production capacity, and high energy consumption caused by excessive waste slag in smelting enterprises. It also avoids environmental pollution caused by zinc smelting, demonstrating significant social benefits and important practical significance for the comprehensive recovery of sulfur-containing materials. Specifically, this method mainly uses the phase transformation diagram of sulfur (S) under different temperature and pressure conditions to set the temperature and pressure of the oxygen pressure treatment stage. Part of the S in the material is converted into elemental sulfur, and part into sulfate ions. This process, while maintaining self-heating, converts sulfur into sulfur. The conversion to sulfate ions is exothermic, providing the energy required for the oxygen pressure treatment stage. This process is simple, has a short flow, and low production cost. Then, in the stepped cooling stage, by adjusting the different cooling endpoint temperatures and holding times, the nucleation and growth of sulfur particles are controlled, ultimately yielding a high-grade sulfur product. The first cooling stage in the stepped cooling process controls sulfur nucleation, and after holding for a certain time, the second cooling stage controls sulfur crystal growth, ultimately obtaining easily separable sulfur particles. The sulfur product can then be obtained through mechanical sieving. This method is simple to operate and low in cost. Unlike existing technologies that produce sulfur in a molten slurry state, requiring hot filtration and high-temperature, corrosion-resistant filtration equipment, this method offers a significant advantage. The entire recycling process is short, easy to operate and controllable, improves sulfur recovery efficiency, solves the problems of insufficient processing space, low smelting production capacity, and high energy consumption of waste residue in smelting enterprises, and can also avoid environmental pollution caused by zinc smelting. It has good social benefits and is of great practical significance for the comprehensive recycling of sulfur-containing materials.

[0030] 2. The method for producing sulfur from sulfur-containing materials provided in this application can control the size of the resulting sulfur particles by adjusting the cooling time.

[0031] 3. The method for producing sulfur from sulfur-containing materials provided in this application uses a sieve for physical separation, which is carried out at a low temperature and is visible to the naked eye. It is simple to operate and has a low cost.

[0032] 4. The method for producing sulfur from sulfur-containing materials provided in this application can save water resources and improve washing efficiency as much as possible while ensuring that sulfur particles are washed clean, by setting the washing parameters. Attached Figure Description

[0033] To more clearly illustrate the technical solutions in the specific embodiments of this application or the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0034] Figure 1 This is a process flow diagram of the method for producing sulfur from sulfur-containing materials provided in this application. Detailed Implementation

[0035] The following embodiments are provided to better understand this application and are not limited to the preferred embodiments described herein. They do not constitute a limitation on the content and scope of protection of this application. Any product that is the same as or similar to this application, derived by anyone under the guidance of this application or by combining features of this application with other prior art, falls within the scope of protection of this application.

[0036] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the application; the terms “comprising” and “having” and any variations thereof in the text of this application are intended to cover non-exclusive inclusion.

[0037] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.

[0038] The "range" disclosed in this application is defined by a lower limit and an upper limit. A given range is defined by selecting a lower limit and an upper limit, which define the boundaries of the specific range. Ranges defined in this way can include or exclude endpoints and can be arbitrarily combined; that is, any lower limit can be combined with any upper limit to form a range. In this application, unless otherwise stated, the numerical range "ab" represents a shortened representation of any combination of real numbers from a to b, where a and b are real numbers. For example, the numerical range "0-5" indicates that all real numbers between "0-5" have been listed herein, and "0-5" is merely a shortened representation of these numerical combinations. Furthermore, when a parameter is described as an integer ≥ 2, it is equivalent to disclosing that the parameter can be, for example, integers 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0039] In the description of the embodiments of this application, the term "and / or" is merely a description of the relationship between related objects, indicating that there can be three relationships. For example, A and / or B can represent three situations: A exists alone, A and B exist simultaneously, and B exists alone.

[0040] In the description of the embodiments of this application, the term "at least one" refers to one or more (including two).

[0041] Unless otherwise specified, all steps in this application may be performed sequentially or randomly, preferably sequentially. For example, the method includes steps (a) and (b), indicating that the method may include steps (a) and (b) performed sequentially, or it may include steps (b) and (a) performed sequentially. For example, the mention that the method may also include step (c) indicates that step (c) may be added to the method in any order. For example, the method may include steps (a), (b), and (c), or it may include steps (a), (c), and (b), or it may include steps (c), (a), and (b), etc.

