A high-performance insoluble sulfur production system and method

Abstract

The invention discloses a high-performance insoluble sulfur production system and method. The system includes a quenching tower, a discharge pump, a sand mill, and a filtering, washing, and drying device; the discharge port of the quenching tower is connected to the discharge pump inlet through a pipeline, the discharge pump outlet is connected to the sand mill feed port, the sand mill discharge port is connected to the feed port of the filtering, washing, and drying device, the filtrate outlet of the filtering, washing, and drying device is connected to the filtrate discharge pipe through a pipeline, the sulfur product discharge port of the filtering, washing, and drying device is connected to the sulfur product discharge pipe, the hot air inlet pipe is connected to the quenching tower hot air inlet and the filtering, washing, and drying device hot air inlet through a pipeline, and the extractant inlet pipe is connected to the quenching tower extractant inlet and the extractant inlet of the filtering, washing, and drying device at the same time. By wet ball milling sulfur, drying, aging, and extraction treatment, a non-oil-filled insoluble sulfur product can be obtained. The invention has the advantages of simple production process, safe and reliable process, etc.

Description

Technical Field

[0001] The invention belongs to the technical field of petrochemical industry and relates to a high-performance insoluble sulfur production system and method. Background Art

[0002] With the sharp increase in oil consumption, global oil resources are becoming increasingly scarce, and the heavy and inferior quality of refinery raw materials are becoming increasingly serious; at the same time, environmental protection regulations in various countries are becoming increasingly stringent, and the total sulfur content of petroleum products and natural gas is being controlled more strictly. Therefore, the production capacity of sulfur recovery units in major refineries and natural gas purification plants has increased rapidly. The domestic and foreign markets for this type of ordinary sulfur have become saturated, so the price is low. How to provide high-value-added sulfur products that are in short supply in the market has become the focus of attention of related companies.

[0003] Insoluble sulfur is a highly efficient rubber vulcanizer with the advantages of good distribution stability in the rubber compound and uniform crosslinking points of the product. It can overcome the frost on the rubber compound surface and improve the bonding performance between rubber and steel wire or chemical fiber cord. The main production methods of insoluble sulfur are low-temperature melting method and gasification method.

[0004] Patent CN102070127A discloses a method for producing insoluble sulfur, which comprises the following steps: (1) melt polymerization; (2) atomization cold extraction; (3) solidification; (4) centrifugal separation; (5) continuous drying; (6) crushing, screening and oil filling to finally obtain a finished product. This method is a continuous production method, but the sulfur polymerization operating temperature and pressure of this method are relatively high, the operating temperature is 580-690°C, and the operating pressure is 0.8-1.2MPa, which places high requirements on the reaction equipment.

[0005] Patent CN 206915765 U discloses a production system for insoluble sulfur, including a polymerization reaction unit and an extrusion pelletizing unit, wherein the discharge port of the polymerization reaction unit is connected to the feed port of the extrusion pelletizing unit, and the polymerization reaction unit is used to polymerize the raw sulfur to obtain an insoluble sulfur melt; the extrusion pelletizing unit includes an extruder, a die face pelletizer, a quenching container, a dehydrator and an air conveying device. The utility model has a reasonable structure, can shorten the process flow, reduce material loss, save costs, improve production efficiency, reduce labor intensity, improve the working environment, and realize the safe production of insoluble sulfur. However, when the sulfur temperature is 250°C to 270°C, the sulfur viscosity is high, the material is seriously wired, and there is a problem of difficulty in extrusion pelletizing. Therefore, the production system of an insoluble sulfur disclosed in the patent is not suitable for producing insoluble sulfur by a low-temperature melting method.

[0006] Patent CN 104401946B discloses a gasification quenching process for insoluble sulfur. The process method first heats liquid sulfur to make it in a superheated liquid sulfur state, sprays the superheated sulfur liquid into a circulating spray cooling medium liquid curtain, and under the action of a huge pressure difference, the superheated sulfur liquid is converted into dispersed gas mist two phases, which are fully quenched and absorbed by the cooling medium, and then enters the cooling medium liquid environment at the bottom of the reaction tank for solidification and extraction to obtain insoluble sulfur. The method circulates the cooling medium to form a liquid curtain, which changes the traditional practice of directly impacting liquid sulfur with the cooling medium. The formed liquid curtain increases the contact area with the gas mist two-phase sulfur, which can make the cooling medium liquid curtain quench the gas mist two-phase sulfur more fully and carefully, avoiding the rough practice in the traditional quenching process. The insoluble sulfur product obtained by this method has fine particles, high purity, good finished product dispersibility, and is suitable for industrial production. The quenching process is suitable for the production of insoluble sulfur by gasification method, but not suitable for the production of insoluble sulfur by low-temperature melting method.

[0007] At present, the insoluble sulfur produced by the existing low-temperature melting method has poor thermal stability and low yield, the system operates intermittently, the polymerized sulfur has high viscosity, and granulation is difficult. Summary of the invention

[0008] In view of the problems existing in the prior art, the object of the present invention is to provide a high-performance insoluble sulfur production system and method.

[0009] The high-performance insoluble sulfur production system and method can obtain non-oil-filled insoluble sulfur products by wet ball milling and integrated equipment drying, aging and extraction treatment of sulfur. The production process is simple, and the production process is safe and reliable, the equipment and operation are simple, the operating cost is low, and the energy-saving effect is obvious.

