A desulfurization process and device for chlorine leaching residue

By using a medium-frequency induction heating and stirring transmission mechanism with metal balls as the medium, the chlorine leaching residue is crushed and heated in stages, solving the problems of low desulfurization rate and uneven heating of the equipment, and achieving efficient and stable sulfur recovery and enrichment of valuable metals.

CN117139342BActive Publication Date: 2026-01-06SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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Patent Information

Application Number
CN202311094224.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-08-28
Publication Date
2026-01-06
Estimated Expiration
2043-08-28

AI Technical Summary

Technical Problem

Existing chlorine leaching residue treatment processes suffer from problems such as low desulfurization rates, uneven equipment heating, and chlorine leaching residue accumulation and caking, making it difficult to effectively and quickly desulfurize.

Method used

Using metal balls as the magnetic induction medium, medium-frequency induction heating and stirring are used to fully mix the metal balls with the chlorine leaching residue, achieving crushing and heat transfer. Metal balls of different diameters are used in stages to crush and sublimate the chlorine leaching residue for desulfurization. Combined with a protective atmosphere and a material stirring and conveying mechanism, effective mixing and heat transfer are ensured.

Benefits of technology

It improved the desulfurization rate and sulfur recovery rate of chlorine leaching residue, solved the problems of residue accumulation and agglomeration, achieved an efficient and stable desulfurization process, and reduced the difficulty of operation and energy consumption.

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Abstract

The application discloses a kind of chloridizing residue desulfurization process and chloridizing residue desulfurization device, belong to chemical technology field.The chloridizing residue desulfurization process of the present application uses metal ball as magnetic induction medium, utilizes the metal ball of intermediate frequency induction heating, fully mixes it with chloridizing residue under stirring, and realizes the crushing and heat transfer of chloridizing residue by its collision and friction with chloridizing residue, makes the granulation of agglomerated chloridizing residue and the sulfur in chloridizing residue fully sublimate by heating;The crushing and heat transfer of metal ball to chloridizing residue are divided into at least two stages, first, using large-diameter metal ball to crush and heat chloridizing residue, make the granulation of agglomerated chloridizing residue, and after the sulfur in it sublimate by heating, continue to use small-diameter metal ball to crush and heat chloridizing residue, make it fully granulate, so as to realize full desulfurization.The application also discloses a chloridizing residue desulfurization device using the above process.The application improves the desulfurization rate and desulfurization efficiency;Overall process is automatic process, simple operation, continuous and efficient production is convenient.
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Description

Technical Field

[0001] This invention belongs to the field of chemical technology, specifically to the field of sulfur recovery technology, and more particularly to a desulfurization process and device for chlorine leaching residue, and a vaporization sublimation desulfurization process and device for chlorine leaching residue. Background Technology

[0002] Chlorine leaching residue is a material produced in the nickel electrolysis process. It contains a high level of elemental sulfur and a certain amount of precious metals, making it highly valuable for recycling. However, chlorine leaching residue is highly corrosive, viscous, and has a high moisture content, making it difficult to transport and process. Current technologies for treating chlorine leaching residue commonly employ methods such as hot filtration, flotation, solvent extraction, vacuum distillation, pressure leaching, and roasting. However, these existing processes suffer from processing difficulties and low desulfurization rates.

[0003] Furthermore, current domestic desulfurization equipment for chlorine leaching residue suffers from long process flows, high costs, uneven heating, and problems such as residue accumulation, caking, and agglomeration, hindering effective and rapid desulfurization. Therefore, providing a chlorine leaching residue desulfurization process and device to address the poor desulfurization and separation effects of existing technologies and improve the desulfurization rate has become a pressing issue for those skilled in the art. Summary of the Invention

[0004] One of the objectives of this invention is to provide a desulfurization process for chlorine leaching residue, which solves the problem of uneven heating and agglomeration of chlorine leaching residue during the heating process, thereby improving the desulfurization rate and achieving the goal of increasing sulfur recovery rate and enriching valuable metals.