[0042] For experiments not specifically described in the examples, the procedures or conditions should be followed according to the conventional experimental procedures described in the literature in this field. Reagents or instruments whose manufacturers are not specified are all commercially available conventional reagent products.

[0043] The present application will now be described with reference to specific embodiments. It should be noted that these embodiments are merely descriptive and do not limit the present application in any way.

[0044] Example 1

[0045] This embodiment provides a method for producing sulfur from sulfur-containing materials, and its process flow diagram is as follows: Figure 1 As shown, the specific steps and operating parameters are as follows:

[0046] Zinc sulfide concentrate (S 29wt.%, Zn 44wt.%, Fe 10wt.%, balance C, H, O, etc.) and acid solution (undersize slurry) were mixed at a liquid-to-solid mass ratio of 5:1 and an acid-to-ore mass ratio of 0.2:1. Oxygen was introduced into the mixture, and oxygen pressure treatment was carried out at a reaction temperature of 150℃ and a pressure of 0.6MPa for 2.0h.

[0047] After the reaction is completed, the slurry is cooled once, with the final temperature controlled at 135℃ for 1.0 h and the holding time at 45 min. Then the slurry is cooled a second time, with the final temperature controlled at 105℃ for 0.2 h.

[0048] After the cascade cooling is completed, the slurry is sieved to obtain sulfur particles and undersize slurry. The undersize slurry is returned to the oxygen pressure treatment process. The sulfur particles are washed with water at a ratio of sulfur particles:water = 20 g / mL for 30 min to obtain sulfur with an average particle size of 0.8 mm, an S content of 96.6 wt.%, and a sulfur recovery rate of 92%.

[0049] Example 2

[0050] This embodiment provides a method for producing sulfur from sulfur-containing materials, and its process flow diagram is as follows: Figure 1 As shown, the specific steps and operating parameters are as follows:

[0051] Nickel sulfide concentrate (S 31wt.%, Ni 14wt.%, Fe 31wt.%, balance C, H, O, etc.) and acid solution (undersize slurry) were mixed at a liquid-to-solid mass ratio of 3:1. Sulfuric acid and acid-to-ore mass ratio of 0.1:1 were added, and air was introduced into the mixture. Oxygen pressure treatment was carried out at a reaction temperature of 165℃ and a partial pressure of 0.1MPa for 4.0 h.

[0052] After the reaction is completed, the slurry is cooled once, with the final temperature controlled at 145℃ for 0.2h and the holding time at 40min. Then the slurry is cooled a second time, with the final temperature controlled at 80℃ for 1.0h.

[0053] After the cascade cooling is completed, the slurry is sieved to obtain sulfur particles and undersize slurry. The undersize slurry is returned to the oxygen pressure treatment process. The sulfur particles are washed with water at a ratio of 5 g / mL for 10 min to obtain sulfur with an average particle size of 5 mm, an S content of 95.0 wt.%, and a sulfur recovery rate of 90%.

[0054] Example 3

[0055] This embodiment provides a method for producing sulfur from sulfur-containing materials, and its process flow diagram is as follows: Figure 1As shown, the specific steps and operating parameters are as follows:

[0056] Pyrite (S 38wt.%, Fe 34wt.%, balance C, H, O, etc.) and acid solution (undersize slurry) were mixed at a liquid-to-solid mass ratio of 10:1. Sulfuric acid and acid-to-ore mass ratio of 0.3:1 were added. A mixture of air and oxygen was introduced into the mixture at a ratio of 5:5. Oxygen pressure treatment was carried out at a reaction temperature of 130℃ and a pressure of 0.8MPa for a reaction time of 0.75h.

[0057] After the reaction is completed, the slurry is cooled once, with the final temperature controlled at 120℃ for 2.0 h and the holding time at 50 min. Then the slurry is cooled a second time, with the final temperature controlled at 90℃ for 0.5 h.

[0058] After the cascade cooling is completed, the slurry is sieved to obtain sulfur particles and undersize slurry. The undersize slurry is returned to the oxygen pressure treatment process. The sulfur particles are washed with water at a ratio of 15 g / mL for 15 min to obtain sulfur with an average particle size of 2.0 mm, an S content of 96.1 wt.%, and a sulfur recovery rate of 88%.