[0010] According to a first aspect of the present invention, the present invention provides a high performance insoluble sulfur production system.

[0011] Specifically, the insoluble sulfur production system includes a quenching tower, a discharge pump, a sand mill, a filtering, washing and drying device and corresponding connecting pipelines; wherein the discharge port of the quenching tower is connected to the inlet of the discharge pump through a pipeline, the outlet of the discharge pump is connected to the feed port of the sand mill, the discharge port of the sand mill is connected to the feed port of the filtering, washing and drying device, the filtrate outlet of the filtering, washing and drying device is connected to the filtrate discharge pipe through a pipeline, the insoluble sulfur product discharge port of the filtering, washing and drying device is connected to the insoluble sulfur product discharge pipe, the hot air inlet pipe is connected to the hot air inlet of the quenching tower and the hot air inlet of the filtering, washing and drying device through a pipeline, and the extractant inlet pipe is connected to the extractant inlet of the quenching tower and the extractant inlet of the filtering, washing and drying device through a pipeline.

[0012] Furthermore, the quenching tower comprises a cylinder, and a rotating shaft is provided at the center of the cylinder axis; the cylinder interior comprises a feeding section, a quenching section and a crushing section from top to bottom;

[0013] The feed section is located at the upper part of the quenching tower, and is provided with a quenching liquid inlet, a sulfur inlet, an extractant inlet, a hot air inlet and a sulfur distributor;

[0014] The quenching section is located in the middle (section) of the quenching tower, and no components are arranged in the quenching section so that the high-temperature material is directly quenched with the quenching water;

[0015] The crushing section is located at the lower part of the quenching tower, a stirring rod and a crushing ball are arranged in the crushing section, and a grading mesh plate is arranged at the bottom of the crushing section.

[0016] Furthermore, the quenching tower is used to cool, mix and crush the high-temperature sulfur entering the device. The quenching tower is a cylindrical barrel structure.

[0017] Furthermore, the quenching liquid inlet and the sulfur inlet are located at the top or upper wall of the quenching tower cylinder, and the sulfur distributor is arranged in the cylinder. The sulfur inlet is connected to the sulfur distributor inlet through a pipeline.

[0018] Furthermore, the quenching liquid inlet, the sulfur inlet, the extractant inlet and the hot air inlet are arranged at the top or the upper wall of the quenching tower, and the sulfur distributor is arranged in the cylinder. The sulfur inlet is connected to the sulfur distributor inlet through a pipeline.

[0019] Furthermore, a motor is arranged outside the top of the cylinder, and the motor is used to drive the rotating shaft. The rotating shaft runs through the feeding section, the quenching section and the crushing section. The stirring rods are evenly distributed on the rotating shaft and fixedly connected to the rotating shaft; the crushing balls are dispersed in the crushing section. The grading discharge module is located at the center of the axis of the crushing section.

[0020] Furthermore, the grading discharging module includes a grading mesh plate and a discharging port. The grading mesh plate includes a mesh plate tube and a mesh plate top cover located at the top of the mesh plate tube. The grading mesh plate is a cylindrical structure, and the mesh plate top cover is fixedly connected to the rotating shaft. The mesh plate tube constitutes the rotating shaft of the crushing section (i.e., the lower section of the rotating shaft), and stirring rods are evenly distributed on the outer wall of the mesh plate tube. The cylinder wall of the mesh plate tube is provided with a plurality of slits or openings, and the slit width or the opening diameter is smaller than the diameter of the crushing ball. There is a gap between the lower edge of the mesh plate tube and the bottom plate of the quenching tower, and the height of the gap should be smaller than the diameter of the crushing ball, generally 0.5 to 0.8 times the diameter of the crushing ball. A discharging port is provided in the center of the bottom plate of the quenching tower, and the diameter of the discharging port is not larger than the diameter of the grading mesh plate. The grading mesh plate is used to isolate the crushing balls to prevent them from entering the grading mesh plate.

[0021] Furthermore, the sulfur distributor can be a granulator, an extruder or an atomizer, etc. The sulfur distributor is used to disperse the sulfur in the quenching tower.

[0022] In the present invention, the filtering, washing and drying equipment can adopt the conventional structure in the art. The present invention recommends the use of a three-in-one equipment with the following structure.

[0023] Furthermore, the integrated filtering, washing and drying equipment comprises:

[0024] The filter sleeve comprises an outer sleeve and an inner sleeve; the outer sleeve is sleeved outside the inner sleeve, an inner sleeve jacket is arranged in the annular space formed by the outer sleeve and the inner sleeve, and the inner sleeve jacket is used to heat the material in the inner sleeve; a filter screen is arranged on the inner sleeve wall opposite to the inner sleeve jacket, and a filtrate outlet is arranged on the outer sleeve wall corresponding to the filter screen, and the filtrate outlet can also be used as a hot air outlet;

[0025] The material inlet and outlet cylinder is horizontally arranged and communicated with the filter sleeve; the material inlet and outlet cylinder includes a material inlet at the top, a material outlet at the bottom, and a material inlet and outlet jacket, and the material inlet can also be used as a hot air inlet;

[0026] A rotating jacket shaft can rotate in a filter sleeve; the rotating jacket shaft is composed of an outer shaft tube and an inner shaft tube: the inner shaft tube is provided with an inlet for a shaft heating medium, and the outer shaft tube is provided with an outlet for a shaft heating medium; a plurality of distribution branches are provided on the circumferential outer wall of the inner shaft tube, and a plurality of stirring paddles are provided on the circumferential outer wall of the outer shaft tube, and the plurality of distribution branches are provided correspondingly to the plurality of stirring paddles, and the outlets of the distribution branches are located in the corresponding internal spaces of the stirring paddles.