[0005] The second objective of this invention is to provide a desulfurization device for chlorine leaching residue, used in the aforementioned desulfurization process for chlorine leaching residue.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0007] The present invention discloses a desulfurization process for chlorine leaching residue, which uses metal balls as a magnetic induction medium and utilizes medium-frequency induction heating of the metal balls. Under the stirring action, the metal balls and chlorine leaching residue are fully mixed. Through the collision and friction between the metal balls and the chlorine leaching residue, the chlorine leaching residue is broken up and heat is transferred, so that the agglomerated chlorine leaching residue is fully degranulated and the sulfur in the chlorine leaching residue is fully sublimated by heat.

[0008] The crushing and heat transfer of chlorine leaching residue by metal balls is divided into at least two stages. First, large-diameter metal balls are used to crush and heat the chlorine leaching residue, causing the clumps of chlorine leaching residue to break up into smaller particles. After the sulfur in the chlorine leaching residue sublimates upon heating, small-diameter metal balls are used to continue crushing and heating the chlorine leaching residue, causing it to break up into smaller particles, thereby achieving full desulfurization.

[0009] In some embodiments of the present invention, the crushing and heat transfer of the chlorine leaching residue by the metal balls includes three stages, with the diameter of the metal balls used in each stage gradually decreasing.

[0010] The diameter of the metal spheres in the first stage is 15-20 mm, the diameter of the metal spheres in the second stage is 10-15 mm, and the diameter of the metal spheres in the third stage is 5-10 mm.

[0011] Preferably, the particle size of the chlorine leaching residue after the first stage of crushing and heat transfer is less than 12 mm;

[0012] Preferably, the particle size of the chlorine leaching residue after the second stage of crushing and heat transfer is less than 8 mm;

[0013] Preferably, the particle size of the chlorine leaching residue after the third stage of crushing and heat transfer is less than 2 mm;

[0014] Preferably, the volume ratio of metal balls to chlorine leaching residue in each stage is 0.8 to 1.5:1, more preferably 1:1.

[0015] In some embodiments of the present invention, the desulfurization process is carried out under a protective atmosphere; preferably, the protective gas is an inert gas; more preferably, the inert gas is argon.

[0016] In some embodiments of the present invention, the metal ball is heated to 450-470°C, preferably 460°C, by medium-frequency induction heating;

[0017] Preferably, the residence time of the chlorine leaching residue in each stage is 30 to 60 seconds.

[0018] The applicant found that if the residence time of the chlorine leaching residue in each stage is too short, the chlorine leaching residue is not broken down to a size smaller than the pores and cannot migrate from the pores to the next area; if the residence time is too long, the metal balls do not have enough kinetic energy to break up the clumps of chlorine leaching residue, resulting in insufficient breakage of the chlorine leaching residue and affecting the desulfurization effect.

[0019] In some embodiments of the present invention, the chlorine leaching residue is first heated and dehydrated to a moisture content of 10-15 wt.% before desulfurization is carried out.

[0020] Preferably, when heating and dehydrating the chlorine leaching residue, the temperature of the chlorine leaching residue is controlled at 100-105°C, preferably 105°C.

[0021] If the temperature of the chlorine leaching residue exceeds 105℃, it will harden and clump, clogging the feed inlet. The purpose of preheating and drying the chlorine leaching residue is to prevent the mixing of water vapor and sulfur, reduce the interference of moisture on the desulfurization process during subsequent heating, and improve the desulfurization effect and process stability.

[0022] In some embodiments of the present invention, sulfur vapor is recovered as solid sulfur after dust removal and condensation;

[0023] Preferably, the heat recovered during condensation is returned to the chlorine leaching residue heating and dehydration step. The chlorine leaching residue desulfurization process disclosed in this invention uses a chlorine leaching residue desulfurization device, which includes a desulfurization tank for containing the material to be desulfurized, an inlet, an outlet, and a sulfur exhaust steam pipe respectively disposed on the desulfurization tank, and a heating mechanism for heating and desulfurizing the material to be desulfurized in the desulfurization tank; the desulfurization tank is provided with at least three partitions, which divide the internal space of the desulfurization tank into a discharge chamber and at least three desulfurization chambers arranged side by side; the diameter of the partitions is smaller than the inner diameter of the desulfurization tank, and pores are formed between the partitions and the inner wall of the desulfurization tank, and the discharge chamber and the desulfurization chambers, as well as adjacent desulfurization chambers, are connected through the pores;

[0024] Preferably, the heating mechanism includes a plurality of metal balls disposed in the desulfurization chamber, and a medium-frequency induction heater for heating the metal balls;

[0025] Preferably, the medium-frequency induction heater includes a medium-frequency generator and an induction coil wound around the outer wall of the desulfurization tank and connected to the medium-frequency generator.