[0059] Example 4

[0060] This embodiment provides a method for producing sulfur from sulfur-containing materials, and its process flow diagram is as follows: Figure 1 As shown, the specific steps and operating parameters are as follows:

[0061] Sulfur-containing anode mud (S 12wt.%, Fe 9wt.%, Mn 30wt.%, Zn 7wt.%, Pb 5wt.%, balance C, H, O, etc.) and acid solution (under-sieved slurry) were mixed at a liquid-to-solid mass ratio of 7:1. Sulfuric acid and acid-to-ore mass ratio of 0.15:1 were added, and oxygen was introduced into the mixture. The mixture was subjected to oxygen pressure treatment at a reaction temperature of 140℃ and a pressure of 0.4MPa for 1.5 hours.

[0062] After the reaction is completed, the slurry is cooled once, with the final temperature controlled at 130℃ for 0.5 hours and the holding time at 35 minutes. Then the slurry is cooled a second time, with the final temperature controlled at 100℃ for 0.4 hours.

[0063] After the cascade cooling is completed, the slurry is sieved to obtain sulfur particles and undersize slurry. The undersize slurry is returned to the oxygen pressure treatment process. The sulfur particles are washed with water at a ratio of 10 g / mL for 20 minutes to obtain sulfur with an average particle size of 1.0 mm, an S content of 97.2 wt.%, and a sulfur recovery rate of 89%.

[0064] Example 5

[0065] This embodiment provides a method for producing sulfur from sulfur-containing materials, and its process flow diagram is as follows: Figure 1 As shown, the specific steps and operating parameters are as follows:

[0066] Zinc sulfide concentrate (S 29wt.%, Zn 44wt.%, Fe 10wt.%, balance C, H, O, etc.) and acid solution (undersize slurry) were mixed at a liquid-to-solid mass ratio of 3:1 and an acid-to-ore mass ratio of 0.3:1. A mixture of air and oxygen was introduced into the mixture at a ratio of 8:2. The mixture was subjected to oxygen pressure treatment at a reaction temperature of 130℃ and a pressure of 0.1MPa for 4 hours.

[0067] After the reaction is complete, the slurry is cooled once, with the final temperature controlled at 145℃ for 0.2 hours and the holding time at 30 minutes. Then the slurry is cooled a second time, with the final temperature controlled at 105℃ for 0.2 hours.

[0068] After the cascade cooling is completed, the slurry is sieved to obtain sulfur particles and undersize slurry. The undersize slurry is returned to the oxygen pressure treatment process. The sulfur particles are washed with water at a ratio of 20 g / mL for 10 min to obtain sulfur with an average particle size of 0.5 mm, an S content of 95 wt.%, and a sulfur recovery rate of 85%.

[0069] Example 6

[0070] This embodiment provides a method for producing sulfur from sulfur-containing materials, and its process flow diagram is as follows: Figure 1 As shown, the specific steps and operating parameters are as follows:

[0071] Nickel sulfide concentrate (S 31wt.%, Ni 14wt.%, Fe 31wt.%, balance C, H, O, etc.) and acid solution (undersize slurry) were mixed at a liquid-to-solid mass ratio of 10:1 and an acid-to-ore mass ratio of 0.1:1. Oxygen was introduced into the mixture, and oxygen pressure treatment was carried out at a reaction temperature of 165℃ and a pressure of 0.8MPa for 0.75h.

[0072] After the reaction is completed, the slurry is cooled once, with the final temperature controlled at 120℃ for 2 hours and the holding time at 60 minutes. Then the slurry is cooled a second time, with the final temperature controlled at 80℃ for 1 hour.

[0073] After the cascade cooling is completed, the slurry is sieved to obtain sulfur particles and undersize slurry. The undersize slurry is returned to the oxygen pressure treatment process. The sulfur particles are washed with water at a ratio of 5 g / mL for 30 minutes to obtain sulfur with an average particle size of 4 mm, an S content of 95 wt.%, and a sulfur recovery rate of 87%.

[0074] Comparative Example 1

[0075] The main difference between Comparative Example 1 and Example 5 is that the cascade cooling parameters are not within the given numerical range. The initial cooling endpoint temperature is set to 110°C, the cooling time is 0.2 h, the holding time is 15 min, and the secondary cooling endpoint temperature is set to 70°C, with a cooling time of 0.2 h. The resulting sulfur has an average particle size of 0.1 mm, an S content of 64 wt.%, and a sulfur recovery rate of 60%.