[0027] Furthermore, the filter sleeve is arranged horizontally. End face flange covers are arranged at both ends of the filter sleeve. The filtrate outlet is arranged at the bottom of the outer cylinder, and the filter screen is located at the bottom of the inner cylinder. A vacuum gas outlet is also arranged on the side of the outer cylinder. Preferably, the arc width of the filter screen is 0.5 to 1.0 times the arc width of the inner cylinder jacket.

[0028] Furthermore, in the filter sleeve, the heat medium inlet of the inner tube jacket and the heat medium outlet of the inner tube jacket are both arranged on the side of the inner tube and pass through the end face flange cover.

[0029] Furthermore, the material inlet and outlet cylinder is a cylindrical jacket structure, which is equivalent to the diameter of the filter sleeve. The material inlet is located at the top of the material inlet and outlet cylinder, and the material outlet is located at the bottom of the material inlet and outlet cylinder. The material inlet is arranged at the top of the material inlet and outlet cylinder, and the heating medium inlet and heating medium outlet of the material inlet and outlet jacket are both arranged at the bottom of the material inlet and outlet cylinder.

[0030] Further, the material inlet and outlet (heating) jacket is arranged around the material inlet and outlet, and includes a jacket heating medium inlet and a jacket heating medium outlet. Preferably, the jacket heating medium inlet, the material outlet, and the jacket heating medium outlet are all arranged at the bottom of the material inlet and outlet barrel.

[0031] Furthermore, the shaft inner tube and shaft outer tube are coaxial central inner and outer sleeves, the shaft heating medium inlet is arranged on the outer wall of the shaft inner tube, and the shaft heating medium outlet is arranged on the outer wall of the shaft outer tube. The stirring paddle on the outer wall of the shaft outer tube and the distribution branch pipe on the outer wall of the shaft inner tube are both located in a closed space formed by the end face flange cover, the filter sleeve, and the material inlet and outlet tube.

[0032] Furthermore, the device of the present invention further comprises a motor, which is used to drive the rotating jacket shaft to rotate. The motor is located at one end of the rotating jacket shaft, and the shaft heating medium inlet and the shaft heating medium outlet are located at the other end of the rotating jacket shaft. The motor and the shaft heating medium inlet and the shaft heating medium outlet are all located outside the closed space formed by the end face flange cover, the filter sleeve, and the material inlet and outlet cylinder.

[0033] Furthermore, the rotating jacket shaft passes through the end face flange cover, the filter sleeve and the center of the material inlet and outlet cylinder shaft. Preferably, the filter sleeve and the material inlet and outlet cylinder are fixedly connected by a flange. The two ends of the filtering, washing and drying equipment composed of the filter sleeve and the material inlet and outlet cylinder are fixedly sealed by the end face flange cover, and the filtering, washing and drying equipment is composed of at least one combination of the filter sleeve and the material inlet and outlet cylinder.

[0034] Furthermore, the stirring paddle may be of rake type or disc type. Preferably, fins are evenly distributed on the outer wall of the stirring paddle.

[0035] Furthermore, the two ends of the shaft outer cylinder are connected to the end face flange cover via a sealing component, and the sealing component can be a mechanical seal, a gas seal or a packing seal.

[0036] Furthermore, the rotating shaft is driven by a motor to drive a stirring paddle to rotate, and a heating medium flows in the rotating jacket shaft to heat the stirring material.

[0037] Furthermore, the filter sleeve is used for solid-liquid separation and heating in filtering, washing and drying equipment, and the material inlet and outlet cylinder is used for material inlet and outlet and jacket heating.

[0038] Furthermore, the material inlet and outlet cylinder is used for filtering the material in and out of the washing and drying equipment and for jacket heating.

[0039] Furthermore, the discharge pump and sand mill are technologies well known in the art.

[0040] The second aspect of the present invention provides a high-performance insoluble sulfur production method, which adopts the insoluble sulfur production system described above.

[0041] Specifically, the production method includes the following contents:

[0042] (1) The quenching liquid continuously enters the quenching tower through the quenching liquid inlet to control the liquid level of the quenching liquid in the quenching tower. At the same time, the quenching liquid continuously discharges the quenching tower through the discharge port and is discharged from the production system through the quenching liquid discharge pipe;

[0043] (2) After the quenching liquid level in the quenching tower is controlled to be stable, the high-temperature sulfur enters the sulfur distributor through the sulfur inlet and then enters the quenching section. The dispersed sulfur enters the quenching liquid to be cooled or mixed. The dispersed sulfur after cooling or mixing is quenched and becomes brittle in the quenching section.