[0026] In this invention, by setting up a partition, the metal ball and the chlorine leaching residue material with larger pores are confined to the original area, while the chlorine leaching residue material with smaller pores after crushing migrates from the pores to the next area.

[0027] Preferably, the gap between the discharge chamber and the desulfurization chamber is smaller than the diameter of the metal ball in the desulfurization chamber; more preferably, the gap between the discharge chamber and the desulfurization chamber is 2 mm. This design not only ensures that the metal ball is confined to its original area but also prevents blockage of the discharge port. In some embodiments of the present invention, the inlet is connected to the desulfurization chamber at one end, the outlet is connected to the discharge chamber at the other end, and the desulfurization box is equipped with a material stirring and conveying mechanism that allows the material to sequentially pass from the desulfurization chamber connected to the inlet through the intermediate desulfurization chamber and then to the discharge chamber connected to the outlet.

[0028] In some embodiments of the present invention, the desulfurization box is a hollow cylinder, the partition is a circular plate, a circular shaft is provided inside the desulfurization box, the partition is fixed on the circular shaft, and the desulfurization box, the partition and the circular shaft are coaxially distributed.

[0029] Preferably, the material stirring and conveying mechanism includes a geared motor mounted on the desulfurization box, and a spiral stirring blade mounted in the desulfurization chamber and the discharge chamber and connected to the drive end of the geared motor and adapted to the pore size.

[0030] In some embodiments of the present invention, the diameter of the metal spheres in each desulfurization chamber is different, and the diameter of the metal spheres decreases sequentially along the material flow direction;

[0031] Preferably, the pores formed between each partition and the inner wall of the desulfurization chamber are of different sizes, and the pores decrease sequentially along the material flow direction. Preferably, the desulfurization chamber is provided with a gas inlet for filling with protective gas.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] This invention is scientifically designed and ingeniously conceived. The chlorine leaching residue vaporization and sublimation desulfurization process of this invention uses metal balls as the crushing and heat transfer medium to effectively crush the solid phase and exchange heat, thereby enhancing the desulfurization efficiency.

[0034] Chlorine leaching residue has poor fluidity, and over time, this can lead to accumulation and agglomeration, clogging the feed inlet and flow channels. This invention incorporates a certain proportion of metal induction balls into the heated chlorine leaching residue. These metal balls can break up and grind the residue, effectively removing agglomerates. Simultaneously, the metal balls can sense a medium-frequency magnetic field and generate heat; heat is transferred through contact with the chlorine leaching residue and through thermal radiation.

[0035] The present invention incorporates a material stirring and conveying mechanism in the desulfurization device for chlorine leaching residue. This mechanism enables the metal balls and chlorine leaching residue to be fully mixed, achieving both effective mixing and heat transfer, as well as crushing and grinding of the chlorine leaching residue by the metal balls. This process fully disintegrates the chlorine leaching residue particles, thereby improving the desulfurization rate of the chlorine leaching residue.

[0036] This invention's process boasts high throughput and stability in dewatering, granulation, sulfur vaporization, dust removal, refrigeration, sulfur preparation, continuous heating, and temperature control of chlorine leaching residue, improving desulfurization rate and efficiency. The entire process is automated, simple to operate, and reduces the need for operator experience. Data can be monitored and adjusted in real time, facilitating continuous and efficient production. This process offers advantages such as flexible operation, high processing efficiency, and low energy consumption. It can also be applied to other dewatering processes, such as sludge dewatering, tailings dewatering, and oil sludge pyrolysis. Attached Figure Description

[0037] Appendix Figure 1 This is a process flow diagram of the present invention.

[0038] Appendix Figure 2 This is a schematic diagram of the desulfurization device for chlorine leaching residue of the present invention.