[0076] Comparative Example 2

[0077] The main difference between Comparative Example 2 and Example 6 is that the cascade cooling parameters are not within the given numerical range. The initial cooling endpoint temperature is set to 160°C, the cooling time is 2 hours, the holding time is 5 minutes, and the secondary cooling endpoint temperature is set to 115°C with a cooling time of 1 hour. The resulting sulfur has an average particle size of 0.05 mm, an S content of 53 wt.%, and a sulfur recovery rate of 45%.

[0078] Comparative Example 3

[0079] The main difference between Comparative Example 3 and Example 6 is that the oxygen pressure treatment parameters are not within the given numerical range, the temperature is set at 180°C, the time is 0.5h, the pressure is 1MPa, and no sulfur is produced.

[0080] Comparative Example 4

[0081] The main difference between Comparative Example 4 and Example 5 is that the oxygen pressure treatment parameters are not within the given numerical range, the temperature is set at 100°C, the time is 5 hours, the pressure is 0.05 MPa, and no sulfur is produced.

[0082] Comparative Example 5

[0083] The main difference between Comparative Example 5 and Example 6 is that the sulfur was directly cooled to 80°C for 3 hours. The resulting sulfur had an average particle size of 0.01 mm, an S content of 46 wt.%, and a sulfur recovery rate of 39%.

[0084] The above comparison shows that in the embodiments of this application, the sulfur produced by using reasonable stepped cooling and oxygen pressure treatment parameters has suitable particle size and high purity. In contrast, in the comparative examples, when the stepped cooling or oxygen pressure treatment parameters deviate from the reasonable range, not only does the sulfur particle size become abnormally fine, but the purity also drops significantly, and in some cases, sulfur cannot be produced at all. This fully demonstrates that the specific parameter settings of this application play a crucial role in ensuring the quality and production stability of the sulfur product, highlighting its technical advantages.

[0085] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A method for producing sulfur from sulfur-containing materials, characterized in that, Includes the following steps: S1, sulfur-containing materials are mixed with acid solution to form a slurry, which is then subjected to oxygen pressure treatment to obtain slurry A. The oxygen pressure treatment is carried out at a temperature of 130~165℃ for a time of 0.75~4.0h and a pressure of 0.1~0.8MPa. S2, the slurry A is cooled once, with the final temperature controlled at 120~145℃ and the holding time being 30~60min. Then, it is cooled a second time, with the final temperature controlled at 80~105℃, to obtain slurry B. S3, slurry B is screened to obtain slurry C and sulfur particles; the screening method is mechanical screening; the screening temperature is 40~70℃; S4, the sulfur particles are washed to obtain a sulfur product.

2. The method for producing sulfur from sulfur-containing materials according to claim 1, characterized in that, In S2, the cooling time for the first cooling cycle is 0.2~2.0h; And / or, the cooling time for the secondary cooling is 0.2~1.0h.

3. The method for producing sulfur from sulfur-containing materials according to claim 1, characterized in that, In S1, the sulfur-containing material includes at least one of zinc sulfide ore, nickel sulfide ore, pyrite, or sulfur-containing anode mud.

4. The method for producing sulfur from sulfur-containing materials according to claim 1, characterized in that, In S1, the mass ratio of the acid solution to the sulfur-containing material is 3~10:

1.

5. The method for producing sulfur from sulfur-containing materials according to claim 1, characterized in that, In S1, the mass ratio of acid in the acid solution to sulfur-containing material is 0.1~0.3:

1.

6. The method for producing sulfur from sulfur-containing materials according to claim 1, characterized in that, In S1, oxygen-containing gas is introduced during the oxygen pressure treatment step.

7. The method for producing sulfur from sulfur-containing materials according to claim 1, characterized in that, In S3, the sieve mesh size is 0.2~5mm.

8. The method for producing sulfur from sulfur-containing materials according to claim 1, characterized in that, In step S3, the resulting slurry C is reused in the mixing and conditioning step in step S1. And / or, in S1, the acid in the acid solution includes sulfuric acid.

9. The method for producing sulfur from sulfur-containing materials according to claim 1, characterized in that, In S4, the mass ratio of sulfur particles to water in the washing process is 5~20g:1mL; And / or, the washing time is 10~30 minutes.

10. The method for producing sulfur from sulfur-containing materials according to any one of claims 1-9, characterized in that, In S4, the sulfur product contains S≥95wt.%, and the average particle size of the sulfur product is 0.5~5 mm.

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