[0044] (3) After the sulfur is quenched, stop introducing the quenching liquid into the quenching tower, and discharge the quenching liquid in the quenching tower through the outlet of the quenching tower; introduce hot air into the quenching tower from the hot air inlet, and use the hot air to dry the sulfur until the moisture content is less than 1%; continue to introduce hot air for aging;

[0045] (4) After the sulfur is dried and matured, the extractant is continuously added to the quenching tower through the extractant inlet, and the motor at the top of the quenching tower is started. The motor drives the stirring rod and the crushing ball to rotate, so that the sulfur that has become brittle after rapid cooling is crushed and extraction is achieved at the same time; during the sulfur crushing process, sulfur powder smaller than the slit width or the opening diameter of the grading mesh plate passes through the mesh holes and enters the grading mesh plate, and enters the discharge pump together with the extractant through the discharge port;

[0046] (5) The material discharged from the quenching tower outlet is lifted and transported to the sand mill through the discharge pump, and further ground to 100-300 mesh. The slurry containing 100-mesh sulfur powder is discharged from the sand mill outlet and enters the filtering, washing and drying equipment;

[0047] (6) The slurry is first filtered in a filtering, washing and drying device to filter out the extractant and obtain a sulfur powder filter cake;

[0048] (7) The sulfur powder filter cake is further extracted in a filtering, washing and drying device. The insoluble sulfur obtained after extraction and filtration is dried again with hot air to obtain an un-oiled insoluble sulfur product.

[0049] Furthermore, in step (2), the quenching time of sulfur in the quenching section of the quenching tower is 1 h to 2 h.

[0050] Furthermore, the temperature of hot air drying in step (3) is 50° C. to 70° C. The conditions of hot air aging include: aging time of 30 h to 50 h, aging temperature of 50° C. to 70° C. The hot air can be hot gas such as nitrogen gas, carbon dioxide gas, etc.

[0051] Furthermore, in step (4), the sulfur particles passing through the slits or openings of the grading mesh are 1 mm to 8 mm.

[0052] Furthermore, in step (7), intermittent extraction is performed 2 to 4 times, and the mass ratio of the extractant to solid is 2 to 4:1. The temperature of hot air drying is 50°C to 70°C. The extractant on the surface of the sulfur powder is removed by hot air drying. The extractant is selected from at least one solvent such as carbon disulfide, benzene, and cyclohexane.

[0053] Compared with the prior art, the high-performance insoluble sulfur production system and method of the present invention has the following advantages:

[0054] 1. In the insoluble sulfur production system of the present invention, the polymerized sulfur quenching, crushing and extraction operations are realized in the quenching tower, which improves the high-temperature sulfur quenching effect and ensures the yield and thermal stability of the product.

[0055] 2. In the insoluble sulfur production system of the present invention, the high-temperature sulfur is distributed, quenched, crushed and extracted in the quenching tower, and is further crushed in the sand mill, so that the high-temperature sulfur is directly converted into sulfur powder that meets the product particle size requirements (the sulfur powder particle size is required to be less than 100 meshes), avoiding the transportation of solid sulfur particles and avoiding the problem of blockage in the production system.

[0056] 3. In the insoluble sulfur production system of the present invention, 100-mesh sulfur is subjected to sulfur extraction, filtration and extractant drying in the filtering, washing and drying equipment, and the filtering, drying and washing processes are completed simultaneously in the same equipment, thereby simplifying the process flow.

[0057] 4. In the insoluble sulfur production system of the present invention, compared with the intermittent quenching process of producing insoluble sulfur by the conventional low-temperature melting method, the system has the advantages of safety and reliability, simple equipment and operation, and low operating cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0058] Figure 1 It is a schematic diagram of the high-performance insoluble sulfur production system of the present invention.

[0059] Figure 2 It is a schematic diagram of a grading screen in the high-performance insoluble sulfur production system of the present invention.

[0060] Figure 3 It is a cross-sectional view of the filtering, washing and drying equipment of the present invention.

[0061] Figure 4 It is a view of the inner cylinder axis in the filtering, washing and drying equipment of the present invention.

[0062] Figure 5 It is a schematic cross-sectional view of DD in the filtering, washing and drying equipment of the present invention.

[0063] In the figure, the numbers correspond to the following parts: 1-discharging pump, 2-sand mill, 3-discharging pipe for insoluble sulfur product, 4-hot air inlet, 5-extractant inlet, 6-filtrate discharging pipe, 7-quenching liquid discharging pipe, 100-quenching tower, 101-sulfur feeding pipeline, 102-sulfur inlet, 103-quenching liquid feeding pipeline, 104-quenching liquid inlet, 105-motor, 106-sulfur distributor, 107-discharging port, 108-rotating shaft, 109-mesh cylinder, 110-stirring rod, 111-crushing ball, 112-grading mesh, 120-mesh, 121-mesh top cover, 122-extractant inlet, 123-hot air inlet, A-quenching tower feeding section, B-quenching tower quenching section, C-quenching tower crushing section.

[0064] 300- filtering, washing and drying equipment, 310- rotating shaft, 311- motor, 312- rotating jacket shaft, 313- shaft outer cylinder, 314- shaft inner cylinder, 315- shaft heating medium inlet, 316- shaft heating medium outlet, 317- stirring paddle, 318- distribution branch pipe, 320- end face flange cover, 330- filter sleeve, 331- outer cylinder, 332- filtrate outlet (hot air outlet), 333- inner cylinder, 334- filter screen, 335- inner cylinder jacket, 336- inner cylinder jacket heat medium inlet, 337- inner cylinder jacket heat medium outlet, 338- vacuum gas outlet, 340- material in and out of the cylinder, 341- material inlet (hot air inlet, extractant inlet), 342- material in and out of the cylinder jacket, 343- jacket heating medium inlet, 344- material outlet, 345- jacket heating medium outlet. DETAILED DESCRIPTION

[0065] The present invention will be further described below by way of specific examples, but is not limited to the following examples.