[0039] The corresponding names of the attached figures are: 1-Desulfurization box, 2-Inlet, 3-Outlet, 4-Sulfur exhaust steam pipe, 5-Metal ball, 6-Medium frequency generator, 7-Baffle plate, 8-Desulfurization chamber, 9-Pore, 10-Spiral agitator blade, 11-Round shaft, 12-Gear motor, 13-Induction coil, 14-Discharge chamber. Detailed Implementation

[0040] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0041] Example 1

[0042] As attached Figure 2 As shown in the figure, this embodiment discloses the desulfurization device for chlorine leaching residue of the present invention, including a desulfurization tank 1 for containing the material to be desulfurized, an inlet 2, an outlet 3 and a sulfur exhaust steam pipe 4 respectively provided on the desulfurization tank 1, and a heating mechanism for heating and desulfurizing the material to be desulfurized in the desulfurization tank 1.

[0043] The heating mechanism includes several metal balls 5 disposed inside the desulfurization tank 1, and a medium-frequency induction heater for heating the metal balls 5. The medium-frequency induction heater includes a medium-frequency generator 6 and an induction coil 13 wound around the outer wall of the desulfurization tank 1 and connected to the medium-frequency generator 6.

[0044] The desulfurization chamber 1 is a hollow cylinder with at least three circular partitions 7 inside. The partitions 7 divide the internal space of the desulfurization chamber 1 into a discharge chamber 14 and at least three desulfurization chambers 8 arranged side by side. The metal ball 5 is located inside the desulfurization chamber 8. The diameter of the partition 7 is smaller than the inner diameter of the desulfurization chamber 1. A pore 9 is formed between the partition 7 and the inner wall of the desulfurization chamber 1. The discharge chamber 14 and the desulfurization chamber 8, as well as adjacent desulfurization chambers 8, are all connected through the pores 9.

[0045] The desulfurization box 1 is equipped with a circular shaft 11, and the partition 7 is fixed on the circular shaft 11. The desulfurization box 1, the partition 7 and the circular shaft 11 are coaxially distributed.

[0046] The feed inlet 2 is connected to the desulfurization chamber 8 at one end, and the discharge outlet 3 is connected to the discharge chamber 14 at the other end. The desulfurization box 1 is equipped with a material stirring and conveying mechanism that allows the material to sequentially pass from the desulfurization chamber 8 connected to the feed inlet 2 through the middle desulfurization chamber 8 and then to the discharge chamber 14 connected to the discharge outlet 3.

[0047] The material mixing and conveying mechanism includes a geared motor 12 mounted on the desulfurization box 1, and a spiral mixing blade 10 mounted in the desulfurization chamber 8 and the discharge chamber 14 and connected to the drive end of the geared motor 12 and adapted to the orifice 9.

[0048] The diameter of the metal balls 5 in each desulfurization chamber 8 is different, and the diameter of the metal balls 5 decreases sequentially along the material flow direction;

[0049] The pores 9 formed between each partition 7 and the inner wall of the desulfurization box 1 are of different sizes, and the pores 9 decrease in size sequentially along the material flow direction.

[0050] The desulfurization box 1 is also equipped with a gas inlet for filling with protective gas.

[0051] Example 2

[0052] As attached Figure 1 As shown, this embodiment discloses the desulfurization process for chlorine leaching residue of the present invention. The crushing and heat transfer desulfurization step is carried out using the chlorine leaching residue desulfurization device of Example 1. The specific steps are as follows:

[0053] S1. Preheating and drying: The chlorine leaching residue is heated at 105℃ to dehydrate, and its moisture content is controlled to be 10wt.%.

[0054] S2. Crushing and Heat Transfer Desulfurization: The preheated and dried chlorine leaching residue is placed in the chlorine leaching residue desulfurization device of Example 1. After the medium-frequency induction heater is energized, the induction coil causes eddy currents in the magnetic induction medium metal balls, generating an induced electromotive force, which in turn generates an induced current, causing the surface of the metal balls to be uniformly heated. The metal balls are heated to 460°C and kept constant at 460°C. First, in the first desulfurization chamber, metal balls with a diameter of 20mm are used to crush and heat the chlorine leaching residue: Under the stirring action of the spiral stirring blades, the metal balls and chlorine leaching residue are fully mixed, and the collision and friction between the metal balls and the chlorine leaching residue achieves crushing and heat transfer, breaking up the agglomerated chlorine leaching residue in one step, and realizing the sublimation of sulfur in the chlorine leaching residue by heat.