[0066] Example 1

[0067] This embodiment will describe the insoluble sulfur production system of the present invention in detail with reference to the accompanying drawings.

[0068] like Figure 1-3As shown, the insoluble sulfur production system includes a quenching tower 100, a discharge pump 1, a sand mill 2, a filtering, washing and drying device 300 and corresponding connecting pipelines. The quenching tower discharge port 107 is connected to the discharge pump 1 inlet through a pipeline, the discharge pump 1 outlet is connected to the sand mill 2 feed port, the sand mill 2 discharge port is connected to the feed port 341 of the filtering, washing and drying device 300, the filtrate outlet 332 of the filtering, washing and drying device 300 is connected to the filtrate discharge pipe 6 through a pipeline, the insoluble sulfur product discharge port 344 of the filtering, washing and drying device 300 is connected to the insoluble sulfur product discharge pipe 3, the hot air inlet pipe 4 is connected to the quenching tower hot air inlet 123 and the hot air inlet (material inlet) 341 of the filtering, washing and drying device through a pipeline, and the extractant inlet pipe 5 is connected to the quenching tower extractant inlet 122 and the extractant inlet (material inlet) 341 of the filtering, washing and drying device through a pipeline.

[0069] The quenching tower 100 includes a cylinder, and a rotating shaft 108 is provided at the center of the cylinder axis; the cylinder includes a feed section A, a quenching section B and a crushing section C from top to bottom. The feed section A is located at the upper part of the quenching tower 100, and the feed section A is provided with a quenching liquid inlet 104, a sulfur inlet 102, an extractant inlet 122, a hot air inlet 123 and a sulfur distributor 106. The quenching section B is located in the middle of the quenching tower, and no components are provided in the quenching section. The crushing section C is located at the lower part of the quenching tower 100, and a stirring rod 110 and a crushing ball 111 are provided in the crushing section C, and a grading mesh plate 112 is provided at the bottom of the crushing section. The quenching tower 100 is used to cool, mix and crush the high-temperature sulfur entering the device. The quenching tower 100 is a cylindrical cylinder structure.

[0070] The quenching liquid inlet 104, the sulfur inlet 102, the extractant inlet 122, and the hot air inlet 123 are arranged at the top or the upper wall of the quenching tower 100, and the sulfur distributor 106 is arranged in the cylinder. The sulfur inlet 102 is connected to the inlet of the sulfur distributor 106 through a pipeline.

[0071] A motor 105 is arranged outside the top of the cylinder, and the motor 105 is used to drive a rotating shaft 108. The rotating shaft 108 passes through the feeding section A, the quenching section B and the crushing section C. The stirring rods 110 are evenly distributed on the rotating shaft 108 and are fixedly connected to the rotating shaft 108; the crushing balls 111 are dispersed in the crushing section C. The grading mesh plate 112 is located at the axis center of the crushing section C.

[0072] The grading mesh plate 112 includes a mesh plate cylinder 109 and a mesh plate top cover 121 located at the top of the mesh plate cylinder. The grading mesh plate is a cylindrical structure, and the mesh plate top cover 121 is fixedly connected to the rotating shaft 108. The mesh plate cylinder 109 constitutes the lower section of the rotating shaft, and the stirring rods 110 are evenly distributed on the outer wall of the mesh plate cylinder 109. The cylinder wall of the mesh plate cylinder 109 is provided with a plurality of slits or mesh holes 120, and the slit width or mesh hole diameter is smaller than the diameter of the crushing ball 111. There is a gap between the lower edge of the mesh plate cylinder 109 and the bottom plate of the quenching tower 100, and the height of the gap is smaller than the diameter of the crushing ball 111, generally 0.5 times to 0.8 times the diameter of the crushing ball 111. A discharge port 107 is provided at the center of the bottom plate of the quenching tower 100, and the diameter of the discharge port 107 is not greater than the diameter of the grading mesh plate 112. The grading mesh plate 112 is used to block the crushing ball 111 to prevent it from entering the grading mesh plate 112.

[0073] The sulfur distributor 106 can be selected from a granulator, an extruder or an atomizer, and the sulfur distributor is used to disperse the sulfur in the quench tower 100 .

[0074] like Figure 3-5 As shown, the filtering, washing and drying integrated equipment comprises:

[0075] The filter sleeve 330 includes an outer sleeve 331 and an inner sleeve 333; the outer sleeve 331 is sleeved outside the inner sleeve 333, and an inner sleeve jacket 335 is arranged in the annular space formed by the outer sleeve 331 and the inner sleeve 333, and the inner sleeve jacket 335 is used to keep the material in the inner sleeve 333 warm and heat it; a filter screen 334 is arranged on the wall of the inner sleeve 333 opposite to the inner sleeve jacket 335, and a filtrate outlet 332 is arranged on the wall of the outer sleeve 331 corresponding to the filter screen 334;

[0076] The material inlet and outlet cylinder 340 is horizontally arranged and communicated with the filter sleeve 330; the material inlet and outlet cylinder 340 includes a material inlet 341 at the top, a material outlet 344 at the bottom, and a material inlet and outlet jacket 342;

[0077] The rotating jacket shaft 312 can rotate in the filter sleeve 330; the rotating jacket shaft 312 is composed of an outer shaft cylinder 313 and an inner shaft cylinder 314: the inner shaft cylinder 314 is provided with an shaft heating medium inlet 315, and the outer shaft cylinder 313 is provided with an shaft heating medium outlet 316; a plurality of distribution branches 318 are provided on the circumferential outer wall of the inner shaft cylinder 314, and a plurality of stirring paddles 317 are provided on the circumferential outer wall of the outer shaft cylinder 313, and the plurality of distribution branches 318 are respectively provided corresponding to the plurality of stirring paddles 317, and the outlets of the distribution branches 318 are located in the corresponding internal spaces of the stirring paddles 317.