[0055] After the initial crushing and heat transfer, the chlorine leaching residue has a particle size of less than 12 mm. Under the action of the spiral stirring blades, the crushed and heat-transferred chlorine leaching residue enters the second desulfurization chamber through the pores. The pore size between the first and second desulfurization chambers is 12 mm.

[0056] In the second desulfurization chamber, the chlorine-leaching residue, after initial crushing and heat transfer, is further crushed and heated by metal balls with a diameter of 15 mm. This process breaks down the agglomerated chlorine-leaching residue into medium-sized particles, allowing the residual sulfur in the residue to sublimate upon heating. The chlorine-leaching residue after the second crushing and heat transfer has a particle size of less than 8 mm and enters the third desulfurization chamber through pores under the action of the spiral stirring blades. The pore size between the second and third desulfurization chambers is 8 mm.

[0057] In the third desulfurization chamber, the chlorine-leaching residue after secondary crushing and heat transfer is crushed and heated by metal balls with a diameter of 10 mm, causing the agglomerated chlorine-leaching residue to be broken into smaller particles three times, achieving the sublimation of the remaining sulfur in the chlorine-leaching residue. The chlorine-leaching residue after the three crushing and heat transfer is a residue with a particle size of less than 2 mm, which enters the discharge chamber through the pores under the action of the spiral agitator blades, and is then discharged through the outlet. The pore size between the discharge chamber and the desulfurization chamber is 2 mm.

[0058] The sublimated sulfur vapor is removed by dust removal and condensation, and then recovered as liquid or solid sulfur. The heat recovered during condensation is returned to the preheating and drying step for dehydration and drying of the chlorine leaching residue.

[0059] In this embodiment, the volume ratio of chlorine leaching residue to metal balls in each desulfurization chamber is 1:1, and the entire desulfurization process is carried out under an argon atmosphere.

[0060] In this embodiment, the rotation speed of the spiral stirring blades is controlled so that the residence time of the chlorine leaching residue in each desulfurization chamber is 40 to 50 seconds.

[0061] In this embodiment, the recovery rate of elemental sulfur is greater than 99%.

[0062] Example 3

[0063] As attached Figure 1 As shown, this embodiment discloses the desulfurization process for chlorine leaching residue of the present invention. The crushing and heat transfer desulfurization step is carried out using the chlorine leaching residue desulfurization device of Example 1. The specific steps are as follows:

[0064] S1. Preheating and drying: The chlorine leaching residue is heated at 105℃ to dehydrate, and its moisture content is controlled to be 15wt.%.

[0065] S2. Crushing and Heat Transfer Desulfurization: The preheated and dried chlorine leaching residue is placed in the chlorine leaching residue desulfurization device of Example 1. After the medium-frequency induction heater is energized, the induction coil causes eddy currents in the magnetic induction medium metal balls, generating an induced electromotive force, which in turn generates an induced current, causing the surface of the metal balls to be uniformly heated. The metal balls are heated to 470°C and kept constant at 470°C. First, in the first desulfurization chamber, metal balls with a diameter of 15mm are used to crush and heat the chlorine leaching residue: Under the stirring action of the spiral stirring blades, the metal balls and chlorine leaching residue are fully mixed, and the collision and friction between the metal balls and the chlorine leaching residue achieves crushing and heat transfer, breaking up the agglomerated chlorine leaching residue in one step, and realizing the sublimation of elemental sulfur in the chlorine leaching residue by heating.

[0066] After the initial crushing, the chlorine leaching residue has a particle size of less than 12 mm. Under the action of the spiral stirring blades, it enters the second desulfurization chamber through the pores. The pore size between the first and second desulfurization chambers is 12 mm.

[0067] In the second desulfurization chamber, the chlorine-leaching residue, after initial crushing and heat transfer, is further crushed and heated by metal balls with a diameter of 10 mm. This process breaks up the agglomerated chlorine-leaching residue of medium particle size, allowing the remaining sulfur in the residue to sublimate upon heating. The chlorine-leaching residue after the second crushing and heat transfer has a particle size of less than 8 mm. Under the action of the spiral stirring blades, it enters the third desulfurization chamber through the pores. The pore size between the second and third desulfurization chambers is 8 mm.

[0068] In the third desulfurization chamber, the chlorine leaching residue, after secondary crushing and heat transfer, is further crushed and heat-transferred by metal balls with a diameter of 5 mm. This process breaks down the agglomerated chlorine leaching residue into smaller particles three times, allowing the remaining sulfur in the chlorine leaching residue to sublimate upon heating. The chlorine leaching residue after the three crushings is a residue with a particle size of less than 2 mm. Under the action of the spiral agitator blades, it enters the discharge chamber through the pores and is then discharged through the outlet. The pore size between the discharge chamber and the desulfurization chamber is 2 mm.

[0069] The sublimated sulfur vapor is removed by dust removal and condensation, and then recovered as solid sulfur. The heat recovered during condensation is returned to the preheating and drying step for dehydration and drying of the chlorine leaching residue.

[0070] In this embodiment, the volume ratio of chlorine leaching residue to metal balls in each desulfurization chamber is 1:0.8, and the entire desulfurization process is carried out under an argon atmosphere.

[0071] In this embodiment, the rotation speed of the spiral agitator blades is controlled so that the residence time of the chlorine leaching residue in each desulfurization chamber is 50 to 60 seconds.

[0072] In this embodiment, the recovery rate of elemental sulfur is greater than 99%.

[0073] Example 4

[0074] As attached Figure 1 As shown, this embodiment discloses the desulfurization process for chlorine leaching residue of the present invention. The crushing and heat transfer desulfurization step is carried out using the chlorine leaching residue desulfurization device of Example 1. The specific steps are as follows:

[0075] S1. Preheating and drying: The chlorine leaching residue is heated at 100℃ to dehydrate, and its moisture content is controlled to be 12wt.%.

[0076] S2. Crushing and Heat Transfer Desulfurization: The preheated and dried chlorine leaching residue is placed in the chlorine leaching residue desulfurization device of Example 1. After the medium-frequency induction heater is energized, the induction coil causes eddy currents in the magnetic induction medium metal balls, generating an induced electromotive force, which in turn generates an induced current, causing the surface of the metal balls to be uniformly heated. The metal balls are heated to 450°C and kept constant at 450°C. First, in the first desulfurization chamber, metal balls with a diameter of 15mm are used to crush and heat the chlorine leaching residue: Under the stirring action of the spiral stirring blades, the metal balls and chlorine leaching residue are fully mixed, and the collision and friction between the metal balls and the chlorine leaching residue achieves crushing and heat transfer, breaking up the agglomerated chlorine leaching residue in one step, and realizing the sublimation of sulfur in the chlorine leaching residue by heat.

[0077] After the initial crushing and heat transfer, the chlorine leaching residue has a particle size of less than 12 mm. Under the action of the spiral stirring blades, it enters the second desulfurization chamber through the pores. The pore size between the first and second desulfurization chambers is 12 mm.

[0078] In the second desulfurization chamber, the chlorine-leaching residue, after its initial crushing and heat transfer, is further crushed and heated by metal balls with a diameter of 10 mm. This process further breaks down the agglomerated chlorine-leaching residue particles into medium-sized particles, allowing the residual sulfur in the residue to sublimate upon heating. The chlorine-leaching residue particles after the secondary crushing and heat transfer are less than 8 mm in size. Under the action of the spiral stirring blades, they enter the third desulfurization chamber through pores. The pore size between the second and third desulfurization chambers is 8 mm.

[0079] In the third desulfurization chamber, the chlorine leaching residue, after secondary crushing, is further crushed and heated by metal balls with a diameter of 5 mm. This process breaks down the agglomerated chlorine leaching residue into smaller particles three times, allowing the remaining elemental sulfur in the chlorine leaching residue to sublimate upon heating. The chlorine leaching residue after the three crushing and heat transfer processes, consisting of residue with a particle size of less than 2 mm, enters the discharge chamber through the pores under the action of the spiral agitator blades and is then discharged through the outlet. The pore size between the discharge chamber and the desulfurization chamber is 2 mm.