[0078] The filter sleeve 330 is arranged horizontally, and end face flange covers 320 are arranged at both ends. The inner tube jacket heat medium inlet 336 and the inner tube jacket heat medium outlet 337 are both arranged on the side of the inner tube and pass through the end face flange cover 320. The filtrate outlet 332 is arranged at the bottom of the outer tube, and the filter screen 334 is located at the bottom of the inner tube. A vacuum gas outlet 338 is also arranged on the side of the outer tube. The arc width of the filter screen 334 is 0.5~1.0 times the arc width of the inner tube jacket 335.

[0079] The material inlet and outlet cylinder 340 is a cylindrical jacket structure, which has a diameter equivalent to that of the filter sleeve 330. The heating medium inlet 343 and the heating medium outlet 345 of the material inlet and outlet cylinder jacket 342 are both arranged at the bottom of the material inlet and outlet cylinder 340. The material inlet and outlet (heating) jacket 342 is arranged around the material inlet and outlet.

[0080] In the rotating jacket shaft 312, the shaft inner cylinder 314 and the shaft outer cylinder 315 are coaxial central inner and outer sleeves, the shaft heating medium inlet 315 is arranged on the outer wall of the shaft inner cylinder 314, and the shaft heating medium outlet 316 is arranged on the outer wall of the shaft outer cylinder 313. The stirring paddle 317 on the outer wall of the shaft outer cylinder 313 and the distribution branch pipe 317 on the outer wall of the shaft inner cylinder 314 are both located in a closed space formed by the end face flange cover 320, the filter sleeve 330, and the material inlet and outlet cylinder 340.

[0081] The filtering, washing and drying device 300 further includes a motor 311, which is used to drive the rotating jacket shaft 312 to rotate. The motor 311 is located at one end of the rotating jacket shaft 312, and the shaft heating medium inlet 315 and the shaft heating medium outlet 316 are located at the other end of the rotating jacket shaft 312. The motor 311 and the shaft heating medium inlet 315 and the shaft heating medium outlet 316 are all located outside the closed space formed by the end face flange cover 320, the filter sleeve 330, and the material inlet and outlet cylinder 340.

[0082] The rotating jacket shaft 312 passes through the end face flange cover 320, the filter sleeve 330 and the center of the material inlet and outlet cylinder shaft 340. The filter sleeve 330 and the material inlet and outlet cylinder 340 are fixedly connected by a flange. The two ends of the filtering, washing and drying device 300 composed of the filter sleeve 330 and the material inlet and outlet cylinder 340 are fixedly sealed by the end face flange cover 320. The filtering, washing and drying device 300 is composed of at least one combination of the filter sleeve 330 and the material inlet and outlet cylinder 340.

[0083] The stirring paddle 317 can be of rake type or disc type. Preferably, fins are evenly distributed on the outer wall of the stirring paddle 317. Both ends of the shaft outer cylinder 313 are connected to the end face flange cover 320 through a sealing member, and the sealing member can be a mechanical seal, a gas seal or a packing seal. The rotating shaft 310 is used to drive the stirring paddle 317 to rotate under the drive of the motor 311, and the heating medium is used to flow in the rotating jacket shaft 312 to heat the stirring material.

[0084] The material inlet and outlet cylinder 340 is used for filtering the material in and out of the washing and drying equipment 300 and for jacket heating.

[0085] Example 2

[0086] This embodiment will describe the insoluble sulfur production method of the present invention in detail with reference to the accompanying drawings.

[0087] Combination Figure 1-5 , the insoluble sulfur production method comprises:

[0088] (1) The quenching liquid continuously enters the quenching tower 100 through the quenching liquid inlet 104, the quenching liquid level in the quenching tower 100 is controlled, and the quenching liquid continuously discharges the quenching tower 100 through the discharge port 107 and is discharged from the production system through the quenching night discharge pipe 7;

[0089] (2) After the quenching liquid level in the quenching tower 100 is controlled to be stable, the high-temperature sulfur enters the sulfur distributor 106 through the sulfur inlet 102, and then enters the quenching section B of the quenching tower. The dispersed sulfur enters the quenching liquid to be cooled or mixed. The dispersed sulfur after cooling or mixing is quenched and becomes brittle in the quenching section B and the crushing section C.

[0090] (3) After the sulfur is quenched, the quenching liquid is stopped from being introduced, and the quenching liquid in the quenching tower 100 is discharged through the discharge port 107; hot air is introduced into the quenching tower 100 from the hot air inlet 123, and the sulfur is dried by the heat medium until the moisture content of the sulfur is less than 1%; hot air is continued to be introduced to mature the sulfur;

[0091] (4) After the sulfur is dried and matured, the extractant is continuously added to the quenching tower through the extractant inlet 122, and the motor is started, and the rotating shaft 108 drives the stirring rod 110 and the crushing ball 111 to rotate; the sulfur that has become brittle after rapid cooling is crushed and extracted at the same time; during the crushing process, sulfur powder that is smaller than the slit width or mesh aperture of the grading mesh plate 112 enters the grading mesh plate 112 through the mesh 120, and enters the discharge pump 1 together with the extractant through the discharge port 107;

[0092] (5) The material discharged from the quench tower 100 is lifted and transported to the sand mill 2 by the discharge pump 1, and further ground to 100-300 meshes. The slurry containing 100-mesh sulfur powder is discharged from the discharge port of the sand mill 2 and enters the filtering, washing and drying equipment 300;

[0093] (6) The slurry is first filtered in the filtering, washing and drying equipment 300 to obtain a sulfur powder filter cake;

[0094] (7) The sulfur powder filter cake is further extracted in the filtering, washing and drying equipment 300. The insoluble sulfur obtained after extraction and filtration is dried again with hot air to obtain an insoluble sulfur product that is not filled with oil.

[0095] The low-temperature melting method insoluble sulfur production system and method of the present invention adopts a quenching tower and a sand mill for two-stage crushing, thereby improving the reliability of the production system and reducing the equipment scale and investment of the quenching tower. Since the quenched sulfur is first dried and matured by hot air and then crushed and extracted, the production system not only greatly shortens the process operation flow and reduces the system investment, but also reduces the energy consumption of the drying process, thereby achieving the purpose of system energy saving.

Claims

1. A high-performance insoluble sulfur production system, characterized in that: The system includes a quenching tower, a discharge pump, a sand mill, a filtering, washing and drying device and corresponding connecting pipelines; wherein, The quenching tower discharge port is connected to the discharge pump inlet through a pipeline, the discharge pump outlet is connected to the sand mill feed port, the sand mill discharge port is connected to the feed port of the filtering, washing and drying equipment, the filtrate outlet of the filtering, washing and drying equipment is connected to the filtrate discharge pipe through a pipeline, the insoluble sulfur product discharge port of the filtering, washing and drying equipment is connected to the insoluble sulfur product discharge pipe, the hot air inlet pipe is connected to the quenching tower hot air inlet and the filtering, washing and drying equipment hot air inlet through a pipeline, and the extractant inlet pipe is connected to the quenching tower extractant inlet and the extractant inlet of the filtering, washing and drying equipment through a pipeline; The filtering, washing and drying equipment comprises: The filter sleeve comprises an outer sleeve and an inner sleeve; the outer sleeve is sleeved outside the inner sleeve, an inner sleeve jacket is arranged in the annular space formed by the outer sleeve and the inner sleeve, and the inner sleeve jacket is used to heat the material in the inner sleeve; a filter screen is arranged on the inner sleeve wall opposite to the inner sleeve jacket, and a filtrate outlet is arranged on the outer sleeve wall corresponding to the filter screen, and the filtrate outlet can also be used as a hot air outlet; The material inlet and outlet cylinder is horizontally arranged and communicated with the filter sleeve; the material inlet and outlet cylinder includes a material inlet at the top, a material outlet at the bottom, and a material inlet and outlet jacket, and the material inlet can also be used as a hot air inlet; A rotating jacket shaft can rotate in a filter sleeve; the rotating jacket shaft is composed of an outer shaft tube and an inner shaft tube: the inner shaft tube is provided with an inlet for a shaft heating medium, and the outer shaft tube is provided with an outlet for a shaft heating medium; a plurality of distribution branches are provided on the circumferential outer wall of the inner shaft tube, and a plurality of stirring paddles are provided on the circumferential outer wall of the outer shaft tube, and the plurality of distribution branches are provided correspondingly to the plurality of stirring paddles, and the outlets of the distribution branches are located in the corresponding internal spaces of the stirring paddles.

2. The system according to claim 1, characterized in that The quenching tower comprises a cylinder, the axis center of which is provided with a rotating shaft; the cylinder interior comprises a feeding section, a quenching section and a crushing section in order from top to bottom; The feed section is located at the upper part of the quenching tower, and is provided with a quenching liquid inlet, a sulfur inlet, an extractant inlet, a hot air inlet and a sulfur distributor; The quenching section is located in the middle of the quenching tower, and no components are arranged in the quenching section, so that the high-temperature material is directly quenched with the quenching water; The crushing section is located at the lower part of the quenching tower, a stirring rod and a crushing ball are arranged in the crushing section, and a grading mesh plate is arranged at the bottom of the crushing section.

3. The system according to claim 2, characterized in that The quenching liquid inlet and the sulfur inlet are located at the top or upper wall of the quenching tower cylinder, and the sulfur distributor is arranged in the cylinder; the sulfur inlet is connected with the sulfur distributor inlet through a pipeline.

4. The system according to claim 2, characterized in that A motor is arranged outside the top of the cylinder, and the motor is used to drive a rotating shaft; the rotating shaft passes through the feeding section, the quenching section and the crushing section, the stirring rods are evenly distributed on the rotating shaft and fixedly connected to the rotating shaft, and the grading discharging module is located at the axis center of the crushing section.