[0080] The sublimated sulfur vapor is removed by dust removal and condensation, and then recovered as solid sulfur. The heat recovered during condensation is returned to the preheating and drying step for dehydration and drying of the chlorine leaching residue.

[0081] In this embodiment, the volume ratio of chlorine leaching residue to metal balls in each desulfurization chamber is 1:1.5, and the entire desulfurization process is carried out under an argon atmosphere.

[0082] In this embodiment, the rotation speed of the spiral agitator blades is controlled so that the residence time of the chlorine leaching residue particles in each desulfurization chamber is 30 to 40 seconds.

[0083] In this embodiment, the recovery rate of elemental sulfur is greater than 99%.

[0084] In summary, this invention is scientifically designed, ingeniously conceived, and capable of automated control with simple operation. The process of this invention possesses the ability to process chlorine leaching residue in terms of capacity and dehydration, chlorine leaching residue granulation, sulfur vaporization, dust removal, refrigeration, sulfur preparation, continuous operation heating capacity, and stable temperature control, thus improving the desulfurization rate and efficiency. All data can be monitored and adjusted in real time, facilitating continuous and efficient production. This process and apparatus are also suitable for the deoiling process of oil sludge; except for the temperature difference, the remaining steps are similar. Therefore, this patented process method is also suitable for the pyrolysis of oil sludge.

[0085] Finally, it should be noted that the above embodiments are merely preferred embodiments of the present invention used to illustrate the technical solutions of the present invention, and are not intended to limit it, much less limit the patent scope of the present invention; although the present invention has been described in detail with reference to the foregoing embodiments, any modifications or refinements made to the main design concept and spirit of the present invention that are not of substantial significance, but which still solve the same technical problem as the present invention, should be included within the protection scope of the present invention; in addition, the direct or indirect application of the technical solutions of the present invention to other related technical fields are similarly included within the patent protection scope of the present invention.

Claims

1. A chlorination slag desulfurization device for a chlorination slag desulfurization process, characterized by, The chlorination residue desulfurization process is as follows: under a protective atmosphere, metal balls are used as magnetic induction medium, and the metal balls are heated to 450-470 DEG C by using intermediate frequency induction, and the metal balls are mixed with the chlorination residue under stirring, and the collision and friction between the metal balls and the chlorination residue realize the crushing and heat transfer of the chlorination residue, and the agglomerated chlorination residue is fully broken and the elemental sulfur in the chlorination residue is fully heated and sublimated; The crushing and heat transfer of the metal balls to the chlorination residue are divided into at least two stages, first, large-diameter metal balls are used to crush and heat the chlorination residue, so that the agglomerated chlorination residue is broken, and the sulfur in the chlorination residue is heated and sublimated, then small-diameter metal balls are used to continue crushing and heating the chlorination residue, so that the chlorination residue is fully broken, thereby realizing full desulfurization; The chlorination residue desulfurization device comprises a desulfurization tank (1), a feeding port (2), a discharging port (3) and a sulfur vapor discharge pipe (4) arranged on the desulfurization tank (1), and a heating mechanism; the desulfurization tank (1) is provided with at least three partitions (7), and the partitions (7) divide the internal space of the desulfurization tank (1) into a discharging chamber (14) and at least three desulfurization chambers (8) arranged side by side; the diameter of the partitions (7) is smaller than the inner diameter of the desulfurization tank (1), and the partitions (7) and the inner wall of the desulfurization tank (1) form apertures (9), and the discharging chamber (14) and the desulfurization chambers (8) and the adjacent desulfurization chambers (8) are communicated through the apertures (9); The heating mechanism comprises a plurality of metal balls (5) arranged in the desulfurization chambers (8), and an intermediate frequency induction heater for heating the metal balls (5); the diameters of the metal balls (5) in each desulfurization chamber (8) are different, and the diameters of the metal balls (5) gradually decrease along the material flow direction; The material stirring and conveying mechanism comprises a speed reducer (12) arranged on the desulfurization tank (1), and a spiral stirring paddle (10) arranged in the desulfurization chambers (8) and the discharging chamber (14) and connected with the driving end of the speed reducer (12) and matched with the apertures (9).