5. The system according to claim 4, characterized in that The grading discharging module comprises a grading mesh plate and a discharging port; the grading mesh plate comprises a mesh plate cylinder and a mesh plate top cover located on the top of the mesh plate cylinder; the grading mesh plate is a cylinder structure, and the mesh plate top cover is fixedly connected to the rotating shaft; the mesh plate cylinder constitutes the rotating shaft of the crushing section; stirring rods are evenly distributed on the outer wall of the mesh plate cylinder; a plurality of slits or openings are opened on the cylinder wall of the mesh plate cylinder, and the slit width or the opening diameter is smaller than the diameter of the crushing ball; There is a gap between the lower edge of the mesh plate cylinder and the bottom plate of the quench tower, and the height of the gap is smaller than the diameter of the crushing ball; A discharge port is arranged at the center of the bottom plate of the quench tower, and the diameter of the discharge port is not larger than the diameter of the grading mesh plate.

6. The system according to claim 1, characterized in that End face flange covers are arranged at both ends of the filtering, washing and drying equipment.

7. The system according to claim 1, characterized in that The filtrate outlet is arranged at the bottom of the outer cylinder, and the filter screen is located at the bottom of the inner cylinder; a vacuum gas outlet is also arranged on the side of the outer cylinder.

8. The system according to claim 1, characterized in that The arc width of the filter screen is 0.5~1.0 times the arc width of the inner tube jacket.

9. The system according to claim 1, characterized in that The shaft inner tube and the shaft outer tube are coaxial central inner and outer sleeves, the shaft heating medium inlet is arranged on the outer wall of the shaft inner tube, and the shaft heating medium outlet is arranged on the outer wall of the shaft outer tube.

10. The system according to claim 1, characterized in that Also included is a motor, which is used to drive the rotating sleeve shaft to rotate.

11. The system according to claim 10, characterized in that The motor is located at one end of the rotating jacket shaft, and the shaft heating medium inlet and the shaft heating medium outlet are located at the other end of the rotating jacket shaft.

12. The system according to claim 6, characterized in that The rotating jacket shaft passes through the end face flange cover, the filter sleeve and the center of the material inlet and outlet shaft.

13. The system according to claim 1, characterized in that The filter sleeve and the material inlet and outlet cylinder are fixedly connected via a flange.

14. The system according to claim 1, characterized in that The outer wall of the stirring paddle is evenly distributed with fins.

15. The system according to claim 6, characterized in that The two ends of the shaft outer cylinder are connected to the end face flange cover through a sealing component.

16. A method for producing high-performance insoluble sulfur, using the insoluble sulfur production system according to any one of claims 1 to 15.

17. The production method according to claim 16, characterized in that: It includes the following: (1) The quenching liquid continuously enters the quenching tower through the quenching liquid inlet to control the liquid level of the quenching liquid in the quenching tower. At the same time, the quenching liquid continuously discharges the quenching tower through the discharge port and is discharged from the production system through the quenching liquid discharge pipe; (2) After the quenching liquid level in the quenching tower is controlled to be stable, the high-temperature sulfur enters the sulfur distributor through the sulfur inlet and then enters the quenching section. The dispersed sulfur enters the quenching liquid to be cooled or mixed. The dispersed sulfur after cooling or mixing is quenched and becomes brittle in the quenching section. (3) After the sulfur is quenched, stop introducing the quenching liquid into the quenching tower, and discharge the quenching liquid in the quenching tower through the quenching tower outlet; Hot air is introduced into the quenching tower from the hot air inlet to dry the sulfur until the moisture content is less than 1%; hot air is continued to be introduced for aging; (4) After the sulfur is dried and matured, the extractant is continuously added to the quenching tower through the extractant inlet, and the motor at the top of the quenching tower is started. The motor drives the stirring rod and the crushing ball to rotate, so that the sulfur that has become brittle after rapid cooling is crushed and extraction is achieved at the same time; during the sulfur crushing process, sulfur powder smaller than the slit width or the opening diameter of the grading mesh plate passes through the mesh holes and enters the grading mesh plate, and enters the discharge pump together with the extractant through the discharge port; (5) The material discharged from the quenching tower outlet is lifted and transported to the sand mill through the discharge pump, and further ground to 100-300 mesh. The slurry containing 100-mesh sulfur powder is discharged from the sand mill outlet and enters the filtering, washing and drying equipment; (6) The slurry is first filtered in a filtering, washing and drying device to filter out the extractant and obtain a sulfur powder filter cake; (7) The sulfur powder filter cake is further extracted in a filtering, washing and drying device. The insoluble sulfur obtained after extraction and filtration is dried again with hot air to obtain an un-oiled insoluble sulfur product.

18. The production method according to claim 17, characterized in that: In step (2), the sulphur is quenched in the quenching section of the quenching tower for 1 h to 2 h.

19. The production method according to claim 17, characterized in that: The hot air drying temperature in step (3) is 50°C to 70°C; the hot air aging conditions include: the aging time is 30h to 50h, and the aging temperature is 50°C to 70°C.

20. The production method according to claim 17, characterized in that: In step (4), the sulfur particles passing through the slits or openings of the grading mesh are 1 mm to 8 mm.

21. The production method according to claim 17, characterized in that: In step (7), intermittent extraction is adopted, the number of intermittent extractions is 2 to 4 times, and the mass ratio of the extractant to solid is 2 to 4:1.

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