2. The apparatus for desulphurization of chlorinatmg slag according to claim 1, characterized in that, The crushing and heat transfer of the metal balls to the chlorination residue are divided into three stages, and the diameters of the metal balls used in the three stages gradually decrease; The diameter of the metal balls used in the first stage is 15-20 mm, the diameter of the metal balls used in the second stage is 10-15 mm, and the diameter of the metal balls used in the third stage is 5-10 mm.

3. A chlorination slag desulphurization device for a chlorination slag desulphurization process according to claim 2, characterized in that, The particle size of the chlorination residue after the first stage of crushing and heat transfer is less than 12 mm; The particle size of the chlorination residue after the second stage of crushing and heat transfer is less than 8 mm; The particle size of the chlorination residue after the third stage of crushing and heat transfer is less than 2 mm.

4. The chlorination slag desulphurization apparatus for use in the chlorination slag desulphurization process according to claim 2, characterized in that, The volume ratio of the metal balls to the chlorination residue in each stage is 0.8-1.5:

1.

5. The chlorination slag desulphurization apparatus for use in the chlorination slag desulphurization process according to claim 2, characterized in that, The volume ratio of the metal balls to the chlorination residue in each stage is 1:

1.

6. The chlorination slag desulphurization device for chlorination slag desulphurization process according to claim 1 or 2, characterized in that, The protective gas is inert gas.

7. A chlorination slag desulphurization apparatus for use in a chlorination slag desulphurization process according to claim 6, characterized in that, The inert gas is argon.

8. The chlorination slag desulphurization device for chlorination slag desulphurization process according to claim 1 or 2, characterized in that, The metal balls are heated to 460 DEG C by intermediate frequency induction.

9. The apparatus for desulphurization of chloridizing slags according to claim 1 or 2, characterized in that, The residence time of the chlorination residue in each stage is 30-60 seconds.

10. The chlorination slag desulphurization device for chlorination slag desulphurization process according to claim 1 or 2, characterized in that, The chlorination residue is first heated and dehydrated to have a water content of 10-15 wt.%, and then desulfurization operation is performed.

11. A chlorination slag desulphurization apparatus for use in a chlorination slag desulphurization process according to claim 10, characterized in that, When the chlorination residue is heated and dehydrated, the material temperature of the chlorination residue is controlled to be 100-105 DEG C.

12. A chlorination slag desulphurization apparatus for use in a chlorination slag desulphurization process according to claim 10, characterized in that, When the chlorination residue is heated and dehydrated, the material temperature of the chlorination residue is controlled to be 105 DEG C.

13. The apparatus for desulphurization of chloridizing slags according to claim 1 or 2, characterized in that, After dust removal and condensation, the sulfur vapor is recovered as liquid or solid sulfur.

14. The apparatus for desulphurization of chlorinatmg slag according to claim 13, characterized in that, The recovered heat during condensation is returned to the chlorination residue to heat the dewatering step.

15. The apparatus for desulphurization of chlorinatmg slag according to claim 1, characterized in that, The intermediate frequency induction heater comprises an intermediate frequency generator (6) and an induction coil (13) wound on the outer wall of the desulfurization tank (1) and connected with the intermediate frequency generator (6).

16. The apparatus for desulphurization of chlorinatmg slag according to claim 1, characterized in that, The feed inlet (2) and the discharge outlet (3) are communicated with the desulfurization chambers (8) at the end portions, the discharge outlet (3) is communicated with the discharge chamber (14) at the other end portion, and the desulfurization tank (1) is provided with a material stirring and conveying mechanism for sequentially conveying the material from the desulfurization chamber (8) communicated with the feed inlet (2) to the discharge chamber (14) communicated with the discharge outlet (3).

17. A chlorination slag desulphurization apparatus for use in a chlorination slag desulphurization process according to claim 16, characterized in that The desulfurization tank (1) is a hollow cylinder, the partition plate (7) is a circular plate, the desulfurization tank (1) is provided with a circular shaft (11), and the partition plate (7) is fixed on the circular shaft (11).

18. The chlorinage slag desulphurization apparatus for use in the chlorinage slag desulphurization process as claimed in claim 17 wherein, The apertures (9) formed between each partition plate (7) and the inner wall of the desulfurization tank (1) are of different sizes, and the apertures (9) sequentially decrease along the material flow direction.

Citation Information

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